# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_H113k
_database_code_depnum_ccdc_archive 'CCDC 2053279'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-19 downloaded from the CCDC.
;
_audit_creation_date             2020-11-10
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C12 H24 O6, C2 H8 N'
_chemical_formula_sum            'C20 H32 N Ni O6 S10'
_chemical_formula_weight         761.77
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHNONiS
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.1765(4)
_cell_length_b                   12.2812(3)
_cell_length_c                   12.6527(4)
_cell_angle_alpha                87.364(2)
_cell_angle_beta                 68.465(3)
_cell_angle_gamma                80.094(2)
_cell_volume                     1591.12(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    12974
_cell_measurement_temperature    113
_cell_measurement_theta_max      30.8270
_cell_measurement_theta_min      2.0940
_shelx_estimated_absorpt_T_max   0.774
_shelx_estimated_absorpt_T_min   0.453
_exptl_absorpt_coefficient_mu    1.302
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             790
_exptl_crystal_size_max          0.724
_exptl_crystal_size_mid          0.378
_exptl_crystal_size_min          0.207
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.790
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22773
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.790
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.892
_diffrn_reflns_theta_min         2.105
_diffrn_ambient_temperature      113
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.790
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -18.00  10.00   0.50    0.06    --    5.18 -99.00   0.00   56
  2  ω    -58.00 -14.00   0.50    0.06    --    5.18 -40.00 -22.00   88
  3  ω     -8.00  18.00   0.50    0.06    --    5.18 -40.00 -22.00   52
  4  ω     -8.00  75.00   0.50    0.06    --    5.18  40.00 130.00  166
  5  ω     53.00  78.00   0.50    0.06    --    5.18  37.00 -90.00   50
  6  ω      1.00  27.00   0.50    0.06    --   -5.03 -99.00 120.00   52
  7  ω     -4.00  28.00   0.50    0.06    --   -5.03 -99.00 -60.00   64
  8  ω    -61.00   4.00   0.50    0.06    --   -5.03 -37.00-120.00  130
  9  ω    -77.00   5.00   0.50    0.06    --   -5.03 -37.00-180.00  164
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0558082000
_diffrn_orient_matrix_UB_12      0.0174628000
_diffrn_orient_matrix_UB_13      0.0491349000
_diffrn_orient_matrix_UB_21      -0.0342591000
_diffrn_orient_matrix_UB_22      0.0242594000
_diffrn_orient_matrix_UB_23      -0.0348977000
_diffrn_orient_matrix_UB_31      -0.0223623000
_diffrn_orient_matrix_UB_32      -0.0504492000
_diffrn_orient_matrix_UB_33      -0.0010850000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6618
_reflns_number_total             7934
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         7934
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0357
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0497P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.0981
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C13(H13A,H13B), C7(H7A,H7B), C5(H5A,H5B), C8(H8A,H8B), C3(H3A,
 H3B), C11(H11A,H11B), C10(H10A,H10B), C9(H9A,H9B), C4(H4A,H4B), C12(H12A,H12B),
  C14(H14A,H14B), C1(H1D,H1E)
2.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C2(H2A,H2B,H2C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.36035(2) 0.11915(2) 0.47174(2) 0.01513(7) Uani 1 1 d . . . . .
S2 S 0.31493(5) 0.06997(4) 0.64615(4) 0.02002(11) Uani 1 1 d . . . . .
S1 S 0.50197(4) 0.21672(3) 0.47688(4) 0.01892(10) Uani 1 1 d . . . . .
S9 S 0.14008(4) -0.03355(3) 0.27199(4) 0.01922(10) Uani 1 1 d . . . . .
S4 S 0.42087(5) 0.12317(4) 0.82332(4) 0.02055(11) Uani 1 1 d . . . . .
S6 S 0.40840(4) 0.16582(4) 0.29584(4) 0.01953(10) Uani 1 1 d . . . . .
S7 S 0.21926(5) 0.02075(3) 0.46674(4) 0.01971(10) Uani 1 1 d . . . . .
S8 S 0.31401(5) 0.09988(4) 0.11542(4) 0.02200(11) Uani 1 1 d . . . . .
S5 S 0.58223(5) 0.24080(4) 0.90694(4) 0.02521(11) Uani 1 1 d . . . . .
S3 S 0.58799(5) 0.26304(4) 0.66989(4) 0.02186(11) Uani 1 1 d . . . . .
S10 S 0.14466(5) -0.01026(4) 0.03502(4) 0.02605(12) Uani 1 1 d . . . . .
O4 O -0.00095(12) 0.69743(10) 0.66812(11) 0.0227(3) Uani 1 1 d . . . . .
O3 O 0.20735(12) 0.72732(9) 0.73360(11) 0.0208(3) Uani 1 1 d . . . . .
O6 O -0.01526(13) 0.34844(9) 0.84314(12) 0.0235(3) Uani 1 1 d . . . . .
O5 O -0.07102(13) 0.48589(10) 0.67683(12) 0.0266(3) Uani 1 1 d . . . . .
O2 O 0.26261(12) 0.58468(10) 0.89374(12) 0.0242(3) Uani 1 1 d . . . . .
O1 O 0.18679(13) 0.37467(10) 0.91897(12) 0.0239(3) Uani 1 1 d . . . . .
N1 N 0.14932(15) 0.50905(11) 0.74088(14) 0.0199(3) Uani 1 1 d . . . . .
H1A H 0.075166 0.516453 0.725167 0.024 Uiso 1 1 calc R U . . .
H1B H 0.168713 0.577107 0.746141 0.024 Uiso 1 1 calc R U . . .
H1C H 0.137130 0.473718 0.807925 0.024 Uiso 1 1 calc R U . . .
C19 C 0.23100(17) 0.03282(13) 0.32770(15) 0.0162(3) Uani 1 1 d . . . . .
C16 C 0.41563(17) 0.13462(13) 0.68706(15) 0.0173(3) Uani 1 1 d . . . . .
C20 C 0.19740(18) 0.01660(13) 0.13544(16) 0.0193(4) Uani 1 1 d . . . . .
C6 C 0.25786(19) 0.76199(14) 0.81237(17) 0.0234(4) Uani 1 1 d . . . . .
H6A H 0.185339 0.791144 0.882899 0.028 Uiso 1 1 calc R U . . .
H6B H 0.309397 0.821469 0.779315 0.028 Uiso 1 1 calc R U . . .
C13 C 0.0499(2) 0.26033(14) 0.88993(18) 0.0266(4) Uani 1 1 d . . . . .
H13A H 0.127573 0.221115 0.828893 0.032 Uiso 1 1 calc R U . . .
H13B H -0.009234 0.206746 0.926249 0.032 Uiso 1 1 calc R U . . .
C15 C 0.49570(17) 0.19933(13) 0.61367(16) 0.0174(3) Uani 1 1 d . . . . .
C7 C 0.12689(19) 0.81674(13) 0.70316(18) 0.0246(4) Uani 1 1 d . . . . .
H7A H 0.176947 0.877429 0.671567 0.030 Uiso 1 1 calc R U . . .
H7B H 0.050719 0.845586 0.771376 0.030 Uiso 1 1 calc R U . . .
C5 C 0.34255(19) 0.66479(14) 0.83859(17) 0.0238(4) Uani 1 1 d . . . . .
H5A H 0.412084 0.632842 0.767580 0.029 Uiso 1 1 calc R U . . .
H5B H 0.384188 0.688021 0.888764 0.029 Uiso 1 1 calc R U . . .
C18 C 0.31163(17) 0.09612(13) 0.25404(15) 0.0169(3) Uani 1 1 d . . . . .
C8 C 0.08149(19) 0.77672(14) 0.61644(17) 0.0229(4) Uani 1 1 d . . . . .
H8A H 0.032882 0.839533 0.589032 0.028 Uiso 1 1 calc R U . . .
H8B H 0.157390 0.742535 0.550634 0.028 Uiso 1 1 calc R U . . .
C3 C 0.2360(2) 0.41774(15) 0.99486(17) 0.0255(4) Uani 1 1 d . . . . .
H3A H 0.279925 0.356278 1.027960 0.031 Uiso 1 1 calc R U . . .
H3B H 0.163235 0.459920 1.057676 0.031 Uiso 1 1 calc R U . . .
C11 C -0.1479(2) 0.40430(15) 0.73400(19) 0.0293(4) Uani 1 1 d . . . . .
H11A H -0.187655 0.377614 0.684053 0.035 Uiso 1 1 calc R U . . .
H11B H -0.219002 0.437148 0.803690 0.035 Uiso 1 1 calc R U . . .
C10 C -0.1495(2) 0.58461(15) 0.6597(2) 0.0302(5) Uani 1 1 d . . . . .
H10A H -0.210318 0.617678 0.733874 0.036 Uiso 1 1 calc R U . . .
H10B H -0.201463 0.567525 0.615775 0.036 Uiso 1 1 calc R U . . .
C17 C 0.53260(17) 0.21043(14) 0.80572(16) 0.0189(4) Uani 1 1 d . . . . .
C9 C -0.0615(2) 0.66435(15) 0.59587(18) 0.0260(4) Uani 1 1 d . . . . .
H9A H 0.005707 0.628554 0.525585 0.031 Uiso 1 1 calc R U . . .
H9B H -0.112681 0.729669 0.574459 0.031 Uiso 1 1 calc R U . . .
C4 C 0.33122(19) 0.49198(15) 0.93058(18) 0.0261(4) Uani 1 1 d . . . . .
H4A H 0.372619 0.516713 0.980216 0.031 Uiso 1 1 calc R U . . .
H4B H 0.400523 0.451519 0.864234 0.031 Uiso 1 1 calc R U . . .
C12 C -0.0632(2) 0.30920(15) 0.76472(19) 0.0298(4) Uani 1 1 d . . . . .
H12A H -0.114445 0.249951 0.799434 0.036 Uiso 1 1 calc R U . . .
H12B H 0.010586 0.278437 0.695667 0.036 Uiso 1 1 calc R U . . .
C14 C 0.0905(2) 0.30762(15) 0.97634(18) 0.0270(4) Uani 1 1 d . . . . .
H14A H 0.014066 0.352753 1.033495 0.032 Uiso 1 1 calc R U . . .
H14B H 0.126849 0.247193 1.016036 0.032 Uiso 1 1 calc R U . . .
C1 C 0.2587(2) 0.44348(16) 0.64842(19) 0.0363(5) Uani 1 1 d . . . . .
H1D H 0.328495 0.412633 0.677297 0.044 Uiso 1 1 calc R U . . .
H1E H 0.227165 0.380713 0.626521 0.044 Uiso 1 1 calc R U . . .
C2 C 0.3139(2) 0.50931(17) 0.5467(2) 0.0386(5) Uani 1 1 d . . . . .
H2A H 0.383621 0.461718 0.487891 0.058 Uiso 1 1 calc R U . . .
H2B H 0.349569 0.569343 0.566929 0.058 Uiso 1 1 calc R U . . .
H2C H 0.245234 0.540556 0.517961 0.058 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S2 2.1571(5) . ?
Ni1 S1 2.1635(5) . ?
Ni1 S6 2.1637(5) . ?
Ni1 S7 2.1649(5) . ?
S2 C16 1.7141(17) . ?
S1 C15 1.7111(18) . ?
S9 C19 1.7486(16) . ?
S9 C20 1.7321(19) . ?
S4 C16 1.7449(18) . ?
S4 C17 1.7297(18) . ?
S6 C18 1.7212(17) . ?
S7 C19 1.7168(18) . ?
S8 C20 1.7324(18) . ?
S8 C18 1.7429(18) . ?
S5 C17 1.6503(18) . ?
S3 C15 1.7464(17) . ?
S3 C17 1.7346(19) . ?
S10 C20 1.6510(18) . ?
O4 C8 1.426(2) . ?
O4 C9 1.429(2) . ?
O3 C6 1.424(2) . ?
O3 C7 1.428(2) . ?
O6 C13 1.428(2) . ?
O6 C12 1.424(2) . ?
O5 C11 1.428(2) . ?
O5 C10 1.427(2) . ?
O2 C5 1.426(2) . ?
O2 C4 1.419(2) . ?
O1 C3 1.428(2) . ?
O1 C14 1.428(2) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N1 C1 1.487(2) . ?
C19 C18 1.357(3) . ?
C16 C15 1.364(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C5 1.495(2) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.500(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.499(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.502(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.503(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C9 1.501(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C1 H1D 0.9900 . ?
C1 H1E 0.9900 . ?
C1 C2 1.477(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S2 Ni1 S1 93.230(18) . . ?
S2 Ni1 S6 178.989(19) . . ?
S2 Ni1 S7 86.639(18) . . ?
S1 Ni1 S6 86.846(18) . . ?
S1 Ni1 S7 179.703(18) . . ?
S6 Ni1 S7 93.281(18) . . ?
C16 S2 Ni1 102.28(6) . . ?
C15 S1 Ni1 102.03(6) . . ?
C20 S9 C19 97.41(8) . . ?
C17 S4 C16 97.44(9) . . ?
C18 S6 Ni1 101.98(6) . . ?
C19 S7 Ni1 101.96(6) . . ?
C20 S8 C18 97.30(8) . . ?
C17 S3 C15 97.79(9) . . ?
C8 O4 C9 112.35(15) . . ?
C6 O3 C7 111.61(13) . . ?
C12 O6 C13 112.02(13) . . ?
C10 O5 C11 111.94(14) . . ?
C4 O2 C5 113.00(13) . . ?
C3 O1 C14 111.83(15) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
S7 C19 S9 122.77(10) . . ?
C18 C19 S9 115.73(13) . . ?
C18 C19 S7 121.50(13) . . ?
S2 C16 S4 122.57(11) . . ?
C15 C16 S2 121.02(14) . . ?
C15 C16 S4 116.40(13) . . ?
S9 C20 S8 113.13(10) . . ?
S10 C20 S9 123.56(11) . . ?
S10 C20 S8 123.31(11) . . ?
O3 C6 H6A 110.0 . . ?
O3 C6 H6B 110.0 . . ?
O3 C6 C5 108.53(14) . . ?
H6A C6 H6B 108.4 . . ?
C5 C6 H6A 110.0 . . ?
C5 C6 H6B 110.0 . . ?
O6 C13 H13A 109.9 . . ?
O6 C13 H13B 109.9 . . ?
O6 C13 C14 108.78(14) . . ?
H13A C13 H13B 108.3 . . ?
C14 C13 H13A 109.9 . . ?
C14 C13 H13B 109.9 . . ?
S1 C15 S3 123.21(11) . . ?
C16 C15 S1 121.43(13) . . ?
C16 C15 S3 115.36(14) . . ?
O3 C7 H7A 109.8 . . ?
O3 C7 H7B 109.8 . . ?
O3 C7 C8 109.27(13) . . ?
H7A C7 H7B 108.3 . . ?
C8 C7 H7A 109.8 . . ?
C8 C7 H7B 109.8 . . ?
O2 C5 C6 108.13(14) . . ?
O2 C5 H5A 110.1 . . ?
O2 C5 H5B 110.1 . . ?
C6 C5 H5A 110.1 . . ?
C6 C5 H5B 110.1 . . ?
H5A C5 H5B 108.4 . . ?
S6 C18 S8 122.37(11) . . ?
C19 C18 S6 121.24(14) . . ?
C19 C18 S8 116.38(13) . . ?
O4 C8 C7 108.42(15) . . ?
O4 C8 H8A 110.0 . . ?
O4 C8 H8B 110.0 . . ?
C7 C8 H8A 110.0 . . ?
C7 C8 H8B 110.0 . . ?
H8A C8 H8B 108.4 . . ?
O1 C3 H3A 109.9 . . ?
O1 C3 H3B 109.9 . . ?
O1 C3 C4 109.08(16) . . ?
H3A C3 H3B 108.3 . . ?
C4 C3 H3A 109.9 . . ?
C4 C3 H3B 109.9 . . ?
O5 C11 H11A 109.7 . . ?
O5 C11 H11B 109.7 . . ?
O5 C11 C12 109.60(16) . . ?
H11A C11 H11B 108.2 . . ?
C12 C11 H11A 109.7 . . ?
C12 C11 H11B 109.7 . . ?
O5 C10 H10A 110.0 . . ?
O5 C10 H10B 110.0 . . ?
O5 C10 C9 108.64(15) . . ?
H10A C10 H10B 108.3 . . ?
C9 C10 H10A 110.0 . . ?
C9 C10 H10B 110.0 . . ?
S4 C17 S3 112.98(10) . . ?
S5 C17 S4 123.86(12) . . ?
S5 C17 S3 123.16(11) . . ?
O4 C9 C10 108.01(16) . . ?
O4 C9 H9A 110.1 . . ?
O4 C9 H9B 110.1 . . ?
C10 C9 H9A 110.1 . . ?
C10 C9 H9B 110.1 . . ?
H9A C9 H9B 108.4 . . ?
O2 C4 C3 108.44(15) . . ?
O2 C4 H4A 110.0 . . ?
O2 C4 H4B 110.0 . . ?
C3 C4 H4A 110.0 . . ?
C3 C4 H4B 110.0 . . ?
H4A C4 H4B 108.4 . . ?
O6 C12 C11 108.45(14) . . ?
O6 C12 H12A 110.0 . . ?
O6 C12 H12B 110.0 . . ?
C11 C12 H12A 110.0 . . ?
C11 C12 H12B 110.0 . . ?
H12A C12 H12B 108.4 . . ?
O1 C14 C13 108.44(16) . . ?
O1 C14 H14A 110.0 . . ?
O1 C14 H14B 110.0 . . ?
C13 C14 H14A 110.0 . . ?
C13 C14 H14B 110.0 . . ?
H14A C14 H14B 108.4 . . ?
N1 C1 H1D 109.0 . . ?
N1 C1 H1E 109.0 . . ?
H1D C1 H1E 107.8 . . ?
C2 C1 N1 112.90(16) . . ?
C2 C1 H1D 109.0 . . ?
C2 C1 H1E 109.0 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S2 C16 S4 -179.70(9) . . . . ?
Ni1 S2 C16 C15 0.97(15) . . . . ?
Ni1 S1 C15 S3 -178.27(9) . . . . ?
Ni1 S1 C15 C16 0.95(15) . . . . ?
Ni1 S6 C18 S8 -177.89(9) . . . . ?
Ni1 S6 C18 C19 0.59(15) . . . . ?
Ni1 S7 C19 S9 178.52(9) . . . . ?
Ni1 S7 C19 C18 -2.10(15) . . . . ?
S2 C16 C15 S1 -1.4(2) . . . . ?
S2 C16 C15 S3 177.90(9) . . . . ?
S9 C19 C18 S6 -179.49(9) . . . . ?
S9 C19 C18 S8 -0.93(19) . . . . ?
S4 C16 C15 S1 179.26(9) . . . . ?
S4 C16 C15 S3 -1.46(19) . . . . ?
S7 C19 C18 S6 1.1(2) . . . . ?
S7 C19 C18 S8 179.65(9) . . . . ?
O3 C6 C5 O2 -63.96(19) . . . . ?
O3 C7 C8 O4 65.24(19) . . . . ?
O6 C13 C14 O1 -66.06(19) . . . . ?
O5 C11 C12 O6 63.7(2) . . . . ?
O5 C10 C9 O4 -66.9(2) . . . . ?
O1 C3 C4 O2 65.12(19) . . . . ?
C19 S9 C20 S8 1.87(11) . . . . ?
C19 S9 C20 S10 -177.13(12) . . . . ?
C16 S4 C17 S5 178.65(12) . . . . ?
C16 S4 C17 S3 -1.48(11) . . . . ?
C20 S9 C19 S7 178.82(11) . . . . ?
C20 S9 C19 C18 -0.59(15) . . . . ?
C20 S8 C18 S6 -179.51(11) . . . . ?
C20 S8 C18 C19 1.95(15) . . . . ?
C6 O3 C7 C8 177.48(16) . . . . ?
C13 O6 C12 C11 171.15(16) . . . . ?
C15 S3 C17 S4 0.86(11) . . . . ?
C15 S3 C17 S5 -179.27(11) . . . . ?
C7 O3 C6 C5 -179.05(15) . . . . ?
C5 O2 C4 C3 175.72(15) . . . . ?
C18 S8 C20 S9 -2.26(11) . . . . ?
C18 S8 C20 S10 176.74(12) . . . . ?
C8 O4 C9 C10 -177.89(14) . . . . ?
C3 O1 C14 C13 -176.64(14) . . . . ?
C11 O5 C10 C9 -178.09(16) . . . . ?
C10 O5 C11 C12 -171.88(16) . . . . ?
C17 S4 C16 S2 -177.56(11) . . . . ?
C17 S4 C16 C15 1.80(15) . . . . ?
C17 S3 C15 S1 179.62(11) . . . . ?
C17 S3 C15 C16 0.36(15) . . . . ?
C9 O4 C8 C7 172.98(14) . . . . ?
C4 O2 C5 C6 -175.44(15) . . . . ?
C12 O6 C13 C14 -176.75(16) . . . . ?
C14 O1 C3 C4 -177.04(14) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.966
_oxdiff_exptl_absorpt_empirical_full_min 0.632
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_213k
_database_code_depnum_ccdc_archive 'CCDC 2053288'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-19 downloaded from the CCDC.
;
_audit_creation_date             2020-11-11
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C12 H24 O6, C2 H7 F N'
_chemical_formula_sum            'C20 H31 F N Ni O6 S10'
_chemical_formula_weight         779.77
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHNOFNiS
_chemical_oxdiff_usercomment     20_20200608
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.4363(3)
_cell_length_b                   12.6370(4)
_cell_length_c                   12.9511(4)
_cell_angle_alpha                70.974(3)
_cell_angle_beta                 79.852(2)
_cell_angle_gamma                80.316(2)
_cell_volume                     1578.17(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    10622
_cell_measurement_temperature    213
_cell_measurement_theta_max      30.4190
_cell_measurement_theta_min      2.0090
_shelx_estimated_absorpt_T_max   0.891
_shelx_estimated_absorpt_T_min   0.554
_exptl_absorpt_coefficient_mu    1.319
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60134
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             806
_exptl_crystal_size_max          0.507
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0441
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.794
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19305
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.794
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.750
_diffrn_reflns_theta_min         1.997
_diffrn_ambient_temperature      213
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.794
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -1.00  78.00   0.50    0.25    --    5.18  57.00 -90.00  158
  2  ω     -6.00  78.00   0.50    0.25    --    5.18  37.00  60.00  168
  3  ω     -4.00  52.00   0.50    0.25    --    5.18  57.00 150.00  112
  4  ω    -18.00  33.00   0.50    0.25    --    5.18 -99.00 -60.00  102
  5  ω    -17.00  32.00   0.50    0.25    --    5.18 -99.00 150.00   98
  6  ω     -6.00  20.00   0.50    0.25    --   -5.03 -99.00 120.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0025160000
_diffrn_orient_matrix_UB_12      0.0549778000
_diffrn_orient_matrix_UB_13      0.0040279000
_diffrn_orient_matrix_UB_21      -0.0105065000
_diffrn_orient_matrix_UB_22      -0.0219124000
_diffrn_orient_matrix_UB_23      0.0582751000
_diffrn_orient_matrix_UB_31      0.0686951000
_diffrn_orient_matrix_UB_32      -0.0085436000
_diffrn_orient_matrix_UB_33      0.0013577000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6022
_reflns_number_total             7814
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       0.0014(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         7814
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0336
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0384P)²+0.1028P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0897
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
2. Others
 Sof(H1AA)=Sof(H1AB)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(F1)=1-FVAR(1)
 Sof(H1BC)=Sof(H1BD)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(F1A)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C7(H7A,H7B), C6(H6A,H6B), C3(H3A,H3B), C4(H4A,H4B), C11(H11A,
 H11B), C8(H8A,H8B), C13(H13A,H13B), C12(H12A,H12B), C14(H14A,H14B), C1(H1BC,
 H1BD), C1(H1AA,H1AB), C9(H9A,H9B), C10(H10A,H10B), C2(H2A,H2B), C2A(H2AA,H2AB)
3.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.16370(2) 0.40564(2) 0.49070(2) 0.02730(8) Uani 1 1 d . . . . .
S2 S -0.07913(4) 0.26639(4) 0.29615(4) 0.03088(11) Uani 1 1 d . . . . .
S4 S 0.00770(4) 0.31387(4) 0.48674(4) 0.03098(11) Uani 1 1 d . . . . .
S6 S 0.10088(5) 0.36913(4) 0.66583(4) 0.03286(12) Uani 1 1 d . . . . .
S5 S 0.22951(5) 0.44022(4) 0.31598(4) 0.03345(12) Uani 1 1 d . . . . .
S8 S 0.19684(5) 0.43712(4) 0.84089(4) 0.03429(12) Uani 1 1 d . . . . .
S3 S 0.12889(5) 0.37612(5) 0.14061(4) 0.03632(12) Uani 1 1 d . . . . .
S9 S 0.40148(5) 0.55176(5) 0.68444(5) 0.03747(13) Uani 1 1 d . . . . .
S7 S 0.31493(5) 0.50211(4) 0.49438(4) 0.03533(12) Uani 1 1 d . . . . .
S10 S 0.37608(6) 0.54823(5) 0.91689(5) 0.04585(15) Uani 1 1 d . . . . .
S1 S -0.04968(6) 0.26424(5) 0.06419(5) 0.04627(15) Uani 1 1 d . . . . .
O2 O 0.16770(12) 0.89551(11) 0.28538(12) 0.0360(3) Uani 1 1 d . . . . .
O3 O 0.26715(13) 1.06499(12) 0.32927(12) 0.0380(3) Uani 1 1 d . . . . .
N1 N 0.44595(14) 0.89061(13) 0.25305(13) 0.0300(3) Uani 1 1 d . . . . .
H1A H 0.402543 0.876822 0.205487 0.036 Uiso 1 1 calc R U . . .
H1B H 0.515946 0.925889 0.215831 0.036 Uiso 1 1 calc R U . . .
H1C H 0.392389 0.934694 0.288848 0.036 Uiso 1 1 calc R U . . .
O5 O 0.68786(13) 0.97933(12) 0.13939(13) 0.0428(4) Uani 1 1 d . . . . .
O1 O 0.31699(13) 0.80811(11) 0.12225(12) 0.0383(3) Uani 1 1 d . . . . .
O6 O 0.59003(14) 0.81704(13) 0.07825(12) 0.0418(3) Uani 1 1 d . . . . .
O4 O 0.54228(13) 1.07217(12) 0.29675(13) 0.0421(4) Uani 1 1 d . . . . .
C16 C 0.02443(17) 0.32438(15) 0.34985(16) 0.0278(4) Uani 1 1 d . . . . .
C18 C 0.20529(18) 0.43595(15) 0.70545(16) 0.0286(4) Uani 1 1 d . . . . .
C19 C 0.29917(17) 0.49205(16) 0.63138(17) 0.0298(4) Uani 1 1 d . . . . .
C17 C 0.12107(17) 0.37737(16) 0.27598(16) 0.0294(4) Uani 1 1 d . . . . .
C20 C 0.32634(18) 0.51520(16) 0.81926(17) 0.0324(4) Uani 1 1 d . . . . .
C15 C -0.00152(18) 0.30000(17) 0.16170(17) 0.0332(4) Uani 1 1 d . . . . .
C5 C 0.08482(19) 0.98152(18) 0.3213(2) 0.0409(5) Uani 1 1 d . . . . .
H5A H 0.002675 0.953276 0.361835 0.049 Uiso 1 1 calc R U . . .
H5B H 0.063847 1.046203 0.257549 0.049 Uiso 1 1 calc R U . . .
C7 C 0.3317(2) 1.11473(18) 0.38769(19) 0.0415(5) Uani 1 1 d . . . . .
H7A H 0.359912 1.057508 0.454057 0.050 Uiso 1 1 calc R U . . .
H7B H 0.271644 1.174174 0.410007 0.050 Uiso 1 1 calc R U . . .
C6 C 0.15405(19) 1.01670(19) 0.39402(19) 0.0405(5) Uani 1 1 d . . . . .
H6A H 0.096135 1.072053 0.424229 0.049 Uiso 1 1 calc R U . . .
H6B H 0.179828 0.951299 0.455456 0.049 Uiso 1 1 calc R U . . .
C3 C 0.1996(2) 0.76512(17) 0.1847(2) 0.0416(5) Uani 1 1 d . . . . .
H3A H 0.220062 0.705209 0.252022 0.050 Uiso 1 1 calc R U . . .
H3B H 0.157291 0.733534 0.141414 0.050 Uiso 1 1 calc R U . . .
C4 C 0.11016(19) 0.85970(18) 0.2132(2) 0.0394(5) Uani 1 1 d . . . . .
H4A H 0.096294 0.922431 0.146147 0.047 Uiso 1 1 calc R U . . .
H4B H 0.024948 0.834472 0.248859 0.047 Uiso 1 1 calc R U . . .
C11 C 0.7706(2) 0.9023(2) 0.0901(2) 0.0493(6) Uani 1 1 d . . . . .
H11A H 0.797971 0.833263 0.147267 0.059 Uiso 1 1 calc R U . . .
H11B H 0.849244 0.936005 0.048158 0.059 Uiso 1 1 calc R U . . .
C8 C 0.4482(2) 1.16329(18) 0.3127(2) 0.0427(5) Uani 1 1 d . . . . .
H8A H 0.421854 1.211997 0.241838 0.051 Uiso 1 1 calc R U . . .
H8B H 0.486136 1.208596 0.345586 0.051 Uiso 1 1 calc R U . . .
C13 C 0.5198(2) 0.7796(2) 0.0137(2) 0.0485(6) Uani 1 1 d . . . . .
H13A H 0.577728 0.725598 -0.018272 0.058 Uiso 1 1 calc R U . . .
H13B H 0.488985 0.843899 -0.046560 0.058 Uiso 1 1 calc R U . . .
C12 C 0.6966(2) 0.8749(2) 0.0153(2) 0.0501(6) Uani 1 1 d . . . . .
H12A H 0.664086 0.944543 -0.038720 0.060 Uiso 1 1 calc R U . . .
H12B H 0.754725 0.827744 -0.024703 0.060 Uiso 1 1 calc R U . . .
C14 C 0.4060(2) 0.72518(19) 0.0856(2) 0.0480(6) Uani 1 1 d . . . . .
H14A H 0.362130 0.692420 0.044352 0.058 Uiso 1 1 calc R U . . .
H14B H 0.436103 0.664563 0.149052 0.058 Uiso 1 1 calc R U . . .
C1 C 0.4903(3) 0.7828(2) 0.3336(2) 0.0532(6) Uani 1 1 d . . . . .
H1BC H 0.424450 0.730970 0.348739 0.064 Uiso 0.714(7) 1 calc R U P A 2
H1BD H 0.572012 0.749164 0.300399 0.064 Uiso 0.714(7) 1 calc R U P A 2
H1AA H 0.486701 0.720987 0.304517 0.064 Uiso 0.286(7) 1 calc R U P A 1
H1AB H 0.582055 0.782966 0.341264 0.064 Uiso 0.286(7) 1 calc R U P A 1
C9 C 0.6645(2) 1.1093(2) 0.2405(2) 0.0505(6) Uani 1 1 d . . . . .
H9A H 0.706910 1.135587 0.287838 0.061 Uiso 1 1 calc R U . . .
H9B H 0.650261 1.172039 0.173546 0.061 Uiso 1 1 calc R U . . .
C10 C 0.7501(2) 1.0128(2) 0.2112(2) 0.0497(6) Uani 1 1 d . . . . .
H10A H 0.835978 1.035973 0.174624 0.060 Uiso 1 1 calc R U . . .
H10B H 0.763356 0.949618 0.278008 0.060 Uiso 1 1 calc R U . . .
C2 C 0.5122(4) 0.7932(3) 0.4364(3) 0.0498(12) Uani 0.714(7) 1 d . . P A 2
H2A H 0.562119 0.856196 0.424619 0.060 Uiso 0.714(7) 1 calc R U P A 2
H2B H 0.557930 0.723638 0.481037 0.060 Uiso 0.714(7) 1 calc R U P A 2
C2A C 0.4173(10) 0.7621(7) 0.4368(7) 0.049(3) Uani 0.286(7) 1 d . . P A 1
H2AA H 0.328403 0.752089 0.430068 0.059 Uiso 0.286(7) 1 calc R U P A 1
H2AB H 0.455653 0.690744 0.484869 0.059 Uiso 0.286(7) 1 calc R U P A 1
F1A F 0.4084(6) 0.8443(5) 0.4878(5) 0.0678(15) Uani 0.714(7) 1 d . . P A 1
F1 F 0.3716(13) 0.8157(13) 0.4891(13) 0.058(3) Uani 0.286(7) 1 d . . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S4 2.1683(5) . ?
Ni1 S6 2.1638(6) . ?
Ni1 S5 2.1661(6) . ?
Ni1 S7 2.1658(5) . ?
S2 C16 1.7472(17) . ?
S2 C15 1.733(2) . ?
S4 C16 1.714(2) . ?
S6 C18 1.7184(18) . ?
S5 C17 1.7197(18) . ?
S8 C18 1.7454(19) . ?
S8 C20 1.736(2) . ?
S3 C17 1.7457(19) . ?
S3 C15 1.729(2) . ?
S9 C19 1.7463(17) . ?
S9 C20 1.729(2) . ?
S7 C19 1.717(2) . ?
S10 C20 1.6404(19) . ?
S1 C15 1.6504(19) . ?
O2 C5 1.420(2) . ?
O2 C4 1.416(2) . ?
O3 C7 1.433(2) . ?
O3 C6 1.424(3) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N1 H1C 0.9000 . ?
N1 C1 1.480(3) . ?
O5 C11 1.425(3) . ?
O5 C10 1.424(3) . ?
O1 C3 1.428(3) . ?
O1 C14 1.424(2) . ?
O6 C13 1.431(3) . ?
O6 C12 1.415(3) . ?
O4 C8 1.427(2) . ?
O4 C9 1.424(3) . ?
C16 C17 1.360(3) . ?
C18 C19 1.357(3) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 C6 1.493(3) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 C8 1.498(3) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 C4 1.492(3) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 C12 1.491(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 C14 1.490(3) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C1 H1BC 0.9800 . ?
C1 H1BD 0.9800 . ?
C1 H1AA 0.9800 . ?
C1 H1AB 0.9800 . ?
C1 C2 1.440(4) . ?
C1 C2A 1.384(10) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 C10 1.498(3) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 F1 1.527(15) . ?
C2A H2AA 0.9800 . ?
C2A H2AB 0.9800 . ?
C2A F1A 1.385(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S6 Ni1 S4 86.996(19) . . ?
S6 Ni1 S5 179.04(2) . . ?
S6 Ni1 S7 92.77(2) . . ?
S5 Ni1 S4 93.311(19) . . ?
S7 Ni1 S4 178.14(2) . . ?
S7 Ni1 S5 86.947(19) . . ?
C15 S2 C16 97.57(9) . . ?
C16 S4 Ni1 101.76(6) . . ?
C18 S6 Ni1 102.51(7) . . ?
C17 S5 Ni1 101.99(7) . . ?
C20 S8 C18 97.16(9) . . ?
C15 S3 C17 97.39(9) . . ?
C20 S9 C19 97.44(9) . . ?
C19 S7 Ni1 102.38(7) . . ?
C4 O2 C5 112.12(14) . . ?
C6 O3 C7 112.31(16) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
C10 O5 C11 113.38(16) . . ?
C14 O1 C3 112.52(16) . . ?
C12 O6 C13 112.97(18) . . ?
C9 O4 C8 112.04(16) . . ?
S4 C16 S2 122.55(11) . . ?
C17 C16 S2 115.58(15) . . ?
C17 C16 S4 121.86(14) . . ?
S6 C18 S8 122.71(12) . . ?
C19 C18 S6 121.02(15) . . ?
C19 C18 S8 116.26(14) . . ?
S7 C19 S9 122.84(12) . . ?
C18 C19 S9 115.88(15) . . ?
C18 C19 S7 121.28(14) . . ?
S5 C17 S3 122.64(12) . . ?
C16 C17 S5 121.05(15) . . ?
C16 C17 S3 116.31(14) . . ?
S9 C20 S8 113.18(10) . . ?
S10 C20 S8 123.81(13) . . ?
S10 C20 S9 122.99(12) . . ?
S3 C15 S2 113.07(10) . . ?
S1 C15 S2 123.00(12) . . ?
S1 C15 S3 123.92(13) . . ?
O2 C5 H5A 109.9 . . ?
O2 C5 H5B 109.9 . . ?
O2 C5 C6 108.72(15) . . ?
H5A C5 H5B 108.3 . . ?
C6 C5 H5A 109.9 . . ?
C6 C5 H5B 109.9 . . ?
O3 C7 H7A 110.1 . . ?
O3 C7 H7B 110.1 . . ?
O3 C7 C8 108.11(18) . . ?
H7A C7 H7B 108.4 . . ?
C8 C7 H7A 110.1 . . ?
C8 C7 H7B 110.1 . . ?
O3 C6 C5 107.83(18) . . ?
O3 C6 H6A 110.1 . . ?
O3 C6 H6B 110.1 . . ?
C5 C6 H6A 110.1 . . ?
C5 C6 H6B 110.1 . . ?
H6A C6 H6B 108.5 . . ?
O1 C3 H3A 110.0 . . ?
O1 C3 H3B 110.0 . . ?
O1 C3 C4 108.30(16) . . ?
H3A C3 H3B 108.4 . . ?
C4 C3 H3A 110.0 . . ?
C4 C3 H3B 110.0 . . ?
O2 C4 C3 108.76(16) . . ?
O2 C4 H4A 109.9 . . ?
O2 C4 H4B 109.9 . . ?
C3 C4 H4A 109.9 . . ?
C3 C4 H4B 109.9 . . ?
H4A C4 H4B 108.3 . . ?
O5 C11 H11A 109.9 . . ?
O5 C11 H11B 109.9 . . ?
O5 C11 C12 108.78(17) . . ?
H11A C11 H11B 108.3 . . ?
C12 C11 H11A 109.9 . . ?
C12 C11 H11B 109.9 . . ?
O4 C8 C7 108.10(17) . . ?
O4 C8 H8A 110.1 . . ?
O4 C8 H8B 110.1 . . ?
C7 C8 H8A 110.1 . . ?
C7 C8 H8B 110.1 . . ?
H8A C8 H8B 108.4 . . ?
O6 C13 H13A 109.9 . . ?
O6 C13 H13B 109.9 . . ?
O6 C13 C14 109.06(19) . . ?
H13A C13 H13B 108.3 . . ?
C14 C13 H13A 109.9 . . ?
C14 C13 H13B 109.9 . . ?
O6 C12 C11 109.3(2) . . ?
O6 C12 H12A 109.8 . . ?
O6 C12 H12B 109.8 . . ?
C11 C12 H12A 109.8 . . ?
C11 C12 H12B 109.8 . . ?
H12A C12 H12B 108.3 . . ?
O1 C14 C13 108.76(18) . . ?
O1 C14 H14A 109.9 . . ?
O1 C14 H14B 109.9 . . ?
C13 C14 H14A 109.9 . . ?
C13 C14 H14B 109.9 . . ?
H14A C14 H14B 108.3 . . ?
N1 C1 H1BC 108.7 . . ?
N1 C1 H1BD 108.7 . . ?
N1 C1 H1AA 108.7 . . ?
N1 C1 H1AB 108.7 . . ?
H1BC C1 H1BD 107.6 . . ?
H1AA C1 H1AB 107.6 . . ?
C2 C1 N1 114.3(2) . . ?
C2 C1 H1BC 108.7 . . ?
C2 C1 H1BD 108.7 . . ?
C2A C1 N1 114.2(4) . . ?
C2A C1 H1AA 108.7 . . ?
C2A C1 H1AB 108.7 . . ?
O4 C9 H9A 109.9 . . ?
O4 C9 H9B 109.9 . . ?
O4 C9 C10 108.75(18) . . ?
H9A C9 H9B 108.3 . . ?
C10 C9 H9A 109.9 . . ?
C10 C9 H9B 109.9 . . ?
O5 C10 C9 108.48(17) . . ?
O5 C10 H10A 110.0 . . ?
O5 C10 H10B 110.0 . . ?
C9 C10 H10A 110.0 . . ?
C9 C10 H10B 110.0 . . ?
H10A C10 H10B 108.4 . . ?
C1 C2 H2A 111.5 . . ?
C1 C2 H2B 111.5 . . ?
C1 C2 F1 101.2(6) . . ?
H2A C2 H2B 109.4 . . ?
F1 C2 H2A 111.5 . . ?
F1 C2 H2B 111.5 . . ?
C1 C2A H2AA 108.3 . . ?
C1 C2A H2AB 108.3 . . ?
H2AA C2A H2AB 107.4 . . ?
F1A C2A C1 115.9(7) . . ?
F1A C2A H2AA 108.3 . . ?
F1A C2A H2AB 108.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S4 C16 S2 -179.03(9) . . . . ?
Ni1 S4 C16 C17 1.96(17) . . . . ?
Ni1 S6 C18 S8 178.59(9) . . . . ?
Ni1 S6 C18 C19 -0.86(16) . . . . ?
Ni1 S5 C17 S3 -178.79(10) . . . . ?
Ni1 S5 C17 C16 0.49(17) . . . . ?
Ni1 S7 C19 S9 178.04(10) . . . . ?
Ni1 S7 C19 C18 -1.69(17) . . . . ?
S2 C16 C17 S5 179.16(9) . . . . ?
S2 C16 C17 S3 -1.5(2) . . . . ?
S4 C16 C17 S5 -1.8(2) . . . . ?
S4 C16 C17 S3 177.57(9) . . . . ?
S6 C18 C19 S9 -177.93(9) . . . . ?
S6 C18 C19 S7 1.8(2) . . . . ?
S8 C18 C19 S9 2.6(2) . . . . ?
S8 C18 C19 S7 -177.66(10) . . . . ?
O2 C5 C6 O3 64.0(2) . . . . ?
O3 C7 C8 O4 -69.0(2) . . . . ?
N1 C1 C2 F1 72.9(6) . . . . ?
N1 C1 C2A F1A -56.1(8) . . . . ?
O5 C11 C12 O6 -64.9(2) . . . . ?
O1 C3 C4 O2 -66.0(2) . . . . ?
O6 C13 C14 O1 65.2(2) . . . . ?
O4 C9 C10 O5 61.6(3) . . . . ?
C16 S2 C15 S3 -2.77(12) . . . . ?
C16 S2 C15 S1 178.15(13) . . . . ?
C18 S8 C20 S9 -0.99(12) . . . . ?
C18 S8 C20 S10 -179.27(12) . . . . ?
C19 S9 C20 S8 2.09(12) . . . . ?
C19 S9 C20 S10 -179.61(12) . . . . ?
C17 S3 C15 S2 2.12(12) . . . . ?
C17 S3 C15 S1 -178.81(13) . . . . ?
C20 S8 C18 S6 179.57(11) . . . . ?
C20 S8 C18 C19 -0.96(16) . . . . ?
C20 S9 C19 S7 177.41(12) . . . . ?
C20 S9 C19 C18 -2.84(16) . . . . ?
C15 S2 C16 S4 -176.47(11) . . . . ?
C15 S2 C16 C17 2.60(16) . . . . ?
C15 S3 C17 S5 178.93(12) . . . . ?
C15 S3 C17 C16 -0.39(17) . . . . ?
C5 O2 C4 C3 -176.74(18) . . . . ?
C7 O3 C6 C5 172.53(15) . . . . ?
C6 O3 C7 C8 -179.72(16) . . . . ?
C3 O1 C14 C13 175.29(18) . . . . ?
C4 O2 C5 C6 -178.36(18) . . . . ?
C11 O5 C10 C9 169.19(19) . . . . ?
C8 O4 C9 C10 -171.12(18) . . . . ?
C13 O6 C12 C11 -175.30(16) . . . . ?
C12 O6 C13 C14 -177.11(17) . . . . ?
C14 O1 C3 C4 -176.66(17) . . . . ?
C9 O4 C8 C7 -170.90(18) . . . . ?
C10 O5 C11 C12 -178.9(2) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.032
_oxdiff_exptl_absorpt_empirical_full_min 0.703
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_173k
_database_code_depnum_ccdc_archive 'CCDC 2053286'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-19 downloaded from the CCDC.
;
_audit_creation_date             2020-11-25
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C12 H24 O6, C2 H7 F N'
_chemical_formula_sum            'C19.98 H31 F0.98 N Ni O6 S10'
_chemical_formula_weight         778.99
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHNOFNiS
_chemical_oxdiff_usercomment     20_20200608
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.4067(3)
_cell_length_b                   12.6314(5)
_cell_length_c                   12.9479(4)
_cell_angle_alpha                70.517(3)
_cell_angle_beta                 79.892(2)
_cell_angle_gamma                80.138(3)
_cell_volume                     1567.96(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    10325
_cell_measurement_temperature    173
_cell_measurement_theta_max      30.6760
_cell_measurement_theta_min      1.9910
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.327
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58251
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             805
_exptl_crystal_size_max          0.507
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.798
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19026
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.798
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.624
_diffrn_reflns_theta_min         1.996
_diffrn_ambient_temperature      173
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.798
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -17.00  28.00   0.50    0.21    --    5.18 -99.00 -30.00   90
  2  ω    -11.00  37.00   0.50    0.21    --    5.18 -99.00 -60.00   96
  3  ω    -62.00  15.00   0.50    0.21    --   -5.03 -77.00-150.00  154
  4  ω     -6.00  77.00   0.50    0.21    --    5.18  37.00  60.00  166
  5  ω    -11.00  78.00   0.50    0.21    --    5.18  77.00 120.00  178
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0021153000
_diffrn_orient_matrix_UB_12      0.0553914000
_diffrn_orient_matrix_UB_13      0.0028582000
_diffrn_orient_matrix_UB_21      -0.0112941000
_diffrn_orient_matrix_UB_22      -0.0211854000
_diffrn_orient_matrix_UB_23      0.0584779000
_diffrn_orient_matrix_UB_31      0.0687963000
_diffrn_orient_matrix_UB_32      -0.0091652000
_diffrn_orient_matrix_UB_33      0.0021173000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6118
_reflns_number_total             7718
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.364
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         7718
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0348
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0357P)²+0.0688P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0915
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
2. Rigid body (RIGU) restrains
 F1A, C2A, C1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(H1AA)=Sof(H1AB)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=1-FVAR(1)
 Sof(H1BC)=Sof(H1BD)=Sof(C2)=Sof(H2A)=Sof(H2B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C7(H7A,H7B), C6(H6A,H6B), C3(H3A,H3B), C4(H4A,H4B), C11(H11A,
 H11B), C8(H8A,H8B), C13(H13A,H13B), C12(H12A,H12B), C14(H14A,H14B), C1(H1BC,
 H1BD), C1(H1AA,H1AB), C9(H9A,H9B), C10(H10A,H10B), C2(H2A,H2B), C2A(H2AA,H2AB)
4.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.16462(2) 0.40691(2) 0.48931(2) 0.02114(8) Uani 1 1 d . . . . .
S2 S -0.07804(5) 0.26596(4) 0.29597(4) 0.02408(11) Uani 1 1 d . . . . .
S4 S 0.00955(5) 0.31340(4) 0.48640(4) 0.02407(11) Uani 1 1 d . . . . .
S6 S 0.10233(5) 0.36948(4) 0.66505(4) 0.02557(11) Uani 1 1 d . . . . .
S5 S 0.23017(5) 0.44179(4) 0.31411(4) 0.02622(11) Uani 1 1 d . . . . .
S8 S 0.19833(5) 0.43760(4) 0.83985(4) 0.02662(12) Uani 1 1 d . . . . .
S3 S 0.12920(5) 0.37770(5) 0.13902(4) 0.02851(12) Uani 1 1 d . . . . .
S9 S 0.40128(5) 0.55542(5) 0.68177(5) 0.02868(12) Uani 1 1 d . . . . .
S7 S 0.31426(5) 0.50575(4) 0.49195(4) 0.02663(12) Uani 1 1 d . . . . .
S10 S 0.37750(6) 0.54978(5) 0.91511(5) 0.03576(14) Uani 1 1 d . . . . .
S1 S -0.04953(6) 0.26478(5) 0.06368(5) 0.03633(14) Uani 1 1 d . . . . .
O2 O 0.16644(13) 0.89472(11) 0.28627(13) 0.0282(3) Uani 1 1 d . . . . .
O3 O 0.26712(13) 1.06442(12) 0.32895(12) 0.0294(3) Uani 1 1 d . . . . .
N1 N 0.44484(15) 0.89021(13) 0.25269(14) 0.0236(3) Uani 1 1 d . . . . .
H1A H 0.407164 0.877184 0.202191 0.028 Uiso 1 1 calc R U . . .
H1B H 0.514043 0.927108 0.219819 0.028 Uiso 1 1 calc R U . . .
H1C H 0.387199 0.931862 0.287287 0.028 Uiso 1 1 calc R U . . .
O5 O 0.68768(13) 0.97848(12) 0.13880(13) 0.0339(3) Uani 1 1 d . . . . .
O1 O 0.31536(13) 0.80808(11) 0.12207(12) 0.0292(3) Uani 1 1 d . . . . .
O6 O 0.58981(14) 0.81576(13) 0.07853(12) 0.0324(3) Uani 1 1 d . . . . .
O4 O 0.54347(14) 1.07173(12) 0.29537(14) 0.0336(3) Uani 1 1 d . . . . .
C16 C 0.02554(18) 0.32464(15) 0.34896(17) 0.0212(4) Uani 1 1 d . . . . .
C18 C 0.20644(18) 0.43743(16) 0.70410(16) 0.0231(4) Uani 1 1 d . . . . .
C19 C 0.29916(18) 0.49472(16) 0.62927(17) 0.0233(4) Uani 1 1 d . . . . .
C17 C 0.12155(18) 0.37839(16) 0.27471(17) 0.0229(4) Uani 1 1 d . . . . .
C20 C 0.32737(19) 0.51694(16) 0.81756(17) 0.0255(4) Uani 1 1 d . . . . .
C15 C -0.00141(19) 0.30075(17) 0.16075(17) 0.0261(4) Uani 1 1 d . . . . .
C5 C 0.08317(19) 0.98105(18) 0.32217(19) 0.0312(5) Uani 1 1 d . . . . .
H5A H 0.001940 0.952902 0.362965 0.037 Uiso 1 1 calc R U . . .
H5B H 0.061743 1.045534 0.258914 0.037 Uiso 1 1 calc R U . . .
C7 C 0.3320(2) 1.11475(18) 0.38637(19) 0.0305(5) Uani 1 1 d . . . . .
H7A H 0.360184 1.058182 0.452662 0.037 Uiso 1 1 calc R U . . .
H7B H 0.272235 1.173962 0.407743 0.037 Uiso 1 1 calc R U . . .
C6 C 0.1540(2) 1.01569(18) 0.39454(18) 0.0311(5) Uani 1 1 d . . . . .
H6A H 0.096939 1.070381 0.424724 0.037 Uiso 1 1 calc R U . . .
H6B H 0.180275 0.950371 0.455392 0.037 Uiso 1 1 calc R U . . .
C3 C 0.1982(2) 0.76446(17) 0.1855(2) 0.0322(5) Uani 1 1 d . . . . .
H3A H 0.219339 0.704853 0.252436 0.039 Uiso 1 1 calc R U . . .
H3B H 0.155777 0.733188 0.143176 0.039 Uiso 1 1 calc R U . . .
C4 C 0.1085(2) 0.85976(18) 0.21390(19) 0.0301(4) Uani 1 1 d . . . . .
H4A H 0.094850 0.922453 0.147239 0.036 Uiso 1 1 calc R U . . .
H4B H 0.023818 0.834979 0.249161 0.036 Uiso 1 1 calc R U . . .
C11 C 0.7708(2) 0.9017(2) 0.0891(2) 0.0379(5) Uani 1 1 d . . . . .
H11A H 0.799017 0.833156 0.145877 0.045 Uiso 1 1 calc R U . . .
H11B H 0.848290 0.935814 0.047047 0.045 Uiso 1 1 calc R U . . .
C8 C 0.4485(2) 1.16324(18) 0.3109(2) 0.0334(5) Uani 1 1 d . . . . .
H8A H 0.421950 1.211609 0.240419 0.040 Uiso 1 1 calc R U . . .
H8B H 0.486086 1.208290 0.342985 0.040 Uiso 1 1 calc R U . . .
C13 C 0.5195(2) 0.7781(2) 0.01451(19) 0.0364(5) Uani 1 1 d . . . . .
H13A H 0.577154 0.724329 -0.016526 0.044 Uiso 1 1 calc R U . . .
H13B H 0.489028 0.841933 -0.045881 0.044 Uiso 1 1 calc R U . . .
C12 C 0.6964(2) 0.8740(2) 0.0147(2) 0.0386(5) Uani 1 1 d . . . . .
H12A H 0.663686 0.943100 -0.039344 0.046 Uiso 1 1 calc R U . . .
H12B H 0.754146 0.827162 -0.024546 0.046 Uiso 1 1 calc R U . . .
C14 C 0.4054(2) 0.72385(19) 0.0863(2) 0.0367(5) Uani 1 1 d . . . . .
H14A H 0.362090 0.691406 0.045492 0.044 Uiso 1 1 calc R U . . .
H14B H 0.435056 0.663620 0.149737 0.044 Uiso 1 1 calc R U . . .
C1 C 0.4883(3) 0.78117(19) 0.3338(2) 0.0406(6) Uani 1 1 d . . . . .
H1BC H 0.420565 0.731522 0.351704 0.049 Uiso 0.819(7) 1 calc R U P A 2
H1BD H 0.567182 0.745494 0.300604 0.049 Uiso 0.819(7) 1 calc R U P A 2
H1AA H 0.474704 0.719808 0.309192 0.049 Uiso 0.181(7) 1 calc R U P A 1
H1AB H 0.581799 0.776558 0.336143 0.049 Uiso 0.181(7) 1 calc R U P A 1
C9 C 0.6658(2) 1.1090(2) 0.2389(2) 0.0390(5) Uani 1 1 d . . . . .
H9A H 0.708124 1.134780 0.285675 0.047 Uiso 1 1 calc R U . . .
H9B H 0.651532 1.171519 0.172232 0.047 Uiso 1 1 calc R U . . .
C10 C 0.7514(2) 1.0117(2) 0.2101(2) 0.0383(5) Uani 1 1 d . . . . .
H10A H 0.836548 1.034338 0.173420 0.046 Uiso 1 1 calc R U . . .
H10B H 0.764795 0.948834 0.276735 0.046 Uiso 1 1 calc R U . . .
C2 C 0.5155(3) 0.7943(2) 0.4363(2) 0.0374(9) Uani 0.819(7) 1 d . . P A 2
H2A H 0.548772 0.721489 0.484678 0.045 Uiso 0.819(7) 1 calc R U P A 2
H2B H 0.582188 0.844855 0.419216 0.045 Uiso 0.819(7) 1 calc R U P A 2
C2A C 0.424(2) 0.7672(12) 0.4374(12) 0.051(5) Uani 0.181(7) 1 d . . P A 1
H2AA H 0.338524 0.746948 0.436118 0.061 Uiso 0.181(7) 1 calc R U P A 1
H2AB H 0.470424 0.700242 0.484538 0.061 Uiso 0.181(7) 1 calc R U P A 1
F1A F 0.40174(18) 0.83785(15) 0.48907(13) 0.0706(6) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S4 2.1690(5) . ?
Ni1 S6 2.1659(6) . ?
Ni1 S5 2.1676(6) . ?
Ni1 S7 2.1675(5) . ?
S2 C16 1.7478(18) . ?
S2 C15 1.735(2) . ?
S4 C16 1.718(2) . ?
S6 C18 1.7223(19) . ?
S5 C17 1.7218(19) . ?
S8 C18 1.7456(19) . ?
S8 C20 1.739(2) . ?
S3 C17 1.748(2) . ?
S3 C15 1.734(2) . ?
S9 C19 1.7491(19) . ?
S9 C20 1.733(2) . ?
S7 C19 1.718(2) . ?
S10 C20 1.642(2) . ?
S1 C15 1.648(2) . ?
O2 C5 1.425(2) . ?
O2 C4 1.415(2) . ?
O3 C7 1.432(2) . ?
O3 C6 1.426(3) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.481(3) . ?
O5 C11 1.427(2) . ?
O5 C10 1.428(3) . ?
O1 C3 1.429(3) . ?
O1 C14 1.435(2) . ?
O6 C13 1.429(3) . ?
O6 C12 1.417(3) . ?
O4 C8 1.431(2) . ?
O4 C9 1.423(3) . ?
C16 C17 1.358(3) . ?
C18 C19 1.355(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.497(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.496(3) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.499(3) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.493(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.487(3) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C1 H1BC 0.9700 . ?
C1 H1BD 0.9700 . ?
C1 H1AA 0.9700 . ?
C1 H1AB 0.9700 . ?
C1 C2 1.471(4) . ?
C1 C2A 1.359(16) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.503(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 F1A 1.384(3) . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?
C2A F1A 1.253(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S6 Ni1 S4 86.95(2) . . ?
S6 Ni1 S5 178.88(2) . . ?
S6 Ni1 S7 92.77(2) . . ?
S5 Ni1 S4 93.29(2) . . ?
S7 Ni1 S4 177.90(2) . . ?
S7 Ni1 S5 87.04(2) . . ?
C15 S2 C16 97.60(10) . . ?
C16 S4 Ni1 101.77(7) . . ?
C18 S6 Ni1 102.48(7) . . ?
C17 S5 Ni1 101.97(7) . . ?
C20 S8 C18 97.07(10) . . ?
C15 S3 C17 97.33(10) . . ?
C20 S9 C19 97.42(10) . . ?
C19 S7 Ni1 102.33(7) . . ?
C4 O2 C5 112.08(14) . . ?
C6 O3 C7 112.42(16) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
C11 O5 C10 113.09(16) . . ?
C3 O1 C14 112.21(16) . . ?
C12 O6 C13 112.84(17) . . ?
C9 O4 C8 112.13(16) . . ?
S4 C16 S2 122.51(12) . . ?
C17 C16 S2 115.69(15) . . ?
C17 C16 S4 121.79(15) . . ?
S6 C18 S8 122.55(12) . . ?
C19 C18 S6 120.90(15) . . ?
C19 C18 S8 116.55(15) . . ?
S7 C19 S9 122.74(12) . . ?
C18 C19 S9 115.78(15) . . ?
C18 C19 S7 121.48(15) . . ?
S5 C17 S3 122.49(12) . . ?
C16 C17 S5 121.14(15) . . ?
C16 C17 S3 116.37(15) . . ?
S9 C20 S8 113.13(11) . . ?
S10 C20 S8 123.86(13) . . ?
S10 C20 S9 122.99(13) . . ?
S3 C15 S2 112.94(11) . . ?
S1 C15 S2 123.07(13) . . ?
S1 C15 S3 123.99(13) . . ?
O2 C5 H5A 110.0 . . ?
O2 C5 H5B 110.0 . . ?
O2 C5 C6 108.40(15) . . ?
H5A C5 H5B 108.4 . . ?
C6 C5 H5A 110.0 . . ?
C6 C5 H5B 110.0 . . ?
O3 C7 H7A 110.0 . . ?
O3 C7 H7B 110.0 . . ?
O3 C7 C8 108.24(17) . . ?
H7A C7 H7B 108.4 . . ?
C8 C7 H7A 110.0 . . ?
C8 C7 H7B 110.0 . . ?
O3 C6 C5 108.00(17) . . ?
O3 C6 H6A 110.1 . . ?
O3 C6 H6B 110.1 . . ?
C5 C6 H6A 110.1 . . ?
C5 C6 H6B 110.1 . . ?
H6A C6 H6B 108.4 . . ?
O1 C3 H3A 110.1 . . ?
O1 C3 H3B 110.1 . . ?
O1 C3 C4 108.03(16) . . ?
H3A C3 H3B 108.4 . . ?
C4 C3 H3A 110.1 . . ?
C4 C3 H3B 110.1 . . ?
O2 C4 C3 108.77(16) . . ?
O2 C4 H4A 109.9 . . ?
O2 C4 H4B 109.9 . . ?
C3 C4 H4A 109.9 . . ?
C3 C4 H4B 109.9 . . ?
H4A C4 H4B 108.3 . . ?
O5 C11 H11A 109.9 . . ?
O5 C11 H11B 109.9 . . ?
O5 C11 C12 109.03(17) . . ?
H11A C11 H11B 108.3 . . ?
C12 C11 H11A 109.9 . . ?
C12 C11 H11B 109.9 . . ?
O4 C8 C7 108.35(17) . . ?
O4 C8 H8A 110.0 . . ?
O4 C8 H8B 110.0 . . ?
C7 C8 H8A 110.0 . . ?
C7 C8 H8B 110.0 . . ?
H8A C8 H8B 108.4 . . ?
O6 C13 H13A 109.8 . . ?
O6 C13 H13B 109.8 . . ?
O6 C13 C14 109.31(18) . . ?
H13A C13 H13B 108.3 . . ?
C14 C13 H13A 109.8 . . ?
C14 C13 H13B 109.8 . . ?
O6 C12 C11 109.27(19) . . ?
O6 C12 H12A 109.8 . . ?
O6 C12 H12B 109.8 . . ?
C11 C12 H12A 109.8 . . ?
C11 C12 H12B 109.8 . . ?
H12A C12 H12B 108.3 . . ?
O1 C14 C13 108.63(17) . . ?
O1 C14 H14A 110.0 . . ?
O1 C14 H14B 110.0 . . ?
C13 C14 H14A 110.0 . . ?
C13 C14 H14B 110.0 . . ?
H14A C14 H14B 108.3 . . ?
N1 C1 H1BC 109.0 . . ?
N1 C1 H1BD 109.0 . . ?
N1 C1 H1AA 108.9 . . ?
N1 C1 H1AB 108.9 . . ?
H1BC C1 H1BD 107.8 . . ?
H1AA C1 H1AB 107.7 . . ?
C2 C1 N1 112.84(19) . . ?
C2 C1 H1BC 109.0 . . ?
C2 C1 H1BD 109.0 . . ?
C2A C1 N1 113.4(5) . . ?
C2A C1 H1AA 108.9 . . ?
C2A C1 H1AB 108.9 . . ?
O4 C9 H9A 110.0 . . ?
O4 C9 H9B 110.0 . . ?
O4 C9 C10 108.41(18) . . ?
H9A C9 H9B 108.4 . . ?
C10 C9 H9A 110.0 . . ?
C10 C9 H9B 110.0 . . ?
O5 C10 C9 108.31(16) . . ?
O5 C10 H10A 110.0 . . ?
O5 C10 H10B 110.0 . . ?
C9 C10 H10A 110.0 . . ?
C9 C10 H10B 110.0 . . ?
H10A C10 H10B 108.4 . . ?
C1 C2 H2A 109.7 . . ?
C1 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
F1A C2 C1 109.9(3) . . ?
F1A C2 H2A 109.7 . . ?
F1A C2 H2B 109.7 . . ?
C1 C2A H2AA 105.6 . . ?
C1 C2A H2AB 105.6 . . ?
H2AA C2A H2AB 106.1 . . ?
F1A C2A C1 127.0(15) . . ?
F1A C2A H2AA 105.6 . . ?
F1A C2A H2AB 105.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S4 C16 S2 -178.86(9) . . . . ?
Ni1 S4 C16 C17 2.29(16) . . . . ?
Ni1 S6 C18 S8 178.88(9) . . . . ?
Ni1 S6 C18 C19 -0.64(16) . . . . ?
Ni1 S5 C17 S3 -178.99(9) . . . . ?
Ni1 S5 C17 C16 0.20(16) . . . . ?
Ni1 S7 C19 S9 177.80(9) . . . . ?
Ni1 S7 C19 C18 -1.99(16) . . . . ?
S2 C16 C17 S5 179.29(9) . . . . ?
S2 C16 C17 S3 -1.5(2) . . . . ?
S4 C16 C17 S5 -1.8(2) . . . . ?
S4 C16 C17 S3 177.45(9) . . . . ?
S6 C18 C19 S9 -177.93(9) . . . . ?
S6 C18 C19 S7 1.9(2) . . . . ?
S8 C18 C19 S9 2.5(2) . . . . ?
S8 C18 C19 S7 -177.67(10) . . . . ?
O2 C5 C6 O3 64.1(2) . . . . ?
O3 C7 C8 O4 -68.8(2) . . . . ?
N1 C1 C2 F1A 62.9(3) . . . . ?
N1 C1 C2A F1A -47(2) . . . . ?
O5 C11 C12 O6 -64.4(2) . . . . ?
O1 C3 C4 O2 -66.6(2) . . . . ?
O6 C13 C14 O1 65.2(2) . . . . ?
O4 C9 C10 O5 61.4(3) . . . . ?
C16 S2 C15 S3 -2.48(12) . . . . ?
C16 S2 C15 S1 177.99(12) . . . . ?
C18 S8 C20 S9 -0.73(12) . . . . ?
C18 S8 C20 S10 -179.22(12) . . . . ?
C19 S9 C20 S8 1.80(11) . . . . ?
C19 S9 C20 S10 -179.70(12) . . . . ?
C17 S3 C15 S2 1.84(12) . . . . ?
C17 S3 C15 S1 -178.63(13) . . . . ?
C20 S8 C18 S6 179.38(11) . . . . ?
C20 S8 C18 C19 -1.08(16) . . . . ?
C20 S9 C19 S7 177.57(12) . . . . ?
C20 S9 C19 C18 -2.62(16) . . . . ?
C15 S2 C16 S4 -176.50(11) . . . . ?
C15 S2 C16 C17 2.41(16) . . . . ?
C15 S3 C17 S5 178.98(12) . . . . ?
C15 S3 C17 C16 -0.24(16) . . . . ?
C5 O2 C4 C3 -176.61(18) . . . . ?
C7 O3 C6 C5 171.85(15) . . . . ?
C6 O3 C7 C8 -179.94(15) . . . . ?
C3 O1 C14 C13 176.00(17) . . . . ?
C4 O2 C5 C6 -177.90(18) . . . . ?
C11 O5 C10 C9 168.6(2) . . . . ?
C8 O4 C9 C10 -170.97(18) . . . . ?
C13 O6 C12 C11 -175.33(16) . . . . ?
C12 O6 C13 C14 -176.84(16) . . . . ?
C14 O1 C3 C4 -177.23(17) . . . . ?
C9 O4 C8 C7 -170.75(18) . . . . ?
C10 O5 C11 C12 -178.9(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.816
_oxdiff_exptl_absorpt_empirical_full_min 0.598
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_273k
_database_code_depnum_ccdc_archive 'CCDC 2053291'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-19 downloaded from the CCDC.
;
_audit_creation_date             2020-11-11
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C12 H24 O6, C2 H7 F N'
_chemical_formula_sum            'C20 H31 F N Ni O6 S10'
_chemical_formula_weight         779.77
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHNOFNiS
_chemical_oxdiff_usercomment     20_20200608
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.4883(2)
_cell_length_b                   12.6467(3)
_cell_length_c                   12.9675(3)
_cell_angle_alpha                71.543(2)
_cell_angle_beta                 79.792(2)
_cell_angle_gamma                80.656(2)
_cell_volume                     1595.30(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    17792
_cell_measurement_temperature    273
_cell_measurement_theta_max      30.3050
_cell_measurement_theta_min      1.9890
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.305
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56941
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             806
_exptl_crystal_size_max          0.507
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.835
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            39570
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.835
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.945
_diffrn_reflns_theta_min         1.986
_diffrn_ambient_temperature      273
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.835
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -55.00  18.00   0.50    0.34    --    5.18 -29.00 -14.39  146
  2  ω    -58.00  19.00   0.50    0.34    --    5.18 -28.00  42.06  154
  3  ω    -46.00  17.00   0.50    0.34    --    5.18 -19.00  90.00  126
  4  ω    -66.00 -40.00   0.50    0.34    --    5.18 -19.00 120.00   52
  5  ω    -19.00  18.00   0.50    0.34    --    5.18 -19.00 120.00   74
  6  ω    -35.00  19.00   0.50    0.34    --    5.18 -28.00 -54.63  108
  7  ω    -68.00  18.00   0.50    0.34    --    5.18 -37.00 -90.00  172
  8  ω    -59.00  19.00   0.50    0.34    --    5.18 -33.00-168.36  156
  9  ω    -17.00  24.00   0.50    0.34    --   -5.03 -99.00  90.00   82
 10  ω    -13.00  23.00   0.50    0.34    --   -5.03 -99.00 150.00   72
 11  ω    -17.00  28.00   0.50    0.34    --   -5.03 -99.00   0.00   90
 12  ω    -17.00  27.00   0.50    0.34    --   -5.03 -99.00 -60.00   88
 13  ω    -18.00  22.00   0.50    0.34    --   -5.03 -99.00-150.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0023778000
_diffrn_orient_matrix_UB_12      0.0546581000
_diffrn_orient_matrix_UB_13      0.0047574000
_diffrn_orient_matrix_UB_21      -0.0104443000
_diffrn_orient_matrix_UB_22      -0.0220259000
_diffrn_orient_matrix_UB_23      0.0579872000
_diffrn_orient_matrix_UB_31      0.0683301000
_diffrn_orient_matrix_UB_32      -0.0083211000
_diffrn_orient_matrix_UB_33      0.0011111000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6037
_reflns_number_total             8451
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.870
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         8451
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0357
_refine_ls_restrained_S_all      0.870
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1327
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
2. Others
 Sof(H1AA)=Sof(H1AB)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(F1)=1-FVAR(1)
 Sof(H1BC)=Sof(H1BD)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(F1A)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C7(H7A,H7B), C6(H6A,H6B), C3(H3A,H3B), C4(H4A,H4B), C11(H11A,
 H11B), C8(H8A,H8B), C13(H13A,H13B), C12(H12A,H12B), C14(H14A,H14B), C1(H1BC,
 H1BD), C1(H1AA,H1AB), C9(H9A,H9B), C10(H10A,H10B), C2(H2A,H2B), C2A(H2AA,H2AB)
3.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.16314(2) 0.40456(2) 0.49198(2) 0.03688(10) Uani 1 1 d . . . . .
S2 S -0.07959(5) 0.26667(4) 0.29637(5) 0.04238(13) Uani 1 1 d . . . . .
S4 S 0.00639(5) 0.31446(4) 0.48689(5) 0.04177(13) Uani 1 1 d . . . . .
S6 S 0.09995(5) 0.36910(4) 0.66647(5) 0.04431(14) Uani 1 1 d . . . . .
S5 S 0.22908(5) 0.43863(5) 0.31789(5) 0.04483(14) Uani 1 1 d . . . . .
S8 S 0.19581(5) 0.43701(5) 0.84130(5) 0.04625(14) Uani 1 1 d . . . . .
S3 S 0.12881(5) 0.37482(5) 0.14247(5) 0.04908(15) Uani 1 1 d . . . . .
S9 S 0.40165(5) 0.54869(5) 0.68680(5) 0.04983(15) Uani 1 1 d . . . . .
S7 S 0.31609(5) 0.49843(5) 0.49666(5) 0.04786(15) Uani 1 1 d . . . . .
S10 S 0.37506(7) 0.54710(6) 0.91820(6) 0.06168(18) Uani 1 1 d . . . . .
S1 S -0.04924(6) 0.26367(7) 0.06511(6) 0.06269(18) Uani 1 1 d . . . . .
O2 O 0.16933(13) 0.89611(12) 0.28397(15) 0.0510(4) Uani 1 1 d . . . . .
O3 O 0.26760(15) 1.06503(13) 0.32997(14) 0.0524(4) Uani 1 1 d . . . . .
N1 N 0.44701(15) 0.89075(13) 0.25415(15) 0.0404(4) Uani 1 1 d . . . . .
H1A H 0.409922 0.876044 0.204322 0.048 Uiso 1 1 calc R U . . .
H1B H 0.515034 0.928369 0.221012 0.048 Uiso 1 1 calc R U . . .
H1C H 0.389351 0.931926 0.289079 0.048 Uiso 1 1 calc R U . . .
O5 O 0.68689(14) 0.98047(14) 0.14058(16) 0.0603(4) Uani 1 1 d . . . . .
O1 O 0.31866(16) 0.80812(13) 0.12206(15) 0.0544(4) Uani 1 1 d . . . . .
O6 O 0.58988(16) 0.81824(15) 0.07790(15) 0.0594(4) Uani 1 1 d . . . . .
O4 O 0.54068(15) 1.07289(13) 0.29813(16) 0.0582(4) Uani 1 1 d . . . . .
C16 C 0.02354(18) 0.32460(16) 0.35050(18) 0.0379(4) Uani 1 1 d . . . . .
C18 C 0.20467(19) 0.43507(16) 0.70655(18) 0.0381(4) Uani 1 1 d . . . . .
C19 C 0.29974(18) 0.48977(17) 0.63274(19) 0.0406(4) Uani 1 1 d . . . . .
C17 C 0.12050(19) 0.37649(17) 0.27746(18) 0.0391(4) Uani 1 1 d . . . . .
C20 C 0.3257(2) 0.51360(18) 0.8202(2) 0.0445(5) Uani 1 1 d . . . . .
C15 C -0.00150(19) 0.29937(18) 0.16288(19) 0.0443(5) Uani 1 1 d . . . . .
C5 C 0.0868(2) 0.9819(2) 0.3198(2) 0.0575(6) Uani 1 1 d . . . . .
H5A H 0.005392 0.954147 0.359059 0.069 Uiso 1 1 calc R U . . .
H5B H 0.067127 1.045375 0.257042 0.069 Uiso 1 1 calc R U . . .
C7 C 0.3312(3) 1.1151(2) 0.3886(2) 0.0581(6) Uani 1 1 d . . . . .
H7A H 0.358017 1.059176 0.454104 0.070 Uiso 1 1 calc R U . . .
H7B H 0.272095 1.173976 0.410455 0.070 Uiso 1 1 calc R U . . .
C6 C 0.1540(2) 1.0174(2) 0.3931(2) 0.0582(6) Uani 1 1 d . . . . .
H6A H 0.096647 1.072362 0.422529 0.070 Uiso 1 1 calc R U . . .
H6B H 0.177988 0.953347 0.453830 0.070 Uiso 1 1 calc R U . . .
C3 C 0.2009(2) 0.7653(2) 0.1840(2) 0.0606(6) Uani 1 1 d . . . . .
H3A H 0.220347 0.706535 0.250274 0.073 Uiso 1 1 calc R U . . .
H3B H 0.159592 0.733712 0.140940 0.073 Uiso 1 1 calc R U . . .
C4 C 0.1120(2) 0.8591(2) 0.2127(2) 0.0564(6) Uani 1 1 d . . . . .
H4A H 0.098037 0.920267 0.146664 0.068 Uiso 1 1 calc R U . . .
H4B H 0.028242 0.833817 0.248309 0.068 Uiso 1 1 calc R U . . .
C11 C 0.7696(2) 0.9030(2) 0.0909(3) 0.0701(8) Uani 1 1 d . . . . .
H11A H 0.796406 0.835459 0.147115 0.084 Uiso 1 1 calc R U . . .
H11B H 0.847059 0.936342 0.049362 0.084 Uiso 1 1 calc R U . . .
C8 C 0.4471(3) 1.1626(2) 0.3152(3) 0.0602(6) Uani 1 1 d . . . . .
H8A H 0.421715 1.210714 0.245539 0.072 Uiso 1 1 calc R U . . .
H8B H 0.484197 1.207316 0.348365 0.072 Uiso 1 1 calc R U . . .
C13 C 0.5190(3) 0.7803(2) 0.0139(2) 0.0683(8) Uani 1 1 d . . . . .
H13A H 0.575602 0.726985 -0.018166 0.082 Uiso 1 1 calc R U . . .
H13B H 0.488861 0.843442 -0.045173 0.082 Uiso 1 1 calc R U . . .
C12 C 0.6958(3) 0.8749(3) 0.0168(2) 0.0703(7) Uani 1 1 d . . . . .
H12A H 0.664543 0.943181 -0.036458 0.084 Uiso 1 1 calc R U . . .
H12B H 0.752881 0.827990 -0.022685 0.084 Uiso 1 1 calc R U . . .
C14 C 0.4060(3) 0.7265(2) 0.0850(3) 0.0682(7) Uani 1 1 d . . . . .
H14A H 0.362712 0.694050 0.044102 0.082 Uiso 1 1 calc R U . . .
H14B H 0.435436 0.666915 0.147205 0.082 Uiso 1 1 calc R U . . .
C1 C 0.4915(3) 0.7840(2) 0.3342(2) 0.0711(8) Uani 1 1 d . . . . .
H1BC H 0.428316 0.731578 0.346950 0.085 Uiso 0.600(9) 1 calc R U P A 2
H1BD H 0.573456 0.752517 0.301688 0.085 Uiso 0.600(9) 1 calc R U P A 2
H1AA H 0.493437 0.723131 0.303270 0.085 Uiso 0.400(9) 1 calc R U P A 1
H1AB H 0.580039 0.786987 0.344637 0.085 Uiso 0.400(9) 1 calc R U P A 1
C9 C 0.6616(2) 1.1105(2) 0.2423(3) 0.0698(8) Uani 1 1 d . . . . .
H9A H 0.702886 1.137367 0.289037 0.084 Uiso 1 1 calc R U . . .
H9B H 0.647595 1.171801 0.176409 0.084 Uiso 1 1 calc R U . . .
C10 C 0.7471(2) 1.0146(2) 0.2130(3) 0.0704(8) Uani 1 1 d . . . . .
H10A H 0.831946 1.037540 0.177756 0.085 Uiso 1 1 calc R U . . .
H10B H 0.759145 0.952598 0.278777 0.085 Uiso 1 1 calc R U . . .
C2 C 0.5091(6) 0.7930(4) 0.4355(4) 0.0683(18) Uani 0.600(9) 1 d . . P A 2
H2A H 0.559725 0.854119 0.425371 0.082 Uiso 0.600(9) 1 calc R U P A 2
H2B H 0.553394 0.723917 0.478389 0.082 Uiso 0.600(9) 1 calc R U P A 2
C2A C 0.4153(9) 0.7600(6) 0.4352(6) 0.062(2) Uani 0.400(9) 1 d . . P A 1
H2AA H 0.451299 0.689598 0.482708 0.075 Uiso 0.400(9) 1 calc R U P A 1
H2AB H 0.327962 0.751396 0.426369 0.075 Uiso 0.400(9) 1 calc R U P A 1
F1A F 0.4087(11) 0.8472(8) 0.4855(8) 0.088(2) Uani 0.600(9) 1 d . . P A 1
F1 F 0.3743(16) 0.8155(12) 0.4903(13) 0.085(3) Uani 0.400(9) 1 d . . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S4 2.1680(5) . ?
Ni1 S6 2.1640(6) . ?
Ni1 S5 2.1651(6) . ?
Ni1 S7 2.1645(5) . ?
S2 C16 1.7468(19) . ?
S2 C15 1.730(2) . ?
S4 C16 1.711(2) . ?
S6 C18 1.717(2) . ?
S5 C17 1.718(2) . ?
S8 C18 1.741(2) . ?
S8 C20 1.731(2) . ?
S3 C17 1.744(2) . ?
S3 C15 1.727(2) . ?
S9 C19 1.7448(19) . ?
S9 C20 1.722(3) . ?
S7 C19 1.712(2) . ?
S10 C20 1.645(2) . ?
S1 C15 1.650(2) . ?
O2 C5 1.419(3) . ?
O2 C4 1.414(3) . ?
O3 C7 1.430(3) . ?
O3 C6 1.424(3) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.482(3) . ?
O5 C11 1.432(3) . ?
O5 C10 1.422(3) . ?
O1 C3 1.434(3) . ?
O1 C14 1.409(3) . ?
O6 C13 1.434(3) . ?
O6 C12 1.400(3) . ?
O4 C8 1.422(3) . ?
O4 C9 1.418(3) . ?
C16 C17 1.358(3) . ?
C18 C19 1.362(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.488(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.486(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.487(3) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.489(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.482(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C1 H1BC 0.9700 . ?
C1 H1BD 0.9700 . ?
C1 H1AA 0.9700 . ?
C1 H1AB 0.9700 . ?
C1 C2 1.400(6) . ?
C1 C2A 1.380(9) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.496(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 F1 1.492(18) . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?
C2A F1A 1.436(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S6 Ni1 S4 87.12(2) . . ?
S6 Ni1 S5 179.17(2) . . ?
S6 Ni1 S7 92.75(2) . . ?
S5 Ni1 S4 93.26(2) . . ?
S7 Ni1 S4 178.51(2) . . ?
S7 Ni1 S5 86.88(2) . . ?
C15 S2 C16 97.53(10) . . ?
C16 S4 Ni1 101.75(7) . . ?
C18 S6 Ni1 102.55(8) . . ?
C17 S5 Ni1 101.96(8) . . ?
C20 S8 C18 97.05(11) . . ?
C15 S3 C17 97.32(10) . . ?
C20 S9 C19 97.57(11) . . ?
C19 S7 Ni1 102.49(7) . . ?
C4 O2 C5 111.98(16) . . ?
C6 O3 C7 112.7(2) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
C10 O5 C11 113.96(19) . . ?
C14 O1 C3 112.60(19) . . ?
C12 O6 C13 113.8(2) . . ?
C9 O4 C8 112.10(19) . . ?
S4 C16 S2 122.53(13) . . ?
C17 C16 S2 115.56(17) . . ?
C17 C16 S4 121.90(15) . . ?
S6 C18 S8 122.72(13) . . ?
C19 C18 S6 120.87(16) . . ?
C19 C18 S8 116.42(15) . . ?
S7 C19 S9 123.23(13) . . ?
C18 C19 S9 115.45(17) . . ?
C18 C19 S7 121.32(15) . . ?
S5 C17 S3 122.55(13) . . ?
C16 C17 S5 121.10(17) . . ?
C16 C17 S3 116.35(15) . . ?
S9 C20 S8 113.45(12) . . ?
S10 C20 S8 123.63(15) . . ?
S10 C20 S9 122.90(14) . . ?
S3 C15 S2 113.16(12) . . ?
S1 C15 S2 123.01(13) . . ?
S1 C15 S3 123.81(14) . . ?
O2 C5 H5A 109.9 . . ?
O2 C5 H5B 109.9 . . ?
O2 C5 C6 108.91(18) . . ?
H5A C5 H5B 108.3 . . ?
C6 C5 H5A 109.9 . . ?
C6 C5 H5B 109.9 . . ?
O3 C7 H7A 110.1 . . ?
O3 C7 H7B 110.1 . . ?
O3 C7 C8 108.2(2) . . ?
H7A C7 H7B 108.4 . . ?
C8 C7 H7A 110.1 . . ?
C8 C7 H7B 110.1 . . ?
O3 C6 C5 107.9(2) . . ?
O3 C6 H6A 110.1 . . ?
O3 C6 H6B 110.1 . . ?
C5 C6 H6A 110.1 . . ?
C5 C6 H6B 110.1 . . ?
H6A C6 H6B 108.4 . . ?
O1 C3 H3A 110.0 . . ?
O1 C3 H3B 110.0 . . ?
O1 C3 C4 108.45(18) . . ?
H3A C3 H3B 108.4 . . ?
C4 C3 H3A 110.0 . . ?
C4 C3 H3B 110.0 . . ?
O2 C4 C3 108.67(18) . . ?
O2 C4 H4A 110.0 . . ?
O2 C4 H4B 110.0 . . ?
C3 C4 H4A 110.0 . . ?
C3 C4 H4B 110.0 . . ?
H4A C4 H4B 108.3 . . ?
O5 C11 H11A 110.0 . . ?
O5 C11 H11B 110.0 . . ?
O5 C11 C12 108.61(19) . . ?
H11A C11 H11B 108.3 . . ?
C12 C11 H11A 110.0 . . ?
C12 C11 H11B 110.0 . . ?
O4 C8 C7 108.8(2) . . ?
O4 C8 H8A 109.9 . . ?
O4 C8 H8B 109.9 . . ?
C7 C8 H8A 109.9 . . ?
C7 C8 H8B 109.9 . . ?
H8A C8 H8B 108.3 . . ?
O6 C13 H13A 109.8 . . ?
O6 C13 H13B 109.8 . . ?
O6 C13 C14 109.5(2) . . ?
H13A C13 H13B 108.2 . . ?
C14 C13 H13A 109.8 . . ?
C14 C13 H13B 109.8 . . ?
O6 C12 C11 110.1(2) . . ?
O6 C12 H12A 109.6 . . ?
O6 C12 H12B 109.6 . . ?
C11 C12 H12A 109.6 . . ?
C11 C12 H12B 109.6 . . ?
H12A C12 H12B 108.2 . . ?
O1 C14 C13 108.9(2) . . ?
O1 C14 H14A 109.9 . . ?
O1 C14 H14B 109.9 . . ?
C13 C14 H14A 109.9 . . ?
C13 C14 H14B 109.9 . . ?
H14A C14 H14B 108.3 . . ?
N1 C1 H1BC 108.5 . . ?
N1 C1 H1BD 108.5 . . ?
N1 C1 H1AA 108.6 . . ?
N1 C1 H1AB 108.6 . . ?
H1BC C1 H1BD 107.5 . . ?
H1AA C1 H1AB 107.6 . . ?
C2 C1 N1 115.2(3) . . ?
C2 C1 H1BC 108.5 . . ?
C2 C1 H1BD 108.5 . . ?
C2A C1 N1 114.5(4) . . ?
C2A C1 H1AA 108.6 . . ?
C2A C1 H1AB 108.6 . . ?
O4 C9 H9A 110.0 . . ?
O4 C9 H9B 110.0 . . ?
O4 C9 C10 108.6(2) . . ?
H9A C9 H9B 108.4 . . ?
C10 C9 H9A 110.0 . . ?
C10 C9 H9B 110.0 . . ?
O5 C10 C9 108.69(19) . . ?
O5 C10 H10A 110.0 . . ?
O5 C10 H10B 110.0 . . ?
C9 C10 H10A 110.0 . . ?
C9 C10 H10B 110.0 . . ?
H10A C10 H10B 108.3 . . ?
C1 C2 H2A 110.8 . . ?
C1 C2 H2B 110.8 . . ?
C1 C2 F1 104.6(7) . . ?
H2A C2 H2B 108.9 . . ?
F1 C2 H2A 110.8 . . ?
F1 C2 H2B 110.8 . . ?
C1 C2A H2AA 109.4 . . ?
C1 C2A H2AB 109.4 . . ?
C1 C2A F1A 111.3(6) . . ?
H2AA C2A H2AB 108.0 . . ?
F1A C2A H2AA 109.4 . . ?
F1A C2A H2AB 109.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S4 C16 S2 -179.54(10) . . . . ?
Ni1 S4 C16 C17 1.88(18) . . . . ?
Ni1 S6 C18 S8 178.39(10) . . . . ?
Ni1 S6 C18 C19 -1.25(18) . . . . ?
Ni1 S5 C17 S3 -178.57(11) . . . . ?
Ni1 S5 C17 C16 0.74(18) . . . . ?
Ni1 S7 C19 S9 178.51(11) . . . . ?
Ni1 S7 C19 C18 -1.31(18) . . . . ?
S2 C16 C17 S5 179.45(10) . . . . ?
S2 C16 C17 S3 -1.2(2) . . . . ?
S4 C16 C17 S5 -1.9(3) . . . . ?
S4 C16 C17 S3 177.47(10) . . . . ?
S6 C18 C19 S9 -178.00(10) . . . . ?
S6 C18 C19 S7 1.8(2) . . . . ?
S8 C18 C19 S9 2.3(2) . . . . ?
S8 C18 C19 S7 -177.84(11) . . . . ?
O2 C5 C6 O3 63.8(3) . . . . ?
O3 C7 C8 O4 -68.5(3) . . . . ?
N1 C1 C2 F1 71.2(7) . . . . ?
N1 C1 C2A F1A -58.5(8) . . . . ?
O5 C11 C12 O6 -64.6(3) . . . . ?
O1 C3 C4 O2 -65.2(3) . . . . ?
O6 C13 C14 O1 65.2(3) . . . . ?
O4 C9 C10 O5 62.3(3) . . . . ?
C16 S2 C15 S3 -2.74(13) . . . . ?
C16 S2 C15 S1 178.32(14) . . . . ?
C18 S8 C20 S9 -1.07(13) . . . . ?
C18 S8 C20 S10 -179.50(13) . . . . ?
C19 S9 C20 S8 2.07(13) . . . . ?
C19 S9 C20 S10 -179.48(13) . . . . ?
C17 S3 C15 S2 2.22(13) . . . . ?
C17 S3 C15 S1 -178.85(14) . . . . ?
C20 S8 C18 S6 179.57(12) . . . . ?
C20 S8 C18 C19 -0.77(17) . . . . ?
C20 S9 C19 S7 177.51(13) . . . . ?
C20 S9 C19 C18 -2.66(18) . . . . ?
C15 S2 C16 S4 -176.26(13) . . . . ?
C15 S2 C16 C17 2.40(17) . . . . ?
C15 S3 C17 S5 178.71(13) . . . . ?
C15 S3 C17 C16 -0.63(18) . . . . ?
C5 O2 C4 C3 -176.8(2) . . . . ?
C7 O3 C6 C5 172.57(18) . . . . ?
C6 O3 C7 C8 -179.53(18) . . . . ?
C3 O1 C14 C13 175.0(2) . . . . ?
C4 O2 C5 C6 -179.3(2) . . . . ?
C11 O5 C10 C9 169.3(2) . . . . ?
C8 O4 C9 C10 -171.6(2) . . . . ?
C13 O6 C12 C11 -175.52(19) . . . . ?
C12 O6 C13 C14 -177.4(2) . . . . ?
C14 O1 C3 C4 -176.2(2) . . . . ?
C9 O4 C8 C7 -171.3(2) . . . . ?
C10 O5 C11 C12 -179.5(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.050
_oxdiff_exptl_absorpt_empirical_full_min 0.385
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_93k
_database_code_depnum_ccdc_archive 'CCDC 2053282'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-19 downloaded from the CCDC.
;
_audit_creation_date             2020-11-11
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C12 H24 O6, C2 H7 F N'
_chemical_formula_sum            'C20 H31 F N Ni O6 S10'
_chemical_formula_weight         779.77
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHNOFNiS
_chemical_oxdiff_usercomment     20_20200608
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.3645(3)
_cell_length_b                   12.6254(5)
_cell_length_c                   12.9123(4)
_cell_angle_alpha                69.835(3)
_cell_angle_beta                 79.972(3)
_cell_angle_gamma                79.948(3)
_cell_volume                     1549.82(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    10163
_cell_measurement_temperature    93
_cell_measurement_theta_max      30.8130
_cell_measurement_theta_min      1.9900
_shelx_estimated_absorpt_T_max   0.889
_shelx_estimated_absorpt_T_min   0.549
_exptl_absorpt_coefficient_mu    1.343
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34916
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             806
_exptl_crystal_size_max          0.507
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.779
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18605
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.779
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.993
_diffrn_reflns_theta_min         1.991
_diffrn_ambient_temperature      93
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.779
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00  73.00   0.50    0.15    --    5.18  57.00 150.00  146
  2  ω     -8.00  75.00   0.50    0.15    --    5.18  57.00  30.00  166
  3  ω     -6.00  78.00   0.50    0.15    --    5.18  37.00 -60.00  168
  4  ω    -10.00  32.00   0.50    0.15    --    5.18 -99.00-180.00   84
  5  ω     -6.00  25.00   0.50    0.15    --    5.18 -99.00  30.00   62
  6  ω     -6.00  20.00   0.50    0.15    --   -5.03 -99.00   0.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0010285000
_diffrn_orient_matrix_UB_12      0.0563204000
_diffrn_orient_matrix_UB_13      0.0000029000
_diffrn_orient_matrix_UB_21      -0.0116157000
_diffrn_orient_matrix_UB_22      -0.0191445000
_diffrn_orient_matrix_UB_23      0.0589143000
_diffrn_orient_matrix_UB_31      0.0690590000
_diffrn_orient_matrix_UB_32      -0.0099586000
_diffrn_orient_matrix_UB_33      0.0025355000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6292
_reflns_number_total             7679
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.782
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         7679
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0329
_refine_ls_restrained_S_all      0.782
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1117
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C8(H8A,H8B), C6(H6A,H6B), C14(H14A,H14B), C7(H7A,H7B), C9(H9A,
 H9B), C11(H11A,H11B), C5(H5A,H5B), C12(H12A,H12B), C13(H13A,H13B), C2(H2A,H2B),
  C3(H3A,H3B), C4(H4A,H4B), C1(H1D,H1E)
2.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.16547(2) 0.90814(2) 0.48778(2) 0.01220(8) Uani 1 1 d . . . . .
S8 S -0.07739(4) 0.76566(4) 0.29562(4) 0.01401(11) Uani 1 1 d . . . . .
S4 S 0.10338(5) 0.87005(4) 0.66458(4) 0.01494(11) Uani 1 1 d . . . . .
S2 S 0.19962(5) 0.93848(4) 0.83945(4) 0.01503(11) Uani 1 1 d . . . . .
S7 S 0.23100(5) 0.94340(4) 0.31146(4) 0.01527(11) Uani 1 1 d . . . . .
S5 S 0.31394(5) 1.00907(4) 0.48902(4) 0.01473(11) Uani 1 1 d . . . . .
S6 S 0.01132(4) 0.81290(4) 0.48618(4) 0.01394(11) Uani 1 1 d . . . . .
S9 S 0.12916(5) 0.87946(4) 0.13637(4) 0.01666(11) Uani 1 1 d . . . . .
S3 S 0.40110(4) 1.05920(4) 0.67888(4) 0.01581(11) Uani 1 1 d . . . . .
S1 S 0.37856(5) 1.05191(4) 0.91369(4) 0.02016(12) Uani 1 1 d . . . . .
S10 S -0.04987(5) 0.76567(5) 0.06195(4) 0.02083(12) Uani 1 1 d . . . . .
O4 O 0.83535(13) 0.60590(11) 0.71237(11) 0.0167(3) Uani 1 1 d . . . . .
O1 O 0.31224(13) 0.52242(12) 0.86123(11) 0.0187(3) Uani 1 1 d . . . . .
O3 O 0.73345(13) 0.43638(12) 0.67120(11) 0.0166(3) Uani 1 1 d . . . . .
F1 F 0.59335(14) 0.65753(12) 0.51021(11) 0.0381(4) Uani 1 1 d . . . . .
O6 O 0.40982(13) 0.68670(12) 0.91969(11) 0.0185(3) Uani 1 1 d . . . . .
O5 O 0.68547(13) 0.69229(11) 0.87747(11) 0.0168(3) Uani 1 1 d . . . . .
O2 O 0.45585(13) 0.42796(11) 0.70586(12) 0.0192(3) Uani 1 1 d . . . . .
N1 N 0.55667(15) 0.60904(13) 0.74849(13) 0.0137(3) Uani 1 1 d . . . . .
H1A H 0.614937 0.564772 0.714551 0.021 Uiso 1 1 calc R U . . .
H1B H 0.483977 0.573263 0.781654 0.021 Uiso 1 1 calc R U . . .
H1C H 0.595355 0.621321 0.800747 0.021 Uiso 1 1 calc R U . . .
C19 C 0.12250(18) 0.87973(16) 0.27216(15) 0.0141(4) Uani 1 1 d . . . . .
C18 C 0.02637(18) 0.82467(16) 0.34813(16) 0.0134(4) Uani 1 1 d . . . . .
C16 C 0.20641(18) 0.93910(16) 0.70291(15) 0.0137(4) Uani 1 1 d . . . . .
C10 C 0.80410(19) 0.73546(16) 0.81377(17) 0.0185(4) Uani 1 1 d . . . . .
H10A H 0.847773 0.766666 0.857322 0.022 Uiso 1 1 calc R U . . .
H10B H 0.782854 0.797218 0.744744 0.022 Uiso 1 1 calc R U . . .
C8 C 0.91883(18) 0.51958(16) 0.67688(17) 0.0174(4) Uani 1 1 d . . . . .
H8A H 0.941383 0.453170 0.742092 0.021 Uiso 1 1 calc R U . . .
H8B H 1.001744 0.548604 0.634511 0.021 Uiso 1 1 calc R U . . .
C6 C 0.66849(19) 0.38516(17) 0.61474(17) 0.0182(4) Uani 1 1 d . . . . .
H6A H 0.730058 0.324514 0.593677 0.022 Uiso 1 1 calc R U . . .
H6B H 0.638957 0.442895 0.546193 0.022 Uiso 1 1 calc R U . . .
C17 C 0.29934(18) 0.99764(16) 0.62693(16) 0.0134(4) Uani 1 1 d . . . . .
C14 C 0.22837(19) 0.59995(18) 0.90982(18) 0.0218(4) Uani 1 1 d . . . . .
H14A H 0.148706 0.565337 0.952842 0.026 Uiso 1 1 calc R U . . .
H14B H 0.199866 0.670459 0.850742 0.026 Uiso 1 1 calc R U . . .
C7 C 0.84623(18) 0.48524(17) 0.60443(16) 0.0176(4) Uani 1 1 d . . . . .
H7A H 0.818722 0.552534 0.541732 0.021 Uiso 1 1 calc R U . . .
H7B H 0.904279 0.429302 0.573690 0.021 Uiso 1 1 calc R U . . .
C9 C 0.89436(18) 0.63964(17) 0.78567(17) 0.0173(4) Uani 1 1 d . . . . .
H9A H 0.981195 0.664886 0.749642 0.021 Uiso 1 1 calc R U . . .
H9B H 0.908234 0.574720 0.854289 0.021 Uiso 1 1 calc R U . . .
C11 C 0.5956(2) 0.77821(18) 0.91068(18) 0.0215(4) Uani 1 1 d . . . . .
H11A H 0.565597 0.839446 0.844374 0.026 Uiso 1 1 calc R U . . .
H11B H 0.640084 0.811947 0.951540 0.026 Uiso 1 1 calc R U . . .
C5 C 0.55166(19) 0.33585(17) 0.69161(17) 0.0183(4) Uani 1 1 d . . . . .
H5A H 0.513264 0.289362 0.659583 0.022 Uiso 1 1 calc R U . . .
H5B H 0.579308 0.286486 0.764334 0.022 Uiso 1 1 calc R U . . .
C12 C 0.4798(2) 0.72407(18) 0.98399(17) 0.0224(4) Uani 1 1 d . . . . .
H12A H 0.510744 0.658588 1.046833 0.027 Uiso 1 1 calc R U . . .
H12B H 0.420905 0.779672 1.014630 0.027 Uiso 1 1 calc R U . . .
C13 C 0.3035(2) 0.62724(19) 0.98510(17) 0.0229(4) Uani 1 1 d . . . . .
H13A H 0.244280 0.674743 1.025264 0.028 Uiso 1 1 calc R U . . .
H13B H 0.337884 0.556184 1.040619 0.028 Uiso 1 1 calc R U . . .
C2 C 0.4815(2) 0.70384(18) 0.56381(18) 0.0230(4) Uani 1 1 d . . . . .
H2A H 0.412378 0.652395 0.586088 0.028 Uiso 1 1 calc R U . . .
H2B H 0.446384 0.777907 0.512876 0.028 Uiso 1 1 calc R U . . .
C3 C 0.24717(19) 0.48761(18) 0.79172(18) 0.0224(4) Uani 1 1 d . . . . .
H3A H 0.231405 0.551769 0.722932 0.027 Uiso 1 1 calc R U . . .
H3B H 0.160810 0.463707 0.830980 0.027 Uiso 1 1 calc R U . . .
C4 C 0.33330(19) 0.38992(18) 0.76316(19) 0.0229(4) Uani 1 1 d . . . . .
H4A H 0.348511 0.325440 0.831838 0.027 Uiso 1 1 calc R U . . .
H4B H 0.289623 0.363919 0.715471 0.027 Uiso 1 1 calc R U . . .
C1 C 0.5170(2) 0.71989(17) 0.66430(17) 0.0223(4) Uani 1 1 d . . . . .
H1D H 0.590624 0.766806 0.641938 0.027 Uiso 1 1 calc R U . . .
H1E H 0.440267 0.761122 0.697718 0.027 Uiso 1 1 calc R U . . .
C15 C 0.32822(18) 1.01913(16) 0.81589(16) 0.0145(4) Uani 1 1 d . . . . .
C20 C -0.00165(18) 0.80113(17) 0.15953(16) 0.0158(4) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S4 2.1671(5) . ?
Ni1 S7 2.1706(5) . ?
Ni1 S5 2.1677(5) . ?
Ni1 S6 2.1676(5) . ?
S8 C18 1.7473(18) . ?
S8 C20 1.733(2) . ?
S4 C16 1.7182(18) . ?
S2 C16 1.7495(18) . ?
S2 C15 1.7392(19) . ?
S7 C19 1.7217(18) . ?
S5 C17 1.7180(19) . ?
S6 C18 1.7183(19) . ?
S9 C19 1.7437(18) . ?
S9 C20 1.740(2) . ?
S3 C17 1.7489(18) . ?
S3 C15 1.734(2) . ?
S1 C15 1.6442(18) . ?
S10 C20 1.6505(19) . ?
O4 C8 1.423(2) . ?
O4 C9 1.422(2) . ?
O1 C14 1.430(2) . ?
O1 C3 1.428(2) . ?
O3 C6 1.432(2) . ?
O3 C7 1.423(2) . ?
F1 C2 1.388(2) . ?
O6 C12 1.428(2) . ?
O6 C13 1.421(2) . ?
O5 C10 1.435(2) . ?
O5 C11 1.434(2) . ?
O2 C5 1.433(2) . ?
O2 C4 1.426(2) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N1 C1 1.488(2) . ?
C19 C18 1.367(3) . ?
C16 C17 1.362(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C9 1.503(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C7 1.506(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C5 1.503(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C13 1.502(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.499(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C1 1.494(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.506(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C1 H1D 0.9900 . ?
C1 H1E 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S4 Ni1 S7 178.80(2) . . ?
S4 Ni1 S5 92.793(18) . . ?
S4 Ni1 S6 86.917(18) . . ?
S5 Ni1 S7 87.063(18) . . ?
S6 Ni1 S7 93.271(19) . . ?
S6 Ni1 S5 177.782(19) . . ?
C20 S8 C18 97.79(9) . . ?
C16 S4 Ni1 102.55(7) . . ?
C15 S2 C16 97.18(9) . . ?
C19 S7 Ni1 102.20(7) . . ?
C17 S5 Ni1 102.36(7) . . ?
C18 S6 Ni1 101.90(7) . . ?
C20 S9 C19 97.37(9) . . ?
C15 S3 C17 97.48(9) . . ?
C9 O4 C8 111.76(14) . . ?
C3 O1 C14 112.80(14) . . ?
C7 O3 C6 112.27(14) . . ?
C13 O6 C12 112.28(15) . . ?
C11 O5 C10 111.79(14) . . ?
C4 O2 C5 111.90(15) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
S7 C19 S9 122.87(12) . . ?
C18 C19 S7 120.74(14) . . ?
C18 C19 S9 116.38(14) . . ?
S6 C18 S8 122.66(12) . . ?
C19 C18 S8 115.51(14) . . ?
C19 C18 S6 121.82(14) . . ?
S4 C16 S2 122.81(12) . . ?
C17 C16 S4 120.93(14) . . ?
C17 C16 S2 116.25(14) . . ?
O5 C10 H10A 110.0 . . ?
O5 C10 H10B 110.0 . . ?
O5 C10 C9 108.43(15) . . ?
H10A C10 H10B 108.4 . . ?
C9 C10 H10A 110.0 . . ?
C9 C10 H10B 110.0 . . ?
O4 C8 H8A 110.1 . . ?
O4 C8 H8B 110.1 . . ?
O4 C8 C7 108.14(15) . . ?
H8A C8 H8B 108.4 . . ?
C7 C8 H8A 110.1 . . ?
C7 C8 H8B 110.1 . . ?
O3 C6 H6A 110.0 . . ?
O3 C6 H6B 110.0 . . ?
O3 C6 C5 108.33(16) . . ?
H6A C6 H6B 108.4 . . ?
C5 C6 H6A 110.0 . . ?
C5 C6 H6B 110.0 . . ?
S5 C17 S3 122.83(12) . . ?
C16 C17 S5 121.32(14) . . ?
C16 C17 S3 115.86(14) . . ?
O1 C14 H14A 109.9 . . ?
O1 C14 H14B 109.9 . . ?
O1 C14 C13 108.78(16) . . ?
H14A C14 H14B 108.3 . . ?
C13 C14 H14A 109.9 . . ?
C13 C14 H14B 109.9 . . ?
O3 C7 C8 107.87(15) . . ?
O3 C7 H7A 110.1 . . ?
O3 C7 H7B 110.1 . . ?
C8 C7 H7A 110.1 . . ?
C8 C7 H7B 110.1 . . ?
H7A C7 H7B 108.4 . . ?
O4 C9 C10 108.51(15) . . ?
O4 C9 H9A 110.0 . . ?
O4 C9 H9B 110.0 . . ?
C10 C9 H9A 110.0 . . ?
C10 C9 H9B 110.0 . . ?
H9A C9 H9B 108.4 . . ?
O5 C11 H11A 110.0 . . ?
O5 C11 H11B 110.0 . . ?
O5 C11 C12 108.31(16) . . ?
H11A C11 H11B 108.4 . . ?
C12 C11 H11A 110.0 . . ?
C12 C11 H11B 110.0 . . ?
O2 C5 C6 108.16(16) . . ?
O2 C5 H5A 110.1 . . ?
O2 C5 H5B 110.1 . . ?
C6 C5 H5A 110.1 . . ?
C6 C5 H5B 110.1 . . ?
H5A C5 H5B 108.4 . . ?
O6 C12 C11 108.77(16) . . ?
O6 C12 H12A 109.9 . . ?
O6 C12 H12B 109.9 . . ?
C11 C12 H12A 109.9 . . ?
C11 C12 H12B 109.9 . . ?
H12A C12 H12B 108.3 . . ?
O6 C13 C14 108.78(16) . . ?
O6 C13 H13A 109.9 . . ?
O6 C13 H13B 109.9 . . ?
C14 C13 H13A 109.9 . . ?
C14 C13 H13B 109.9 . . ?
H13A C13 H13B 108.3 . . ?
F1 C2 H2A 109.9 . . ?
F1 C2 H2B 109.9 . . ?
F1 C2 C1 109.12(17) . . ?
H2A C2 H2B 108.3 . . ?
C1 C2 H2A 109.9 . . ?
C1 C2 H2B 109.9 . . ?
O1 C3 H3A 110.0 . . ?
O1 C3 H3B 110.0 . . ?
O1 C3 C4 108.68(15) . . ?
H3A C3 H3B 108.3 . . ?
C4 C3 H3A 110.0 . . ?
C4 C3 H3B 110.0 . . ?
O2 C4 C3 108.26(16) . . ?
O2 C4 H4A 110.0 . . ?
O2 C4 H4B 110.0 . . ?
C3 C4 H4A 110.0 . . ?
C3 C4 H4B 110.0 . . ?
H4A C4 H4B 108.4 . . ?
N1 C1 C2 111.51(16) . . ?
N1 C1 H1D 109.3 . . ?
N1 C1 H1E 109.3 . . ?
C2 C1 H1D 109.3 . . ?
C2 C1 H1E 109.3 . . ?
H1D C1 H1E 108.0 . . ?
S3 C15 S2 113.18(10) . . ?
S1 C15 S2 123.71(12) . . ?
S1 C15 S3 123.09(11) . . ?
S8 C20 S9 112.89(10) . . ?
S10 C20 S8 123.49(12) . . ?
S10 C20 S9 123.62(12) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S4 C16 S2 179.49(10) . . . . ?
Ni1 S4 C16 C17 -0.77(17) . . . . ?
Ni1 S7 C19 S9 -179.29(10) . . . . ?
Ni1 S7 C19 C18 -0.18(17) . . . . ?
Ni1 S5 C17 S3 177.60(10) . . . . ?
Ni1 S5 C17 C16 -2.35(17) . . . . ?
Ni1 S6 C18 S8 -178.52(10) . . . . ?
Ni1 S6 C18 C19 2.55(17) . . . . ?
S4 C16 C17 S5 2.2(2) . . . . ?
S4 C16 C17 S3 -177.72(10) . . . . ?
S2 C16 C17 S5 -178.02(10) . . . . ?
S2 C16 C17 S3 2.0(2) . . . . ?
S7 C19 C18 S8 179.31(10) . . . . ?
S7 C19 C18 S6 -1.7(2) . . . . ?
S9 C19 C18 S8 -1.5(2) . . . . ?
S9 C19 C18 S6 177.47(10) . . . . ?
O4 C8 C7 O3 -64.03(19) . . . . ?
O1 C14 C13 O6 65.2(2) . . . . ?
O1 C3 C4 O2 -60.2(2) . . . . ?
O3 C6 C5 O2 68.71(18) . . . . ?
F1 C2 C1 N1 -65.6(2) . . . . ?
O5 C10 C9 O4 66.49(19) . . . . ?
O5 C11 C12 O6 -65.6(2) . . . . ?
C19 S9 C20 S8 1.96(12) . . . . ?
C19 S9 C20 S10 -178.78(13) . . . . ?
C18 S8 C20 S9 -2.62(12) . . . . ?
C18 S8 C20 S10 178.11(13) . . . . ?
C16 S2 C15 S3 -0.74(12) . . . . ?
C16 S2 C15 S1 -179.37(12) . . . . ?
C10 O5 C11 C12 -175.58(15) . . . . ?
C8 O4 C9 C10 176.63(16) . . . . ?
C6 O3 C7 C8 -171.11(14) . . . . ?
C17 S3 C15 S2 1.61(12) . . . . ?
C17 S3 C15 S1 -179.75(12) . . . . ?
C14 O1 C3 C4 -168.94(17) . . . . ?
C7 O3 C6 C5 179.80(15) . . . . ?
C9 O4 C8 C7 177.31(16) . . . . ?
C11 O5 C10 C9 178.13(15) . . . . ?
C5 O2 C4 C3 170.42(15) . . . . ?
C12 O6 C13 C14 175.18(15) . . . . ?
C13 O6 C12 C11 175.96(15) . . . . ?
C3 O1 C14 C13 177.47(17) . . . . ?
C4 O2 C5 C6 170.66(15) . . . . ?
C15 S2 C16 S4 178.98(12) . . . . ?
C15 S2 C16 C17 -0.77(17) . . . . ?
C15 S3 C17 S5 177.84(12) . . . . ?
C15 S3 C17 C16 -2.21(16) . . . . ?
C20 S8 C18 S6 -176.46(12) . . . . ?
C20 S8 C18 C19 2.53(17) . . . . ?
C20 S9 C19 S7 178.87(12) . . . . ?
C20 S9 C19 C18 -0.27(17) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.873
_oxdiff_exptl_absorpt_empirical_full_min 0.503
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_113k
_database_code_depnum_ccdc_archive 'CCDC 2053283'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-19 downloaded from the CCDC.
;
_audit_creation_date             2020-12-31
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C12 H24 O6, C2 H7 F N'
_chemical_formula_sum            'C20 H31 F N Ni O6 S10'
_chemical_formula_weight         779.77
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHNOFNiS
_chemical_oxdiff_usercomment     20_20200608
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.3864(2)
_cell_length_b                   12.6343(5)
_cell_length_c                   12.9338(5)
_cell_angle_alpha                69.944(3)
_cell_angle_beta                 79.973(3)
_cell_angle_gamma                79.970(3)
_cell_volume                     1557.90(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    10376
_cell_measurement_temperature    113
_cell_measurement_theta_max      30.5170
_cell_measurement_theta_min      2.0060
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.336
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55315
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             806
_exptl_crystal_size_max          0.507
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.781
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19702
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.781
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.838
_diffrn_reflns_theta_min         1.990
_diffrn_ambient_temperature      113
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.781
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -77.00   4.00   0.50    0.14    --   -4.95 -37.00  60.00  162
  2  ω    -16.00  25.00   0.50    0.14    --   -4.95 -99.00 150.00   82
  3  ω     -6.00  39.00   0.50    0.14    --    5.18 -99.00   0.00   90
  4  ω    -13.00  16.00   0.50    0.14    --    5.18 -99.00 -60.00   58
  5  ω    -77.00  10.00   0.50    0.14    --   -4.95 -57.00-180.00  174
  6  ω    -10.00  67.00   0.50    0.14    --   -4.95  37.00   0.00  154
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0012634000
_diffrn_orient_matrix_UB_12      0.0561269000
_diffrn_orient_matrix_UB_13      0.0005251000
_diffrn_orient_matrix_UB_21      -0.0115234000
_diffrn_orient_matrix_UB_22      -0.0195261000
_diffrn_orient_matrix_UB_23      0.0587790000
_diffrn_orient_matrix_UB_31      0.0689191000
_diffrn_orient_matrix_UB_32      -0.0097923000
_diffrn_orient_matrix_UB_33      0.0024597000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6189
_reflns_number_total             7645
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         7645
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0329
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0362P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0857
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
F1A \\sim C1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
3.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C7(H7A,H7B), C6(H6A,H6B), C3(H3A,H3B), C4(H4A,H4B), C11(H11A,
 H11B), C8(H8A,H8B), C13(H13A,H13B), C12(H12A,H12B), C14(H14A,H14B), C1(H1D,
 H1E), C9(H9A,H9B), C10(H10A,H10B), C2(H2A,H2B)
3.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.16536(2) 0.40799(2) 0.48802(2) 0.01357(7) Uani 1 1 d . . . . .
S2 S -0.07740(4) 0.26573(4) 0.29568(4) 0.01570(10) Uani 1 1 d . . . . .
S4 S 0.01109(4) 0.31296(4) 0.48620(4) 0.01568(10) Uani 1 1 d . . . . .
S6 S 0.10336(4) 0.36992(4) 0.66452(4) 0.01664(11) Uani 1 1 d . . . . .
S5 S 0.23092(4) 0.44316(4) 0.31194(4) 0.01692(11) Uani 1 1 d . . . . .
S8 S 0.19947(5) 0.43839(4) 0.83941(4) 0.01692(10) Uani 1 1 d . . . . .
S3 S 0.12917(5) 0.37927(4) 0.13686(4) 0.01844(11) Uani 1 1 d . . . . .
S9 S 0.40100(4) 0.55884(4) 0.67922(4) 0.01782(11) Uani 1 1 d . . . . .
S7 S 0.31391(4) 0.50878(4) 0.48952(4) 0.01644(10) Uani 1 1 d . . . . .
S10 S 0.37850(5) 0.55162(4) 0.91381(4) 0.02262(12) Uani 1 1 d . . . . .
S1 S -0.04963(5) 0.26557(4) 0.06234(4) 0.02353(12) Uani 1 1 d . . . . .
O2 O 0.16489(12) 0.89429(10) 0.28743(12) 0.0180(3) Uani 1 1 d . . . . .
O3 O 0.26647(12) 1.06381(11) 0.32876(12) 0.0188(3) Uani 1 1 d . . . . .
N1 N 0.44375(14) 0.89053(12) 0.25180(13) 0.0156(3) Uani 1 1 d . . . . .
H1A H 0.407626 0.878161 0.200087 0.019 Uiso 1 1 calc R U . . .
H1B H 0.514181 0.926471 0.220360 0.019 Uiso 1 1 calc R U . . .
H1C H 0.385375 0.933022 0.284832 0.019 Uiso 1 1 calc R U . . .
O5 O 0.68775(12) 0.97762(11) 0.13870(12) 0.0208(3) Uani 1 1 d . . . . .
O1 O 0.31424(12) 0.80778(10) 0.12255(12) 0.0191(3) Uani 1 1 d . . . . .
O6 O 0.59029(13) 0.81373(11) 0.08003(12) 0.0204(3) Uani 1 1 d . . . . .
O4 O 0.54410(12) 1.07191(10) 0.29446(12) 0.0215(3) Uani 1 1 d . . . . .
C16 C 0.02634(17) 0.32506(14) 0.34832(17) 0.0152(4) Uani 1 1 d . . . . .
C18 C 0.20679(17) 0.43881(15) 0.70315(16) 0.0148(4) Uani 1 1 d . . . . .
C19 C 0.29925(17) 0.49764(14) 0.62716(16) 0.0150(4) Uani 1 1 d . . . . .
C17 C 0.12262(18) 0.37953(15) 0.27230(16) 0.0155(4) Uani 1 1 d . . . . .
C20 C 0.32811(17) 0.51910(15) 0.81568(16) 0.0159(4) Uani 1 1 d . . . . .
C15 C -0.00155(18) 0.30117(15) 0.15982(17) 0.0173(4) Uani 1 1 d . . . . .
C5 C 0.08180(18) 0.98014(15) 0.32320(18) 0.0200(4) Uani 1 1 d . . . . .
H5A H 0.000831 0.951543 0.364607 0.024 Uiso 1 1 calc R U . . .
H5B H 0.059509 1.045057 0.259566 0.024 Uiso 1 1 calc R U . . .
C7 C 0.33166(19) 1.11492(16) 0.38539(17) 0.0199(4) Uani 1 1 d . . . . .
H7A H 0.360247 1.058392 0.452415 0.024 Uiso 1 1 calc R U . . .
H7B H 0.271641 1.174412 0.405987 0.024 Uiso 1 1 calc R U . . .
C6 C 0.15359(18) 1.01491(16) 0.39551(17) 0.0194(4) Uani 1 1 d . . . . .
H6A H 0.096578 1.069782 0.425328 0.023 Uiso 1 1 calc R U . . .
H6B H 0.180395 0.949300 0.456940 0.023 Uiso 1 1 calc R U . . .
C3 C 0.19660(19) 0.76446(15) 0.18605(18) 0.0211(4) Uani 1 1 d . . . . .
H3A H 0.217673 0.704103 0.253396 0.025 Uiso 1 1 calc R U . . .
H3B H 0.153924 0.733762 0.143502 0.025 Uiso 1 1 calc R U . . .
C4 C 0.10594(18) 0.86035(16) 0.21454(18) 0.0196(4) Uani 1 1 d . . . . .
H4A H 0.091991 0.923803 0.147568 0.024 Uiso 1 1 calc R U . . .
H4B H 0.021216 0.835395 0.249982 0.024 Uiso 1 1 calc R U . . .
C11 C 0.77108(18) 0.90084(17) 0.09001(18) 0.0228(4) Uani 1 1 d . . . . .
H11A H 0.799344 0.831982 0.147622 0.027 Uiso 1 1 calc R U . . .
H11B H 0.848768 0.935027 0.047943 0.027 Uiso 1 1 calc R U . . .
C8 C 0.44883(19) 1.16393(15) 0.30878(18) 0.0207(4) Uani 1 1 d . . . . .
H8A H 0.422052 1.212342 0.237694 0.025 Uiso 1 1 calc R U . . .
H8B H 0.486488 1.209247 0.340318 0.025 Uiso 1 1 calc R U . . .
C13 C 0.5200(2) 0.77627(17) 0.01571(18) 0.0243(4) Uani 1 1 d . . . . .
H13A H 0.577568 0.721710 -0.014209 0.029 Uiso 1 1 calc R U . . .
H13B H 0.490095 0.840309 -0.045773 0.029 Uiso 1 1 calc R U . . .
C12 C 0.6968(2) 0.87281(17) 0.01469(18) 0.0254(4) Uani 1 1 d . . . . .
H12A H 0.663484 0.942028 -0.040028 0.030 Uiso 1 1 calc R U . . .
H12B H 0.754963 0.825861 -0.024021 0.030 Uiso 1 1 calc R U . . .
C14 C 0.4043(2) 0.72258(16) 0.08840(19) 0.0239(4) Uani 1 1 d . . . . .
H14A H 0.360897 0.689922 0.048048 0.029 Uiso 1 1 calc R U . . .
H14B H 0.433628 0.662305 0.152940 0.029 Uiso 1 1 calc R U . . .
C1 C 0.4840(2) 0.78014(16) 0.33556(18) 0.0246(4) Uani 1 1 d . . . . .
H1D H 0.412807 0.733419 0.356549 0.030 Uiso 1 1 calc R U . . .
H1E H 0.559991 0.740619 0.302997 0.030 Uiso 1 1 calc R U . . .
C9 C 0.66684(19) 1.10927(17) 0.2370(2) 0.0254(5) Uani 1 1 d . . . . .
H9A H 0.709570 1.135146 0.283339 0.030 Uiso 1 1 calc R U . . .
H9B H 0.652067 1.172033 0.169675 0.030 Uiso 1 1 calc R U . . .
C10 C 0.75262(19) 1.01206(17) 0.20892(19) 0.0249(5) Uani 1 1 d . . . . .
H10A H 0.837307 1.035245 0.171035 0.030 Uiso 1 1 calc R U . . .
H10B H 0.767399 0.949242 0.276191 0.030 Uiso 1 1 calc R U . . .
C2 C 0.5171(2) 0.79583(17) 0.43585(19) 0.0269(5) Uani 1 1 d . . . . .
H2A H 0.551609 0.723326 0.485324 0.032 Uiso 1 1 calc R U . . .
H2B H 0.584294 0.846447 0.414871 0.032 Uiso 1 1 calc R U . . .
F1A F 0.40551(14) 0.84112(11) 0.48966(12) 0.0443(4) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S4 2.1707(5) . ?
Ni1 S6 2.1679(6) . ?
Ni1 S5 2.1723(6) . ?
Ni1 S7 2.1712(5) . ?
S2 C16 1.7530(17) . ?
S2 C15 1.735(2) . ?
S4 C16 1.718(2) . ?
S6 C18 1.7240(17) . ?
S5 C17 1.7242(17) . ?
S8 C18 1.7490(19) . ?
S8 C20 1.7426(18) . ?
S3 C17 1.742(2) . ?
S3 C15 1.7409(19) . ?
S9 C19 1.7486(17) . ?
S9 C20 1.732(2) . ?
S7 C19 1.719(2) . ?
S10 C20 1.6484(18) . ?
S1 C15 1.6515(19) . ?
O2 C5 1.419(2) . ?
O2 C4 1.420(2) . ?
O3 C7 1.436(2) . ?
O3 C6 1.427(2) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.487(2) . ?
O5 C11 1.422(2) . ?
O5 C10 1.433(2) . ?
O1 C3 1.429(2) . ?
O1 C14 1.436(2) . ?
O6 C13 1.432(2) . ?
O6 C12 1.423(2) . ?
O4 C8 1.431(2) . ?
O4 C9 1.428(2) . ?
C16 C17 1.369(3) . ?
C18 C19 1.364(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.504(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.506(3) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.509(3) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.504(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.497(3) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C1 C2 1.482(3) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.499(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 F1A 1.384(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S4 Ni1 S5 93.291(19) . . ?
S4 Ni1 S7 177.759(19) . . ?
S6 Ni1 S4 86.902(19) . . ?
S6 Ni1 S5 178.77(2) . . ?
S6 Ni1 S7 92.790(19) . . ?
S7 Ni1 S5 87.064(19) . . ?
C15 S2 C16 97.72(9) . . ?
C16 S4 Ni1 101.74(6) . . ?
C18 S6 Ni1 102.55(7) . . ?
C17 S5 Ni1 102.29(7) . . ?
C20 S8 C18 96.94(9) . . ?
C15 S3 C17 97.39(9) . . ?
C20 S9 C19 97.48(9) . . ?
C19 S7 Ni1 102.43(6) . . ?
C5 O2 C4 111.86(13) . . ?
C6 O3 C7 112.30(15) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
C11 O5 C10 112.87(14) . . ?
C3 O1 C14 112.04(14) . . ?
C12 O6 C13 112.27(17) . . ?
C9 O4 C8 112.16(14) . . ?
S4 C16 S2 122.50(12) . . ?
C17 C16 S2 115.31(15) . . ?
C17 C16 S4 122.18(14) . . ?
S6 C18 S8 122.72(12) . . ?
C19 C18 S6 120.86(15) . . ?
C19 C18 S8 116.42(13) . . ?
S7 C19 S9 122.89(11) . . ?
C18 C19 S9 115.77(15) . . ?
C18 C19 S7 121.34(13) . . ?
S5 C17 S3 122.99(12) . . ?
C16 C17 S5 120.43(15) . . ?
C16 C17 S3 116.57(14) . . ?
S9 C20 S8 113.33(10) . . ?
S10 C20 S8 123.50(12) . . ?
S10 C20 S9 123.15(11) . . ?
S2 C15 S3 112.96(10) . . ?
S1 C15 S2 123.40(11) . . ?
S1 C15 S3 123.64(13) . . ?
O2 C5 H5A 110.0 . . ?
O2 C5 H5B 110.0 . . ?
O2 C5 C6 108.51(14) . . ?
H5A C5 H5B 108.4 . . ?
C6 C5 H5A 110.0 . . ?
C6 C5 H5B 110.0 . . ?
O3 C7 H7A 110.0 . . ?
O3 C7 H7B 110.0 . . ?
O3 C7 C8 108.41(16) . . ?
H7A C7 H7B 108.4 . . ?
C8 C7 H7A 110.0 . . ?
C8 C7 H7B 110.0 . . ?
O3 C6 C5 107.78(17) . . ?
O3 C6 H6A 110.2 . . ?
O3 C6 H6B 110.2 . . ?
C5 C6 H6A 110.2 . . ?
C5 C6 H6B 110.2 . . ?
H6A C6 H6B 108.5 . . ?
O1 C3 H3A 110.0 . . ?
O1 C3 H3B 110.0 . . ?
O1 C3 C4 108.41(15) . . ?
H3A C3 H3B 108.4 . . ?
C4 C3 H3A 110.0 . . ?
C4 C3 H3B 110.0 . . ?
O2 C4 C3 108.49(14) . . ?
O2 C4 H4A 110.0 . . ?
O2 C4 H4B 110.0 . . ?
C3 C4 H4A 110.0 . . ?
C3 C4 H4B 110.0 . . ?
H4A C4 H4B 108.4 . . ?
O5 C11 H11A 109.8 . . ?
O5 C11 H11B 109.8 . . ?
O5 C11 C12 109.22(15) . . ?
H11A C11 H11B 108.3 . . ?
C12 C11 H11A 109.8 . . ?
C12 C11 H11B 109.8 . . ?
O4 C8 C7 108.22(15) . . ?
O4 C8 H8A 110.1 . . ?
O4 C8 H8B 110.1 . . ?
C7 C8 H8A 110.1 . . ?
C7 C8 H8B 110.1 . . ?
H8A C8 H8B 108.4 . . ?
O6 C13 H13A 109.9 . . ?
O6 C13 H13B 109.9 . . ?
O6 C13 C14 108.96(17) . . ?
H13A C13 H13B 108.3 . . ?
C14 C13 H13A 109.9 . . ?
C14 C13 H13B 109.9 . . ?
O6 C12 C11 108.63(18) . . ?
O6 C12 H12A 110.0 . . ?
O6 C12 H12B 110.0 . . ?
C11 C12 H12A 110.0 . . ?
C11 C12 H12B 110.0 . . ?
H12A C12 H12B 108.3 . . ?
O1 C14 C13 108.83(15) . . ?
O1 C14 H14A 109.9 . . ?
O1 C14 H14B 109.9 . . ?
C13 C14 H14A 109.9 . . ?
C13 C14 H14B 109.9 . . ?
H14A C14 H14B 108.3 . . ?
N1 C1 H1D 109.3 . . ?
N1 C1 H1E 109.3 . . ?
H1D C1 H1E 107.9 . . ?
C2 C1 N1 111.72(15) . . ?
C2 C1 H1D 109.3 . . ?
C2 C1 H1E 109.3 . . ?
O4 C9 H9A 110.0 . . ?
O4 C9 H9B 110.0 . . ?
O4 C9 C10 108.67(15) . . ?
H9A C9 H9B 108.3 . . ?
C10 C9 H9A 110.0 . . ?
C10 C9 H9B 110.0 . . ?
O5 C10 C9 108.42(15) . . ?
O5 C10 H10A 110.0 . . ?
O5 C10 H10B 110.0 . . ?
C9 C10 H10A 110.0 . . ?
C9 C10 H10B 110.0 . . ?
H10A C10 H10B 108.4 . . ?
C1 C2 H2A 109.7 . . ?
C1 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
F1A C2 C1 109.80(17) . . ?
F1A C2 H2A 109.7 . . ?
F1A C2 H2B 109.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S4 C16 S2 -178.74(9) . . . . ?
Ni1 S4 C16 C17 2.85(16) . . . . ?
Ni1 S6 C18 S8 179.24(9) . . . . ?
Ni1 S6 C18 C19 -0.42(16) . . . . ?
Ni1 S5 C17 S3 -179.35(9) . . . . ?
Ni1 S5 C17 C16 0.11(16) . . . . ?
Ni1 S7 C19 S9 177.48(9) . . . . ?
Ni1 S7 C19 C18 -1.97(16) . . . . ?
S2 C16 C17 S5 179.37(9) . . . . ?
S2 C16 C17 S3 -1.15(19) . . . . ?
S4 C16 C17 S5 -2.1(2) . . . . ?
S4 C16 C17 S3 177.36(9) . . . . ?
S6 C18 C19 S9 -177.78(9) . . . . ?
S6 C18 C19 S7 1.7(2) . . . . ?
S8 C18 C19 S9 2.54(19) . . . . ?
S8 C18 C19 S7 -177.98(9) . . . . ?
O2 C5 C6 O3 63.79(19) . . . . ?
O3 C7 C8 O4 -68.67(18) . . . . ?
N1 C1 C2 F1A 65.3(2) . . . . ?
O5 C11 C12 O6 -64.6(2) . . . . ?
O1 C3 C4 O2 -66.4(2) . . . . ?
O6 C13 C14 O1 65.31(19) . . . . ?
O4 C9 C10 O5 60.8(2) . . . . ?
C16 S2 C15 S3 -2.48(11) . . . . ?
C16 S2 C15 S1 178.15(12) . . . . ?
C18 S8 C20 S9 -0.71(11) . . . . ?
C18 S8 C20 S10 -179.10(11) . . . . ?
C19 S9 C20 S8 1.79(11) . . . . ?
C19 S9 C20 S10 -179.81(11) . . . . ?
C17 S3 C15 S2 1.98(12) . . . . ?
C17 S3 C15 S1 -178.64(12) . . . . ?
C20 S8 C18 S6 179.22(11) . . . . ?
C20 S8 C18 C19 -1.11(15) . . . . ?
C20 S9 C19 S7 177.91(11) . . . . ?
C20 S9 C19 C18 -2.62(15) . . . . ?
C15 S2 C16 S4 -176.30(11) . . . . ?
C15 S2 C16 C17 2.21(15) . . . . ?
C15 S3 C17 S5 178.96(11) . . . . ?
C15 S3 C17 C16 -0.52(16) . . . . ?
C5 O2 C4 C3 -176.63(16) . . . . ?
C7 O3 C6 C5 171.52(13) . . . . ?
C6 O3 C7 C8 180.00(14) . . . . ?
C3 O1 C14 C13 175.90(15) . . . . ?
C4 O2 C5 C6 -177.45(16) . . . . ?
C11 O5 C10 C9 168.67(17) . . . . ?
C8 O4 C9 C10 -170.70(15) . . . . ?
C13 O6 C12 C11 -175.64(14) . . . . ?
C12 O6 C13 C14 -175.98(15) . . . . ?
C14 O1 C3 C4 -177.89(15) . . . . ?
C9 O4 C8 C7 -170.95(15) . . . . ?
C10 O5 C11 C12 -177.90(17) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.132
_oxdiff_exptl_absorpt_empirical_full_min 0.513
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_293k
_database_code_depnum_ccdc_archive 'CCDC 2053292'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-19 downloaded from the CCDC.
;
_audit_creation_date             2020-11-11
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C12 H24 O6, C2 H7 F N'
_chemical_formula_sum            'C20 H31 F N Ni O6 S10'
_chemical_formula_weight         779.77
_chemical_melting_point          ?
_chemical_oxdiff_formula         CNHFONiS
_chemical_oxdiff_usercomment     20_20200608
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.5115(3)
_cell_length_b                   12.6531(4)
_cell_length_c                   12.9821(3)
_cell_angle_alpha                71.701(2)
_cell_angle_beta                 79.787(2)
_cell_angle_gamma                80.782(2)
_cell_volume                     1603.24(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    11011
_cell_measurement_temperature    293
_cell_measurement_theta_max      30.1490
_cell_measurement_theta_min      2.4070
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.298
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60164
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             806
_exptl_crystal_size_max          0.507
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.793
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20112
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.793
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.719
_diffrn_reflns_theta_min         1.981
_diffrn_ambient_temperature      293
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.793
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -75.00   7.00   0.50    0.52    --   -4.95 -37.00   0.00  164
  2  ω    -38.00  10.00   0.50    0.52    --   -4.95 -57.00 120.00   96
  3  ω    -17.00  27.00   0.50    0.52    --   -4.95 -99.00  90.00   88
  4  ω     -9.00  39.00   0.50    0.52    --    5.18 -99.00 -60.00   96
  5  ω     18.00  73.00   0.50    0.52    --    5.18  37.00-150.00  110
  6  ω    -10.00  68.00   0.50    0.52    --   -4.95  37.00 -60.00  156
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0028350000
_diffrn_orient_matrix_UB_12      0.0544944000
_diffrn_orient_matrix_UB_13      0.0052400000
_diffrn_orient_matrix_UB_21      -0.0102110000
_diffrn_orient_matrix_UB_22      -0.0223540000
_diffrn_orient_matrix_UB_23      0.0578389000
_diffrn_orient_matrix_UB_31      0.0681794000
_diffrn_orient_matrix_UB_32      -0.0078079000
_diffrn_orient_matrix_UB_33      0.0009135000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5651
_reflns_number_total             7909
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.368
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         7909
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0336
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0352P)²+0.2540P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0867
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
2. Others
 Sof(H1AA)=Sof(H1AB)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(F1)=1-FVAR(1)
 Sof(H1BC)=Sof(H1BD)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(F1A)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C7(H7A,H7B), C6(H6A,H6B), C3(H3A,H3B), C4(H4A,H4B), C11(H11A,
 H11B), C8(H8A,H8B), C13(H13A,H13B), C12(H12A,H12B), C14(H14A,H14B), C1(H1BC,
 H1BD), C1(H1AA,H1AB), C9(H9A,H9B), C10(H10A,H10B), C2(H2A,H2B), C2A(H2AA,H2AB)
3.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.16315(2) 0.40449(2) 0.49218(2) 0.03987(8) Uani 1 1 d . . . . .
S2 S -0.07929(5) 0.26664(4) 0.29633(5) 0.04591(13) Uani 1 1 d . . . . .
S4 S 0.00647(5) 0.31461(4) 0.48683(4) 0.04529(13) Uani 1 1 d . . . . .
S6 S 0.10003(5) 0.36913(4) 0.66639(5) 0.04798(13) Uani 1 1 d . . . . .
S5 S 0.22912(5) 0.43859(5) 0.31829(5) 0.04829(13) Uani 1 1 d . . . . .
S8 S 0.19574(6) 0.43713(5) 0.84114(5) 0.05011(13) Uani 1 1 d . . . . .
S3 S 0.12883(5) 0.37474(5) 0.14304(5) 0.05312(14) Uani 1 1 d . . . . .
S9 S 0.40168(5) 0.54842(5) 0.68702(5) 0.05375(15) Uani 1 1 d . . . . .
S7 S 0.31628(5) 0.49780(5) 0.49715(5) 0.05167(14) Uani 1 1 d . . . . .
S10 S 0.37486(7) 0.54705(6) 0.91807(6) 0.06705(18) Uani 1 1 d . . . . .
S1 S -0.04877(6) 0.26361(7) 0.06545(6) 0.06829(19) Uani 1 1 d . . . . .
O2 O 0.16940(13) 0.89564(13) 0.28372(14) 0.0564(4) Uani 1 1 d . . . . .
O3 O 0.26779(14) 1.06478(13) 0.32960(14) 0.0583(4) Uani 1 1 d . . . . .
N1 N 0.44716(15) 0.89033(13) 0.25438(14) 0.0426(4) Uani 1 1 d . . . . .
H1A H 0.405387 0.875371 0.207536 0.051 Uiso 1 1 calc R U . . .
H1B H 0.515325 0.926123 0.217842 0.051 Uiso 1 1 calc R U . . .
H1C H 0.393622 0.933253 0.289943 0.051 Uiso 1 1 calc R U . . .
O5 O 0.68682(14) 0.98079(14) 0.14125(15) 0.0646(4) Uani 1 1 d . . . . .
O1 O 0.31927(16) 0.80800(13) 0.12206(14) 0.0604(4) Uani 1 1 d . . . . .
O6 O 0.58991(16) 0.81845(15) 0.07826(14) 0.0654(4) Uani 1 1 d . . . . .
O4 O 0.53987(15) 1.07319(13) 0.29824(15) 0.0633(4) Uani 1 1 d . . . . .
C16 C 0.02367(18) 0.32450(16) 0.35053(17) 0.0405(4) Uani 1 1 d . . . . .
C18 C 0.20467(19) 0.43485(16) 0.70661(17) 0.0411(4) Uani 1 1 d . . . . .
C19 C 0.29948(18) 0.48920(17) 0.63356(18) 0.0435(5) Uani 1 1 d . . . . .
C17 C 0.12073(18) 0.37660(17) 0.27742(17) 0.0428(4) Uani 1 1 d . . . . .
C20 C 0.3256(2) 0.51332(18) 0.82064(18) 0.0481(5) Uani 1 1 d . . . . .
C15 C -0.00182(19) 0.29922(18) 0.16302(19) 0.0481(5) Uani 1 1 d . . . . .
C5 C 0.0880(2) 0.9820(2) 0.3197(2) 0.0628(6) Uani 1 1 d . . . . .
H5A H 0.006563 0.954744 0.359035 0.075 Uiso 1 1 calc R U . . .
H5B H 0.068739 1.045273 0.257096 0.075 Uiso 1 1 calc R U . . .
C7 C 0.3319(3) 1.1147(2) 0.3881(2) 0.0648(6) Uani 1 1 d . . . . .
H7A H 0.358674 1.058679 0.453269 0.078 Uiso 1 1 calc R U . . .
H7B H 0.273051 1.173257 0.410461 0.078 Uiso 1 1 calc R U . . .
C6 C 0.1547(2) 1.0171(2) 0.3918(2) 0.0646(6) Uani 1 1 d . . . . .
H6A H 0.097508 1.071751 0.421578 0.077 Uiso 1 1 calc R U . . .
H6B H 0.178581 0.953065 0.452265 0.077 Uiso 1 1 calc R U . . .
C3 C 0.2011(2) 0.7655(2) 0.1838(2) 0.0659(7) Uani 1 1 d . . . . .
H3A H 0.220321 0.706735 0.249850 0.079 Uiso 1 1 calc R U . . .
H3B H 0.159886 0.734099 0.140650 0.079 Uiso 1 1 calc R U . . .
C4 C 0.1132(2) 0.8584(2) 0.2127(2) 0.0635(7) Uani 1 1 d . . . . .
H4A H 0.099289 0.919394 0.146913 0.076 Uiso 1 1 calc R U . . .
H4B H 0.029628 0.832940 0.248131 0.076 Uiso 1 1 calc R U . . .
C11 C 0.7689(2) 0.9033(2) 0.0917(3) 0.0774(8) Uani 1 1 d . . . . .
H11A H 0.795044 0.835722 0.147775 0.093 Uiso 1 1 calc R U . . .
H11B H 0.846688 0.936221 0.050622 0.093 Uiso 1 1 calc R U . . .
C8 C 0.4470(3) 1.1623(2) 0.3156(2) 0.0676(7) Uani 1 1 d . . . . .
H8A H 0.421869 1.210539 0.246220 0.081 Uiso 1 1 calc R U . . .
H8B H 0.483923 1.206728 0.349210 0.081 Uiso 1 1 calc R U . . .
C13 C 0.5188(3) 0.7803(3) 0.0142(2) 0.0766(8) Uani 1 1 d . . . . .
H13A H 0.575028 0.726695 -0.017519 0.092 Uiso 1 1 calc R U . . .
H13B H 0.489461 0.843233 -0.045010 0.092 Uiso 1 1 calc R U . . .
C12 C 0.6956(3) 0.8754(3) 0.0170(2) 0.0779(8) Uani 1 1 d . . . . .
H12A H 0.664401 0.943673 -0.035825 0.094 Uiso 1 1 calc R U . . .
H12B H 0.752625 0.828820 -0.022713 0.094 Uiso 1 1 calc R U . . .
C14 C 0.4054(3) 0.7273(2) 0.0844(3) 0.0755(8) Uani 1 1 d . . . . .
H14A H 0.361899 0.695809 0.042804 0.091 Uiso 1 1 calc R U . . .
H14B H 0.434110 0.667193 0.146047 0.091 Uiso 1 1 calc R U . . .
C1 C 0.4924(3) 0.7841(2) 0.3341(2) 0.0757(8) Uani 1 1 d . . . . .
H1BC H 0.430088 0.731132 0.346141 0.091 Uiso 0.588(10) 1 calc R U P A 2
H1BD H 0.574499 0.753597 0.301377 0.091 Uiso 0.588(10) 1 calc R U P A 2
H1AA H 0.494323 0.723050 0.303423 0.091 Uiso 0.412(10) 1 calc R U P A 1
H1AB H 0.580668 0.787657 0.344159 0.091 Uiso 0.412(10) 1 calc R U P A 1
C9 C 0.6610(2) 1.1106(2) 0.2428(3) 0.0751(8) Uani 1 1 d . . . . .
H9A H 0.702055 1.137426 0.289582 0.090 Uiso 1 1 calc R U . . .
H9B H 0.647370 1.171786 0.177015 0.090 Uiso 1 1 calc R U . . .
C10 C 0.7463(2) 1.0149(2) 0.2133(3) 0.0769(8) Uani 1 1 d . . . . .
H10A H 0.831006 1.037892 0.178263 0.092 Uiso 1 1 calc R U . . .
H10B H 0.758172 0.953057 0.278921 0.092 Uiso 1 1 calc R U . . .
C2 C 0.5092(7) 0.7917(5) 0.4349(4) 0.076(2) Uani 0.588(10) 1 d . . P A 2
H2A H 0.562216 0.851043 0.425332 0.091 Uiso 0.588(10) 1 calc R U P A 2
H2B H 0.551853 0.721713 0.477147 0.091 Uiso 0.588(10) 1 calc R U P A 2
C2A C 0.4167(10) 0.7605(6) 0.4348(6) 0.068(3) Uani 0.412(10) 1 d . . P A 1
H2AA H 0.453861 0.691152 0.482439 0.082 Uiso 0.412(10) 1 calc R U P A 1
H2AB H 0.330242 0.749887 0.426224 0.082 Uiso 0.412(10) 1 calc R U P A 1
F1A F 0.4072(13) 0.8463(10) 0.4839(8) 0.106(3) Uani 0.588(10) 1 d . . P A 1
F1 F 0.3775(16) 0.8164(16) 0.4917(12) 0.107(5) Uani 0.412(10) 1 d . . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S4 2.1680(5) . ?
Ni1 S6 2.1640(6) . ?
Ni1 S5 2.1662(6) . ?
Ni1 S7 2.1640(5) . ?
S2 C16 1.7465(19) . ?
S2 C15 1.729(2) . ?
S4 C16 1.713(2) . ?
S6 C18 1.7156(19) . ?
S5 C17 1.7194(19) . ?
S8 C18 1.741(2) . ?
S8 C20 1.731(2) . ?
S3 C17 1.739(2) . ?
S3 C15 1.733(2) . ?
S9 C19 1.7454(19) . ?
S9 C20 1.727(2) . ?
S7 C19 1.719(2) . ?
S10 C20 1.641(2) . ?
S1 C15 1.644(2) . ?
O2 C5 1.422(3) . ?
O2 C4 1.406(3) . ?
O3 C7 1.432(3) . ?
O3 C6 1.419(3) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.483(3) . ?
O5 C11 1.432(3) . ?
O5 C10 1.414(3) . ?
O1 C3 1.437(3) . ?
O1 C14 1.401(3) . ?
O6 C13 1.439(3) . ?
O6 C12 1.403(3) . ?
O4 C8 1.416(3) . ?
O4 C9 1.420(3) . ?
C16 C17 1.362(3) . ?
C18 C19 1.357(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.470(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.478(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.477(3) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.492(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.478(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C1 H1BC 0.9700 . ?
C1 H1BD 0.9700 . ?
C1 H1AA 0.9700 . ?
C1 H1AB 0.9700 . ?
C1 C2 1.386(6) . ?
C1 C2A 1.376(9) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.496(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 F1 1.484(17) . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?
C2A F1A 1.404(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S6 Ni1 S4 87.15(2) . . ?
S6 Ni1 S5 179.16(2) . . ?
S5 Ni1 S4 93.28(2) . . ?
S7 Ni1 S4 178.63(2) . . ?
S7 Ni1 S6 92.74(2) . . ?
S7 Ni1 S5 86.85(2) . . ?
C15 S2 C16 97.70(10) . . ?
C16 S4 Ni1 101.81(6) . . ?
C18 S6 Ni1 102.58(7) . . ?
C17 S5 Ni1 102.06(7) . . ?
C20 S8 C18 97.25(10) . . ?
C15 S3 C17 97.54(10) . . ?
C20 S9 C19 97.29(10) . . ?
C19 S7 Ni1 102.39(7) . . ?
C4 O2 C5 112.76(17) . . ?
C6 O3 C7 113.24(19) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
C10 O5 C11 114.1(2) . . ?
C14 O1 C3 112.83(19) . . ?
C12 O6 C13 113.8(2) . . ?
C8 O4 C9 112.26(19) . . ?
S4 C16 S2 122.58(12) . . ?
C17 C16 S2 115.54(16) . . ?
C17 C16 S4 121.87(15) . . ?
S6 C18 S8 122.79(12) . . ?
C19 C18 S6 121.01(16) . . ?
C19 C18 S8 116.19(15) . . ?
S7 C19 S9 122.83(12) . . ?
C18 C19 S9 115.91(16) . . ?
C18 C19 S7 121.26(15) . . ?
S5 C17 S3 122.78(12) . . ?
C16 C17 S5 120.95(16) . . ?
C16 C17 S3 116.27(15) . . ?
S9 C20 S8 113.30(12) . . ?
S10 C20 S8 123.90(14) . . ?
S10 C20 S9 122.79(13) . . ?
S2 C15 S3 112.88(12) . . ?
S1 C15 S2 123.35(12) . . ?
S1 C15 S3 123.76(14) . . ?
O2 C5 H5A 109.8 . . ?
O2 C5 H5B 109.8 . . ?
O2 C5 C6 109.19(19) . . ?
H5A C5 H5B 108.3 . . ?
C6 C5 H5A 109.8 . . ?
C6 C5 H5B 109.8 . . ?
O3 C7 H7A 110.0 . . ?
O3 C7 H7B 110.0 . . ?
O3 C7 C8 108.6(2) . . ?
H7A C7 H7B 108.3 . . ?
C8 C7 H7A 110.0 . . ?
C8 C7 H7B 110.0 . . ?
O3 C6 C5 108.4(2) . . ?
O3 C6 H6A 110.0 . . ?
O3 C6 H6B 110.0 . . ?
C5 C6 H6A 110.0 . . ?
C5 C6 H6B 110.0 . . ?
H6A C6 H6B 108.4 . . ?
O1 C3 H3A 109.9 . . ?
O1 C3 H3B 109.9 . . ?
O1 C3 C4 108.70(18) . . ?
H3A C3 H3B 108.3 . . ?
C4 C3 H3A 109.9 . . ?
C4 C3 H3B 109.9 . . ?
O2 C4 C3 109.08(19) . . ?
O2 C4 H4A 109.9 . . ?
O2 C4 H4B 109.9 . . ?
C3 C4 H4A 109.9 . . ?
C3 C4 H4B 109.9 . . ?
H4A C4 H4B 108.3 . . ?
O5 C11 H11A 109.9 . . ?
O5 C11 H11B 109.9 . . ?
O5 C11 C12 108.7(2) . . ?
H11A C11 H11B 108.3 . . ?
C12 C11 H11A 109.9 . . ?
C12 C11 H11B 109.9 . . ?
O4 C8 C7 108.6(2) . . ?
O4 C8 H8A 110.0 . . ?
O4 C8 H8B 110.0 . . ?
C7 C8 H8A 110.0 . . ?
C7 C8 H8B 110.0 . . ?
H8A C8 H8B 108.3 . . ?
O6 C13 H13A 109.7 . . ?
O6 C13 H13B 109.7 . . ?
O6 C13 C14 109.8(2) . . ?
H13A C13 H13B 108.2 . . ?
C14 C13 H13A 109.7 . . ?
C14 C13 H13B 109.7 . . ?
O6 C12 C11 109.7(2) . . ?
O6 C12 H12A 109.7 . . ?
O6 C12 H12B 109.7 . . ?
C11 C12 H12A 109.7 . . ?
C11 C12 H12B 109.7 . . ?
H12A C12 H12B 108.2 . . ?
O1 C14 C13 109.2(2) . . ?
O1 C14 H14A 109.8 . . ?
O1 C14 H14B 109.8 . . ?
C13 C14 H14A 109.8 . . ?
C13 C14 H14B 109.8 . . ?
H14A C14 H14B 108.3 . . ?
N1 C1 H1BC 108.3 . . ?
N1 C1 H1BD 108.3 . . ?
N1 C1 H1AA 108.7 . . ?
N1 C1 H1AB 108.7 . . ?
H1BC C1 H1BD 107.4 . . ?
H1AA C1 H1AB 107.6 . . ?
C2 C1 N1 116.0(3) . . ?
C2 C1 H1BC 108.3 . . ?
C2 C1 H1BD 108.3 . . ?
C2A C1 N1 114.3(4) . . ?
C2A C1 H1AA 108.7 . . ?
C2A C1 H1AB 108.7 . . ?
O4 C9 H9A 110.0 . . ?
O4 C9 H9B 110.0 . . ?
O4 C9 C10 108.69(19) . . ?
H9A C9 H9B 108.3 . . ?
C10 C9 H9A 110.0 . . ?
C10 C9 H9B 110.0 . . ?
O5 C10 C9 108.7(2) . . ?
O5 C10 H10A 109.9 . . ?
O5 C10 H10B 109.9 . . ?
C9 C10 H10A 109.9 . . ?
C9 C10 H10B 109.9 . . ?
H10A C10 H10B 108.3 . . ?
C1 C2 H2A 110.4 . . ?
C1 C2 H2B 110.4 . . ?
C1 C2 F1 106.7(8) . . ?
H2A C2 H2B 108.6 . . ?
F1 C2 H2A 110.4 . . ?
F1 C2 H2B 110.4 . . ?
C1 C2A H2AA 109.2 . . ?
C1 C2A H2AB 109.2 . . ?
C1 C2A F1A 112.2(7) . . ?
H2AA C2A H2AB 107.9 . . ?
F1A C2A H2AA 109.2 . . ?
F1A C2A H2AB 109.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S4 C16 S2 -179.56(10) . . . . ?
Ni1 S4 C16 C17 1.68(18) . . . . ?
Ni1 S6 C18 S8 178.24(10) . . . . ?
Ni1 S6 C18 C19 -1.28(18) . . . . ?
Ni1 S5 C17 S3 -178.52(11) . . . . ?
Ni1 S5 C17 C16 0.65(18) . . . . ?
Ni1 S7 C19 S9 178.68(11) . . . . ?
Ni1 S7 C19 C18 -1.15(18) . . . . ?
S2 C16 C17 S5 179.48(11) . . . . ?
S2 C16 C17 S3 -1.3(2) . . . . ?
S4 C16 C17 S5 -1.7(2) . . . . ?
S4 C16 C17 S3 177.54(11) . . . . ?
S6 C18 C19 S9 -178.11(11) . . . . ?
S6 C18 C19 S7 1.7(3) . . . . ?
S8 C18 C19 S9 2.3(2) . . . . ?
S8 C18 C19 S7 -177.81(11) . . . . ?
O2 C5 C6 O3 64.2(3) . . . . ?
O3 C7 C8 O4 -68.6(3) . . . . ?
N1 C1 C2 F1 69.2(9) . . . . ?
N1 C1 C2A F1A -57.4(9) . . . . ?
O5 C11 C12 O6 -65.0(3) . . . . ?
O1 C3 C4 O2 -65.1(3) . . . . ?
O6 C13 C14 O1 64.5(3) . . . . ?
O4 C9 C10 O5 62.2(3) . . . . ?
C16 S2 C15 S3 -2.65(14) . . . . ?
C16 S2 C15 S1 178.14(14) . . . . ?
C18 S8 C20 S9 -0.90(13) . . . . ?
C18 S8 C20 S10 -179.56(14) . . . . ?
C19 S9 C20 S8 1.90(13) . . . . ?
C19 S9 C20 S10 -179.42(14) . . . . ?
C17 S3 C15 S2 2.09(14) . . . . ?
C17 S3 C15 S1 -178.70(15) . . . . ?
C20 S8 C18 S6 179.59(13) . . . . ?
C20 S8 C18 C19 -0.87(18) . . . . ?
C20 S9 C19 S7 177.59(13) . . . . ?
C20 S9 C19 C18 -2.57(18) . . . . ?
C15 S2 C16 S4 -176.42(13) . . . . ?
C15 S2 C16 C17 2.41(18) . . . . ?
C15 S3 C17 S5 178.71(13) . . . . ?
C15 S3 C17 C16 -0.50(18) . . . . ?
C5 O2 C4 C3 -177.3(2) . . . . ?
C7 O3 C6 C5 172.67(19) . . . . ?
C6 O3 C7 C8 -179.48(19) . . . . ?
C3 O1 C14 C13 175.3(2) . . . . ?
C4 O2 C5 C6 -179.1(2) . . . . ?
C11 O5 C10 C9 169.5(2) . . . . ?
C8 O4 C9 C10 -171.8(2) . . . . ?
C13 O6 C12 C11 -175.5(2) . . . . ?
C12 O6 C13 C14 -176.8(2) . . . . ?
C14 O1 C3 C4 -175.8(2) . . . . ?
C9 O4 C8 C7 -171.3(2) . . . . ?
C10 O5 C11 C12 -179.3(2) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.960
_oxdiff_exptl_absorpt_empirical_full_min 0.558
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_153k
_database_code_depnum_ccdc_archive 'CCDC 2053285'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-19 downloaded from the CCDC.
;
_audit_creation_date             2020-11-25
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C12 H24 O6, C2 H7 F N'
_chemical_formula_sum            'C20 H31 F N Ni O6 S10'
_chemical_formula_weight         779.77
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHNOFNiS
_chemical_oxdiff_usercomment     20_20200608
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.3994(3)
_cell_length_b                   12.6286(5)
_cell_length_c                   12.9431(4)
_cell_angle_alpha                70.317(3)
_cell_angle_beta                 79.956(2)
_cell_angle_gamma                80.078(3)
_cell_volume                     1564.10(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    11110
_cell_measurement_temperature    153
_cell_measurement_theta_max      30.7090
_cell_measurement_theta_min      2.0180
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.331
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67479
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             806
_exptl_crystal_size_max          0.507
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.784
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19288
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.784
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.826
_diffrn_reflns_theta_min         2.004
_diffrn_ambient_temperature      153
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.784
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -5.00  75.00   0.50    0.19    --    5.18  37.00   0.00  160
  2  ω     -8.00  70.00   0.50    0.19    --    5.18  77.00  60.00  156
  3  ω    -76.00  16.00   0.50    0.19    --   -5.03 -77.00 150.00  184
  4  ω    -18.00  27.00   0.50    0.19    --    5.18 -99.00 -90.00   90
  5  ω    -14.00  39.00   0.50    0.19    --    5.18 -99.00-120.00  106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0018475000
_diffrn_orient_matrix_UB_12      0.0556759000
_diffrn_orient_matrix_UB_13      0.0020409000
_diffrn_orient_matrix_UB_21      -0.0114175000
_diffrn_orient_matrix_UB_22      -0.0206054000
_diffrn_orient_matrix_UB_23      0.0585849000
_diffrn_orient_matrix_UB_31      0.0688276000
_diffrn_orient_matrix_UB_32      -0.0093885000
_diffrn_orient_matrix_UB_33      0.0023095000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6273
_reflns_number_total             7694
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         7694
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0333
_refine_ls_restrained_S_all      1.072
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0380P)²+0.0235P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0879
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
2. Rigid body (RIGU) restrains
 F1A, C2A, C1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(H1AA)=Sof(H1AB)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=1-FVAR(1)
 Sof(H1BC)=Sof(H1BD)=Sof(C2)=Sof(H2A)=Sof(H2B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C7(H7A,H7B), C6(H6A,H6B), C3(H3A,H3B), C4(H4A,H4B), C11(H11A,
 H11B), C8(H8A,H8B), C13(H13A,H13B), C12(H12A,H12B), C14(H14A,H14B), C1(H1BC,
 H1BD), C1(H1AA,H1AB), C9(H9A,H9B), C10(H10A,H10B), C2(H2A,H2B), C2A(H2AA,H2AB)
4.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.16496(2) 0.40741(2) 0.48879(2) 0.01812(7) Uani 1 1 d . . . . .
S2 S -0.07768(4) 0.26584(4) 0.29585(4) 0.02105(10) Uani 1 1 d . . . . .
S4 S 0.01021(4) 0.31332(4) 0.48627(4) 0.02088(10) Uani 1 1 d . . . . .
S6 S 0.10282(5) 0.36958(4) 0.66481(4) 0.02232(11) Uani 1 1 d . . . . .
S5 S 0.23055(5) 0.44237(4) 0.31334(4) 0.02288(11) Uani 1 1 d . . . . .
S8 S 0.19887(5) 0.43793(4) 0.83957(4) 0.02304(11) Uani 1 1 d . . . . .
S3 S 0.12923(5) 0.37831(4) 0.13832(4) 0.02491(11) Uani 1 1 d . . . . .
S9 S 0.40111(5) 0.55697(4) 0.68068(4) 0.02472(11) Uani 1 1 d . . . . .
S7 S 0.31407(5) 0.50715(4) 0.49101(4) 0.02280(11) Uani 1 1 d . . . . .
S10 S 0.37802(5) 0.55054(4) 0.91445(4) 0.03094(13) Uani 1 1 d . . . . .
S1 S -0.04953(5) 0.26520(4) 0.06324(4) 0.03167(12) Uani 1 1 d . . . . .
O2 O 0.16586(12) 0.89462(10) 0.28685(12) 0.0244(3) Uani 1 1 d . . . . .
O3 O 0.26674(13) 1.06414(10) 0.32907(11) 0.0248(3) Uani 1 1 d . . . . .
N1 N 0.44448(15) 0.88992(11) 0.25217(13) 0.0207(3) Uani 1 1 d . . . . .
H1A H 0.407195 0.876994 0.201384 0.025 Uiso 1 1 calc R U . . .
H1B H 0.514105 0.926435 0.219656 0.025 Uiso 1 1 calc R U . . .
H1C H 0.386687 0.931997 0.286147 0.025 Uiso 1 1 calc R U . . .
O5 O 0.68802(13) 0.97797(10) 0.13898(12) 0.0288(3) Uani 1 1 d . . . . .
O1 O 0.31494(13) 0.80808(10) 0.12211(11) 0.0252(3) Uani 1 1 d . . . . .
O6 O 0.59005(13) 0.81523(11) 0.07883(11) 0.0274(3) Uani 1 1 d . . . . .
O4 O 0.54363(13) 1.07157(10) 0.29513(12) 0.0291(3) Uani 1 1 d . . . . .
C16 C 0.02610(17) 0.32477(13) 0.34860(15) 0.0187(4) Uani 1 1 d . . . . .
C18 C 0.20670(18) 0.43827(14) 0.70334(15) 0.0197(4) Uani 1 1 d . . . . .
C19 C 0.29923(18) 0.49606(14) 0.62848(16) 0.0200(4) Uani 1 1 d . . . . .
C17 C 0.12227(18) 0.37914(14) 0.27364(15) 0.0202(4) Uani 1 1 d . . . . .
C20 C 0.32761(18) 0.51781(14) 0.81688(16) 0.0217(4) Uani 1 1 d . . . . .
C15 C -0.00132(18) 0.30061(14) 0.16043(16) 0.0226(4) Uani 1 1 d . . . . .
C5 C 0.08256(19) 0.98049(15) 0.32270(17) 0.0270(4) Uani 1 1 d . . . . .
H5A H 0.001750 0.951886 0.364095 0.032 Uiso 1 1 calc R U . . .
H5B H 0.060256 1.045008 0.259369 0.032 Uiso 1 1 calc R U . . .
C7 C 0.3321(2) 1.11455(15) 0.38593(17) 0.0274(4) Uani 1 1 d . . . . .
H7A H 0.360671 1.057876 0.452366 0.033 Uiso 1 1 calc R U . . .
H7B H 0.272462 1.173823 0.407237 0.033 Uiso 1 1 calc R U . . .
C6 C 0.15416(19) 1.01553(15) 0.39448(17) 0.0268(4) Uani 1 1 d . . . . .
H6A H 0.097119 1.070343 0.424467 0.032 Uiso 1 1 calc R U . . .
H6B H 0.180643 0.950194 0.455628 0.032 Uiso 1 1 calc R U . . .
C3 C 0.1976(2) 0.76454(15) 0.18536(18) 0.0285(4) Uani 1 1 d . . . . .
H3A H 0.218720 0.704496 0.252350 0.034 Uiso 1 1 calc R U . . .
H3B H 0.155146 0.733623 0.142772 0.034 Uiso 1 1 calc R U . . .
C4 C 0.10781(19) 0.85954(15) 0.21392(17) 0.0261(4) Uani 1 1 d . . . . .
H4A H 0.093843 0.922527 0.147186 0.031 Uiso 1 1 calc R U . . .
H4B H 0.023212 0.834492 0.249182 0.031 Uiso 1 1 calc R U . . .
C11 C 0.7708(2) 0.90120(17) 0.08951(18) 0.0318(5) Uani 1 1 d . . . . .
H11A H 0.798905 0.832336 0.146495 0.038 Uiso 1 1 calc R U . . .
H11B H 0.848534 0.935154 0.047580 0.038 Uiso 1 1 calc R U . . .
C8 C 0.4484(2) 1.16320(15) 0.31033(18) 0.0287(4) Uani 1 1 d . . . . .
H8A H 0.421700 1.211635 0.239669 0.034 Uiso 1 1 calc R U . . .
H8B H 0.485990 1.208360 0.342270 0.034 Uiso 1 1 calc R U . . .
C13 C 0.5196(2) 0.77756(17) 0.01468(18) 0.0322(5) Uani 1 1 d . . . . .
H13A H 0.577123 0.723316 -0.015784 0.039 Uiso 1 1 calc R U . . .
H13B H 0.489459 0.841423 -0.046210 0.039 Uiso 1 1 calc R U . . .
C12 C 0.6963(2) 0.87381(17) 0.01448(18) 0.0333(5) Uani 1 1 d . . . . .
H12A H 0.663205 0.943098 -0.039537 0.040 Uiso 1 1 calc R U . . .
H12B H 0.754018 0.827069 -0.024794 0.040 Uiso 1 1 calc R U . . .
C14 C 0.4046(2) 0.72367(16) 0.08685(18) 0.0318(5) Uani 1 1 d . . . . .
H14A H 0.361114 0.691294 0.046193 0.038 Uiso 1 1 calc R U . . .
H14B H 0.434118 0.663307 0.150663 0.038 Uiso 1 1 calc R U . . .
C1 C 0.4869(2) 0.78049(15) 0.33438(18) 0.0340(5) Uani 1 1 d . . . . .
H1BC H 0.418142 0.731633 0.353283 0.041 Uiso 0.874(6) 1 calc R U P A 2
H1BD H 0.565082 0.743520 0.301655 0.041 Uiso 0.874(6) 1 calc R U P A 2
H1AA H 0.472525 0.718812 0.310628 0.041 Uiso 0.126(6) 1 calc R U P A 1
H1AB H 0.580393 0.774929 0.337596 0.041 Uiso 0.126(6) 1 calc R U P A 1
C9 C 0.6663(2) 1.10870(17) 0.2384(2) 0.0347(5) Uani 1 1 d . . . . .
H9A H 0.708934 1.134173 0.285245 0.042 Uiso 1 1 calc R U . . .
H9B H 0.651957 1.171579 0.171696 0.042 Uiso 1 1 calc R U . . .
C10 C 0.7519(2) 1.01190(17) 0.20945(19) 0.0327(5) Uani 1 1 d . . . . .
H10A H 0.836604 1.035072 0.172062 0.039 Uiso 1 1 calc R U . . .
H10B H 0.766333 0.949019 0.276158 0.039 Uiso 1 1 calc R U . . .
C2 C 0.5155(3) 0.79527(19) 0.4361(2) 0.0312(7) Uani 0.874(6) 1 d . . P A 2
H2A H 0.549502 0.722741 0.484974 0.037 Uiso 0.874(6) 1 calc R U P A 2
H2B H 0.582062 0.846110 0.417452 0.037 Uiso 0.874(6) 1 calc R U P A 2
C2A C 0.417(3) 0.7689(16) 0.4430(16) 0.047(6) Uani 0.126(6) 1 d . . P A 1
H2AA H 0.328827 0.754753 0.440315 0.057 Uiso 0.126(6) 1 calc R U P A 1
H2AB H 0.457895 0.699741 0.492059 0.057 Uiso 0.126(6) 1 calc R U P A 1
F1A F 0.40320(17) 0.83899(12) 0.48910(12) 0.0617(5) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S4 2.1694(5) . ?
Ni1 S6 2.1670(5) . ?
Ni1 S5 2.1692(5) . ?
Ni1 S7 2.1691(5) . ?
S2 C16 1.7496(17) . ?
S2 C15 1.735(2) . ?
S4 C16 1.7191(19) . ?
S6 C18 1.7235(17) . ?
S5 C17 1.7198(18) . ?
S8 C18 1.7495(18) . ?
S8 C20 1.7392(19) . ?
S3 C17 1.7439(19) . ?
S3 C15 1.7385(19) . ?
S9 C19 1.7468(17) . ?
S9 C20 1.735(2) . ?
S7 C19 1.7184(19) . ?
S10 C20 1.6424(18) . ?
S1 C15 1.6462(19) . ?
O2 C5 1.420(2) . ?
O2 C4 1.423(2) . ?
O3 C7 1.431(2) . ?
O3 C6 1.420(2) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.483(2) . ?
O5 C11 1.425(2) . ?
O5 C10 1.424(2) . ?
O1 C3 1.428(2) . ?
O1 C14 1.432(2) . ?
O6 C13 1.432(2) . ?
O6 C12 1.417(3) . ?
O4 C8 1.431(2) . ?
O4 C9 1.427(3) . ?
C16 C17 1.365(3) . ?
C18 C19 1.356(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.498(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.495(3) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.497(3) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.498(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.493(3) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C1 H1BC 0.9700 . ?
C1 H1BD 0.9700 . ?
C1 H1AA 0.9700 . ?
C1 H1AB 0.9700 . ?
C1 C2 1.475(3) . ?
C1 C2A 1.44(2) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.498(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 F1A 1.376(3) . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?
C2A F1A 1.20(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S6 Ni1 S4 86.881(19) . . ?
S6 Ni1 S5 178.78(2) . . ?
S6 Ni1 S7 92.823(19) . . ?
S5 Ni1 S4 93.321(19) . . ?
S5 Ni1 S7 87.021(19) . . ?
S7 Ni1 S4 177.792(19) . . ?
C15 S2 C16 97.63(9) . . ?
C16 S4 Ni1 101.71(6) . . ?
C18 S6 Ni1 102.31(7) . . ?
C17 S5 Ni1 102.16(7) . . ?
C20 S8 C18 96.97(9) . . ?
C15 S3 C17 97.53(9) . . ?
C20 S9 C19 97.38(9) . . ?
C19 S7 Ni1 102.37(6) . . ?
C5 O2 C4 112.17(13) . . ?
C6 O3 C7 112.72(16) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
C10 O5 C11 113.28(15) . . ?
C3 O1 C14 112.07(14) . . ?
C12 O6 C13 112.63(16) . . ?
C9 O4 C8 112.32(14) . . ?
S4 C16 S2 122.40(11) . . ?
C17 C16 S2 115.69(14) . . ?
C17 C16 S4 121.90(13) . . ?
S6 C18 S8 122.37(11) . . ?
C19 C18 S6 121.18(14) . . ?
C19 C18 S8 116.45(13) . . ?
S7 C19 S9 122.76(11) . . ?
C18 C19 S9 115.95(14) . . ?
C18 C19 S7 121.28(13) . . ?
S5 C17 S3 122.91(12) . . ?
C16 C17 S5 120.85(14) . . ?
C16 C17 S3 116.23(13) . . ?
S9 C20 S8 113.19(10) . . ?
S10 C20 S8 123.84(12) . . ?
S10 C20 S9 122.95(11) . . ?
S2 C15 S3 112.84(10) . . ?
S1 C15 S2 123.30(11) . . ?
S1 C15 S3 123.85(12) . . ?
O2 C5 H5A 110.0 . . ?
O2 C5 H5B 110.0 . . ?
O2 C5 C6 108.28(14) . . ?
H5A C5 H5B 108.4 . . ?
C6 C5 H5A 110.0 . . ?
C6 C5 H5B 110.0 . . ?
O3 C7 H7A 110.0 . . ?
O3 C7 H7B 110.0 . . ?
O3 C7 C8 108.52(17) . . ?
H7A C7 H7B 108.4 . . ?
C8 C7 H7A 110.0 . . ?
C8 C7 H7B 110.0 . . ?
O3 C6 C5 108.38(17) . . ?
O3 C6 H6A 110.0 . . ?
O3 C6 H6B 110.0 . . ?
C5 C6 H6A 110.0 . . ?
C5 C6 H6B 110.0 . . ?
H6A C6 H6B 108.4 . . ?
O1 C3 H3A 110.1 . . ?
O1 C3 H3B 110.1 . . ?
O1 C3 C4 108.23(14) . . ?
H3A C3 H3B 108.4 . . ?
C4 C3 H3A 110.1 . . ?
C4 C3 H3B 110.1 . . ?
O2 C4 C3 108.95(15) . . ?
O2 C4 H4A 109.9 . . ?
O2 C4 H4B 109.9 . . ?
C3 C4 H4A 109.9 . . ?
C3 C4 H4B 109.9 . . ?
H4A C4 H4B 108.3 . . ?
O5 C11 H11A 109.9 . . ?
O5 C11 H11B 109.9 . . ?
O5 C11 C12 109.14(15) . . ?
H11A C11 H11B 108.3 . . ?
C12 C11 H11A 109.9 . . ?
C12 C11 H11B 109.9 . . ?
O4 C8 C7 108.32(15) . . ?
O4 C8 H8A 110.0 . . ?
O4 C8 H8B 110.0 . . ?
C7 C8 H8A 110.0 . . ?
C7 C8 H8B 110.0 . . ?
H8A C8 H8B 108.4 . . ?
O6 C13 H13A 109.8 . . ?
O6 C13 H13B 109.8 . . ?
O6 C13 C14 109.18(17) . . ?
H13A C13 H13B 108.3 . . ?
C14 C13 H13A 109.8 . . ?
C14 C13 H13B 109.8 . . ?
O6 C12 C11 108.90(18) . . ?
O6 C12 H12A 109.9 . . ?
O6 C12 H12B 109.9 . . ?
C11 C12 H12A 109.9 . . ?
C11 C12 H12B 109.9 . . ?
H12A C12 H12B 108.3 . . ?
O1 C14 C13 108.82(15) . . ?
O1 C14 H14A 109.9 . . ?
O1 C14 H14B 109.9 . . ?
C13 C14 H14A 109.9 . . ?
C13 C14 H14B 109.9 . . ?
H14A C14 H14B 108.3 . . ?
N1 C1 H1BC 109.2 . . ?
N1 C1 H1BD 109.2 . . ?
N1 C1 H1AA 109.2 . . ?
N1 C1 H1AB 109.2 . . ?
H1BC C1 H1BD 107.9 . . ?
H1AA C1 H1AB 107.9 . . ?
C2 C1 N1 112.22(16) . . ?
C2 C1 H1BC 109.2 . . ?
C2 C1 H1BD 109.2 . . ?
C2A C1 N1 112.2(8) . . ?
C2A C1 H1AA 109.2 . . ?
C2A C1 H1AB 109.2 . . ?
O4 C9 H9A 109.9 . . ?
O4 C9 H9B 109.9 . . ?
O4 C9 C10 108.72(16) . . ?
H9A C9 H9B 108.3 . . ?
C10 C9 H9A 109.9 . . ?
C10 C9 H9B 109.9 . . ?
O5 C10 C9 108.61(15) . . ?
O5 C10 H10A 110.0 . . ?
O5 C10 H10B 110.0 . . ?
C9 C10 H10A 110.0 . . ?
C9 C10 H10B 110.0 . . ?
H10A C10 H10B 108.3 . . ?
C1 C2 H2A 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
F1A C2 C1 110.4(2) . . ?
F1A C2 H2A 109.6 . . ?
F1A C2 H2B 109.6 . . ?
C1 C2A H2AA 106.2 . . ?
C1 C2A H2AB 106.2 . . ?
H2AA C2A H2AB 106.4 . . ?
F1A C2A C1 124.7(17) . . ?
F1A C2A H2AA 106.2 . . ?
F1A C2A H2AB 106.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S4 C16 S2 -178.76(8) . . . . ?
Ni1 S4 C16 C17 2.31(15) . . . . ?
Ni1 S6 C18 S8 179.12(9) . . . . ?
Ni1 S6 C18 C19 -0.71(15) . . . . ?
Ni1 S5 C17 S3 -179.07(9) . . . . ?
Ni1 S5 C17 C16 -0.02(15) . . . . ?
Ni1 S7 C19 S9 177.66(9) . . . . ?
Ni1 S7 C19 C18 -2.08(15) . . . . ?
S2 C16 C17 S5 179.35(9) . . . . ?
S2 C16 C17 S3 -1.54(18) . . . . ?
S4 C16 C17 S5 -1.6(2) . . . . ?
S4 C16 C17 S3 177.46(9) . . . . ?
S6 C18 C19 S9 -177.76(9) . . . . ?
S6 C18 C19 S7 2.0(2) . . . . ?
S8 C18 C19 S9 2.40(18) . . . . ?
S8 C18 C19 S7 -177.85(9) . . . . ?
O2 C5 C6 O3 63.73(18) . . . . ?
O3 C7 C8 O4 -68.88(18) . . . . ?
N1 C1 C2 F1A 63.8(3) . . . . ?
N1 C1 C2A F1A -50(2) . . . . ?
O5 C11 C12 O6 -64.7(2) . . . . ?
O1 C3 C4 O2 -66.4(2) . . . . ?
O6 C13 C14 O1 65.07(19) . . . . ?
O4 C9 C10 O5 60.8(2) . . . . ?
C16 S2 C15 S3 -2.67(11) . . . . ?
C16 S2 C15 S1 178.26(11) . . . . ?
C18 S8 C20 S9 -0.75(11) . . . . ?
C18 S8 C20 S10 -179.20(11) . . . . ?
C19 S9 C20 S8 1.77(11) . . . . ?
C19 S9 C20 S10 -179.76(11) . . . . ?
C17 S3 C15 S2 2.01(11) . . . . ?
C17 S3 C15 S1 -178.93(11) . . . . ?
C20 S8 C18 S6 179.17(10) . . . . ?
C20 S8 C18 C19 -0.99(15) . . . . ?
C20 S9 C19 S7 177.73(11) . . . . ?
C20 S9 C19 C18 -2.52(15) . . . . ?
C15 S2 C16 S4 -176.43(10) . . . . ?
C15 S2 C16 C17 2.57(14) . . . . ?
C15 S3 C17 S5 178.79(11) . . . . ?
C15 S3 C17 C16 -0.30(15) . . . . ?
C5 O2 C4 C3 -176.63(16) . . . . ?
C7 O3 C6 C5 171.94(13) . . . . ?
C6 O3 C7 C8 -179.88(13) . . . . ?
C3 O1 C14 C13 175.88(15) . . . . ?
C4 O2 C5 C6 -177.42(16) . . . . ?
C11 O5 C10 C9 168.82(17) . . . . ?
C8 O4 C9 C10 -170.67(16) . . . . ?
C13 O6 C12 C11 -175.24(14) . . . . ?
C12 O6 C13 C14 -176.32(14) . . . . ?
C14 O1 C3 C4 -177.43(15) . . . . ?
C9 O4 C8 C7 -170.75(16) . . . . ?
C10 O5 C11 C12 -178.16(17) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.570
_oxdiff_exptl_absorpt_empirical_full_min 0.645
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_133k
_database_code_depnum_ccdc_archive 'CCDC 2053284'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-19 downloaded from the CCDC.
;
_audit_creation_date             2020-11-25
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C12 H24 O6, C2 H7 F N'
_chemical_formula_sum            'C20 H31 F N Ni O6 S10'
_chemical_formula_weight         779.77
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHNOFNiS
_chemical_oxdiff_usercomment     20_20200608
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.3884(3)
_cell_length_b                   12.6271(4)
_cell_length_c                   12.9344(4)
_cell_angle_alpha                70.113(3)
_cell_angle_beta                 79.966(2)
_cell_angle_gamma                80.068(2)
_cell_volume                     1559.30(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9576
_cell_measurement_temperature    113
_cell_measurement_theta_max      30.5280
_cell_measurement_theta_min      2.4400
_shelx_estimated_absorpt_T_max   0.889
_shelx_estimated_absorpt_T_min   0.551
_exptl_absorpt_coefficient_mu    1.335
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55431
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             806
_exptl_crystal_size_max          0.507
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_av_unetI/netI     0.0633
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.777
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19502
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.777
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.958
_diffrn_reflns_theta_min         2.455
_diffrn_ambient_temperature      113
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.777
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -17.00  27.00   0.50    0.16    --   -5.03 -99.00  90.00   88
  2  ω    -67.00  14.00   0.50    0.16    --    5.18 -37.00  90.00  162
  3  ω    -76.00   9.00   0.50    0.16    --   -5.03 -57.00-180.00  170
  4  ω    -18.00   9.00   0.50    0.16    --   -5.03 -99.00-180.00   54
  5  ω    -78.00  -1.00   0.50    0.16    --   -5.03 -37.00 -60.00  154
  6  ω     40.00  81.00   0.50    0.16    --    5.18  19.00 -90.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0014574000
_diffrn_orient_matrix_UB_12      0.0559315000
_diffrn_orient_matrix_UB_13      0.0012232000
_diffrn_orient_matrix_UB_21      -0.0114746000
_diffrn_orient_matrix_UB_22      -0.0200396000
_diffrn_orient_matrix_UB_23      0.0587146000
_diffrn_orient_matrix_UB_31      0.0688986000
_diffrn_orient_matrix_UB_32      -0.0096162000
_diffrn_orient_matrix_UB_33      0.0023694000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6046
_reflns_number_total             7689
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         7689
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0383
_refine_ls_restrained_S_all      1.010
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0378P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0902
_refine_ls_wR_factor_ref         0.0961
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
2. Restrained distances
 C2A-F1A \\sim F1A-C2
 with sigma of 0.02
 C2-C1 \\sim C1-C2A
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C1, C2A, F1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H1AA)=Sof(H1AB)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=1-FVAR(1)
 Sof(H1BC)=Sof(H1BD)=Sof(C2)=Sof(H2A)=Sof(H2B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C7(H7A,H7B), C6(H6A,H6B), C3(H3A,H3B), C4(H4A,H4B), C11(H11A,
 H11B), C8(H8A,H8B), C13(H13A,H13B), C12(H12A,H12B), C14(H14A,H14B), C1(H1BC,
 H1BD), C1(H1AA,H1AB), C9(H9A,H9B), C10(H10A,H10B), C2(H2A,H2B), C2A(H2AA,H2AB)
5.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.16521(2) 0.40774(2) 0.48835(2) 0.01701(8) Uani 1 1 d . . . . .
S2 S -0.07759(5) 0.26571(4) 0.29588(4) 0.01933(12) Uani 1 1 d . . . . .
S4 S 0.01070(5) 0.31309(4) 0.48625(4) 0.01944(11) Uani 1 1 d . . . . .
S6 S 0.10319(5) 0.36978(4) 0.66459(4) 0.02045(12) Uani 1 1 d . . . . .
S5 S 0.23078(5) 0.44281(4) 0.31260(4) 0.02106(12) Uani 1 1 d . . . . .
S8 S 0.19922(5) 0.43814(4) 0.83938(4) 0.02084(12) Uani 1 1 d . . . . .
S3 S 0.12922(5) 0.37880(5) 0.13761(4) 0.02277(12) Uani 1 1 d . . . . .
S9 S 0.40115(5) 0.55798(4) 0.67983(5) 0.02220(12) Uani 1 1 d . . . . .
S7 S 0.31404(5) 0.50808(4) 0.49018(4) 0.02042(12) Uani 1 1 d . . . . .
S10 S 0.37830(6) 0.55114(5) 0.91401(5) 0.02780(14) Uani 1 1 d . . . . .
S1 S -0.04950(6) 0.26538(5) 0.06283(5) 0.02880(14) Uani 1 1 d . . . . .
O2 O 0.16551(13) 0.89455(11) 0.28666(13) 0.0224(3) Uani 1 1 d . . . . .
O3 O 0.26672(14) 1.06395(12) 0.32891(13) 0.0231(3) Uani 1 1 d . . . . .
N1 N 0.44406(16) 0.89044(13) 0.25173(14) 0.0194(4) Uani 1 1 d . . . . .
H1A H 0.411890 0.877242 0.196736 0.023 Uiso 1 1 calc R U . . .
H1B H 0.514632 0.929753 0.222501 0.023 Uiso 1 1 calc R U . . .
H1C H 0.380364 0.931655 0.284996 0.023 Uiso 1 1 calc R U . . .
O5 O 0.68793(14) 0.97784(12) 0.13852(13) 0.0257(3) Uani 1 1 d . . . . .
O1 O 0.31451(14) 0.80797(12) 0.12239(13) 0.0238(3) Uani 1 1 d . . . . .
O6 O 0.58981(14) 0.81450(12) 0.07946(13) 0.0254(3) Uani 1 1 d . . . . .
O4 O 0.54401(14) 1.07184(12) 0.29475(14) 0.0261(3) Uani 1 1 d . . . . .
C16 C 0.02611(19) 0.32456(16) 0.34849(17) 0.0181(4) Uani 1 1 d . . . . .
C18 C 0.2065(2) 0.43844(17) 0.70314(17) 0.0189(4) Uani 1 1 d . . . . .
C19 C 0.29911(19) 0.49669(16) 0.62803(17) 0.0189(4) Uani 1 1 d . . . . .
C17 C 0.1219(2) 0.37914(17) 0.27352(17) 0.0187(4) Uani 1 1 d . . . . .
C20 C 0.3276(2) 0.51835(16) 0.81619(18) 0.0200(4) Uani 1 1 d . . . . .
C15 C -0.0011(2) 0.30111(17) 0.16017(18) 0.0218(4) Uani 1 1 d . . . . .
C5 C 0.0825(2) 0.98038(18) 0.32253(19) 0.0250(5) Uani 1 1 d . . . . .
H5A H -0.000194 0.951243 0.364632 0.030 Uiso 1 1 calc R U . . .
H5B H 0.060003 1.046558 0.257725 0.030 Uiso 1 1 calc R U . . .
C7 C 0.3321(2) 1.11483(18) 0.38566(19) 0.0245(5) Uani 1 1 d . . . . .
H7A H 0.361108 1.057147 0.453891 0.029 Uiso 1 1 calc R U . . .
H7B H 0.271095 1.175616 0.406832 0.029 Uiso 1 1 calc R U . . .
C6 C 0.1540(2) 1.01507(18) 0.39481(18) 0.0243(5) Uani 1 1 d . . . . .
H6A H 0.095752 1.070926 0.425436 0.029 Uiso 1 1 calc R U . . .
H6B H 0.181168 0.948122 0.457325 0.029 Uiso 1 1 calc R U . . .
C3 C 0.1969(2) 0.76454(17) 0.1858(2) 0.0260(5) Uani 1 1 d . . . . .
H3A H 0.218385 0.703046 0.254381 0.031 Uiso 1 1 calc R U . . .
H3B H 0.153386 0.733132 0.142335 0.031 Uiso 1 1 calc R U . . .
C4 C 0.1070(2) 0.85973(18) 0.21425(19) 0.0241(5) Uani 1 1 d . . . . .
H4A H 0.092578 0.924160 0.145948 0.029 Uiso 1 1 calc R U . . .
H4B H 0.020693 0.834111 0.250597 0.029 Uiso 1 1 calc R U . . .
C11 C 0.7711(2) 0.90079(19) 0.0899(2) 0.0289(5) Uani 1 1 d . . . . .
H11A H 0.799286 0.830413 0.148512 0.035 Uiso 1 1 calc R U . . .
H11B H 0.850739 0.935298 0.047221 0.035 Uiso 1 1 calc R U . . .
C8 C 0.4489(2) 1.16334(17) 0.3092(2) 0.0249(5) Uani 1 1 d . . . . .
H8A H 0.421518 1.212431 0.236751 0.030 Uiso 1 1 calc R U . . .
H8B H 0.487338 1.209885 0.341182 0.030 Uiso 1 1 calc R U . . .
C13 C 0.5198(2) 0.77678(19) 0.01521(19) 0.0281(5) Uani 1 1 d . . . . .
H13A H 0.578538 0.721118 -0.015390 0.034 Uiso 1 1 calc R U . . .
H13B H 0.489173 0.841942 -0.047392 0.034 Uiso 1 1 calc R U . . .
C12 C 0.6965(2) 0.8735(2) 0.01431(19) 0.0298(5) Uani 1 1 d . . . . .
H12A H 0.662669 0.944351 -0.041051 0.036 Uiso 1 1 calc R U . . .
H12B H 0.755508 0.825781 -0.025657 0.036 Uiso 1 1 calc R U . . .
C14 C 0.4044(2) 0.72309(18) 0.0880(2) 0.0287(5) Uani 1 1 d . . . . .
H14A H 0.360009 0.689550 0.046951 0.034 Uiso 1 1 calc R U . . .
H14B H 0.434501 0.661762 0.153661 0.034 Uiso 1 1 calc R U . . .
C1 C 0.4856(3) 0.77978(18) 0.3355(2) 0.0309(5) Uani 1 1 d D . . . .
H1BC H 0.414020 0.731043 0.356197 0.037 Uiso 0.925(6) 1 calc R U P A 2
H1BD H 0.564172 0.740554 0.302179 0.037 Uiso 0.925(6) 1 calc R U P A 2
H1AA H 0.482371 0.717245 0.306513 0.037 Uiso 0.075(6) 1 calc R U P A 1
H1AB H 0.577885 0.778048 0.346809 0.037 Uiso 0.075(6) 1 calc R U P A 1
C9 C 0.6670(2) 1.10942(19) 0.2375(2) 0.0309(5) Uani 1 1 d . . . . .
H9A H 0.710677 1.135466 0.285141 0.037 Uiso 1 1 calc R U . . .
H9B H 0.652169 1.173632 0.169130 0.037 Uiso 1 1 calc R U . . .
C10 C 0.7525(2) 1.0119(2) 0.2089(2) 0.0312(5) Uani 1 1 d . . . . .
H10A H 0.839115 1.035415 0.170432 0.037 Uiso 1 1 calc R U . . .
H10B H 0.767309 0.947722 0.277291 0.037 Uiso 1 1 calc R U . . .
C2 C 0.5167(2) 0.7954(2) 0.4358(2) 0.0288(7) Uani 0.925(6) 1 d D . P A 2
H2A H 0.552061 0.721586 0.486059 0.035 Uiso 0.925(6) 1 calc R U P A 2
H2B H 0.584806 0.847529 0.415158 0.035 Uiso 0.925(6) 1 calc R U P A 2
C2A C 0.403(4) 0.761(2) 0.441(2) 0.060(9) Uani 0.075(6) 1 d D . P A 1
H2AA H 0.311099 0.761137 0.429709 0.072 Uiso 0.075(6) 1 calc R U P A 1
H2AB H 0.432282 0.685677 0.491818 0.072 Uiso 0.075(6) 1 calc R U P A 1
F1A F 0.40456(17) 0.83981(14) 0.48933(13) 0.0536(5) Uani 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S4 2.1690(5) . ?
Ni1 S6 2.1663(6) . ?
Ni1 S5 2.1697(6) . ?
Ni1 S7 2.1691(5) . ?
S2 C16 1.7468(19) . ?
S2 C15 1.736(2) . ?
S4 C16 1.719(2) . ?
S6 C18 1.719(2) . ?
S5 C17 1.723(2) . ?
S8 C18 1.749(2) . ?
S8 C20 1.736(2) . ?
S3 C17 1.748(2) . ?
S3 C15 1.733(2) . ?
S9 C19 1.7477(19) . ?
S9 C20 1.734(2) . ?
S7 C19 1.721(2) . ?
S10 C20 1.647(2) . ?
S1 C15 1.651(2) . ?
O2 C5 1.419(2) . ?
O2 C4 1.418(2) . ?
O3 C7 1.434(2) . ?
O3 C6 1.422(3) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N1 C1 1.496(3) . ?
O5 C11 1.424(3) . ?
O5 C10 1.429(3) . ?
O1 C3 1.429(3) . ?
O1 C14 1.433(3) . ?
O6 C13 1.430(3) . ?
O6 C12 1.423(3) . ?
O4 C8 1.426(3) . ?
O4 C9 1.431(3) . ?
C16 C17 1.361(3) . ?
C18 C19 1.357(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.500(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.501(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.499(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.503(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.495(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C1 H1BC 0.9900 . ?
C1 H1BD 0.9900 . ?
C1 H1AA 0.9900 . ?
C1 H1AB 0.9900 . ?
C1 C2 1.472(3) . ?
C1 C2A 1.450(19) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.503(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 F1A 1.382(3) . ?
C2A H2AA 0.9900 . ?
C2A H2AB 0.9900 . ?
C2A F1A 1.342(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S4 Ni1 S5 93.30(2) . . ?
S4 Ni1 S7 177.78(2) . . ?
S6 Ni1 S4 86.90(2) . . ?
S6 Ni1 S5 178.77(2) . . ?
S6 Ni1 S7 92.78(2) . . ?
S7 Ni1 S5 87.06(2) . . ?
C15 S2 C16 97.51(10) . . ?
C16 S4 Ni1 101.86(7) . . ?
C18 S6 Ni1 102.50(8) . . ?
C17 S5 Ni1 101.97(8) . . ?
C20 S8 C18 97.06(10) . . ?
C15 S3 C17 97.24(10) . . ?
C20 S9 C19 97.17(10) . . ?
C19 S7 Ni1 102.30(7) . . ?
C4 O2 C5 112.16(14) . . ?
C6 O3 C7 112.62(17) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
C11 O5 C10 112.85(15) . . ?
C3 O1 C14 112.05(16) . . ?
C12 O6 C13 112.32(17) . . ?
C8 O4 C9 112.19(16) . . ?
S4 C16 S2 122.59(13) . . ?
C17 C16 S2 115.70(16) . . ?
C17 C16 S4 121.70(15) . . ?
S6 C18 S8 122.70(13) . . ?
C19 C18 S6 121.13(16) . . ?
C19 C18 S8 116.17(15) . . ?
S7 C19 S9 122.59(13) . . ?
C18 C19 S9 116.16(16) . . ?
C18 C19 S7 121.25(15) . . ?
S5 C17 S3 122.49(13) . . ?
C16 C17 S5 121.12(16) . . ?
C16 C17 S3 116.38(15) . . ?
S9 C20 S8 113.38(11) . . ?
S10 C20 S8 123.76(14) . . ?
S10 C20 S9 122.84(13) . . ?
S3 C15 S2 113.10(12) . . ?
S1 C15 S2 123.07(13) . . ?
S1 C15 S3 123.82(14) . . ?
O2 C5 H5A 110.0 . . ?
O2 C5 H5B 110.0 . . ?
O2 C5 C6 108.50(15) . . ?
H5A C5 H5B 108.4 . . ?
C6 C5 H5A 110.0 . . ?
C6 C5 H5B 110.0 . . ?
O3 C7 H7A 110.1 . . ?
O3 C7 H7B 110.1 . . ?
O3 C7 C8 108.21(18) . . ?
H7A C7 H7B 108.4 . . ?
C8 C7 H7A 110.1 . . ?
C8 C7 H7B 110.1 . . ?
O3 C6 C5 108.03(18) . . ?
O3 C6 H6A 110.1 . . ?
O3 C6 H6B 110.1 . . ?
C5 C6 H6A 110.1 . . ?
C5 C6 H6B 110.1 . . ?
H6A C6 H6B 108.4 . . ?
O1 C3 H3A 110.0 . . ?
O1 C3 H3B 110.0 . . ?
O1 C3 C4 108.32(17) . . ?
H3A C3 H3B 108.4 . . ?
C4 C3 H3A 110.0 . . ?
C4 C3 H3B 110.0 . . ?
O2 C4 C3 108.83(15) . . ?
O2 C4 H4A 109.9 . . ?
O2 C4 H4B 109.9 . . ?
C3 C4 H4A 109.9 . . ?
C3 C4 H4B 109.9 . . ?
H4A C4 H4B 108.3 . . ?
O5 C11 H11A 109.9 . . ?
O5 C11 H11B 109.9 . . ?
O5 C11 C12 108.94(16) . . ?
H11A C11 H11B 108.3 . . ?
C12 C11 H11A 109.9 . . ?
C12 C11 H11B 109.9 . . ?
O4 C8 C7 108.49(17) . . ?
O4 C8 H8A 110.0 . . ?
O4 C8 H8B 110.0 . . ?
C7 C8 H8A 110.0 . . ?
C7 C8 H8B 110.0 . . ?
H8A C8 H8B 108.4 . . ?
O6 C13 H13A 109.9 . . ?
O6 C13 H13B 109.9 . . ?
O6 C13 C14 108.79(18) . . ?
H13A C13 H13B 108.3 . . ?
C14 C13 H13A 109.9 . . ?
C14 C13 H13B 109.9 . . ?
O6 C12 C11 108.58(19) . . ?
O6 C12 H12A 110.0 . . ?
O6 C12 H12B 110.0 . . ?
C11 C12 H12A 110.0 . . ?
C11 C12 H12B 110.0 . . ?
H12A C12 H12B 108.4 . . ?
O1 C14 C13 108.90(18) . . ?
O1 C14 H14A 109.9 . . ?
O1 C14 H14B 109.9 . . ?
C13 C14 H14A 109.9 . . ?
C13 C14 H14B 109.9 . . ?
H14A C14 H14B 108.3 . . ?
N1 C1 H1BC 109.2 . . ?
N1 C1 H1BD 109.2 . . ?
N1 C1 H1AA 109.1 . . ?
N1 C1 H1AB 109.1 . . ?
H1BC C1 H1BD 107.9 . . ?
H1AA C1 H1AB 107.8 . . ?
C2 C1 N1 111.86(18) . . ?
C2 C1 H1BC 109.2 . . ?
C2 C1 H1BD 109.2 . . ?
C2A C1 N1 112.5(14) . . ?
C2A C1 H1AA 109.1 . . ?
C2A C1 H1AB 109.1 . . ?
O4 C9 H9A 110.0 . . ?
O4 C9 H9B 110.0 . . ?
O4 C9 C10 108.43(18) . . ?
H9A C9 H9B 108.4 . . ?
C10 C9 H9A 110.0 . . ?
C10 C9 H9B 110.0 . . ?
O5 C10 C9 108.59(16) . . ?
O5 C10 H10A 110.0 . . ?
O5 C10 H10B 110.0 . . ?
C9 C10 H10A 110.0 . . ?
C9 C10 H10B 110.0 . . ?
H10A C10 H10B 108.4 . . ?
C1 C2 H2A 109.7 . . ?
C1 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
F1A C2 C1 109.96(19) . . ?
F1A C2 H2A 109.7 . . ?
F1A C2 H2B 109.7 . . ?
C1 C2A H2AA 108.8 . . ?
C1 C2A H2AB 108.8 . . ?
H2AA C2A H2AB 107.7 . . ?
F1A C2A C1 113.7(16) . . ?
F1A C2A H2AA 108.8 . . ?
F1A C2A H2AB 108.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S4 C16 S2 -178.61(10) . . . . ?
Ni1 S4 C16 C17 2.37(17) . . . . ?
Ni1 S6 C18 S8 179.22(10) . . . . ?
Ni1 S6 C18 C19 -0.66(17) . . . . ?
Ni1 S5 C17 S3 -179.17(10) . . . . ?
Ni1 S5 C17 C16 -0.15(17) . . . . ?
Ni1 S7 C19 S9 177.60(10) . . . . ?
Ni1 S7 C19 C18 -2.13(17) . . . . ?
S2 C16 C17 S5 179.32(10) . . . . ?
S2 C16 C17 S3 -1.6(2) . . . . ?
S4 C16 C17 S5 -1.6(2) . . . . ?
S4 C16 C17 S3 177.48(10) . . . . ?
S6 C18 C19 S9 -177.76(10) . . . . ?
S6 C18 C19 S7 2.0(2) . . . . ?
S8 C18 C19 S9 2.4(2) . . . . ?
S8 C18 C19 S7 -177.89(10) . . . . ?
O2 C5 C6 O3 63.9(2) . . . . ?
O3 C7 C8 O4 -68.94(19) . . . . ?
N1 C1 C2 F1A 64.8(3) . . . . ?
N1 C1 C2A F1A -61(3) . . . . ?
O5 C11 C12 O6 -65.0(2) . . . . ?
O1 C3 C4 O2 -66.2(2) . . . . ?
O6 C13 C14 O1 65.2(2) . . . . ?
O4 C9 C10 O5 60.7(2) . . . . ?
C16 S2 C15 S3 -2.64(12) . . . . ?
C16 S2 C15 S1 178.10(13) . . . . ?
C18 S8 C20 S9 -0.78(12) . . . . ?
C18 S8 C20 S10 -179.17(12) . . . . ?
C19 S9 C20 S8 1.77(12) . . . . ?
C19 S9 C20 S10 -179.81(13) . . . . ?
C17 S3 C15 S2 1.95(13) . . . . ?
C17 S3 C15 S1 -178.80(13) . . . . ?
C20 S8 C18 S6 179.17(12) . . . . ?
C20 S8 C18 C19 -0.94(17) . . . . ?
C20 S9 C19 S7 177.74(12) . . . . ?
C20 S9 C19 C18 -2.50(17) . . . . ?
C15 S2 C16 S4 -176.50(12) . . . . ?
C15 S2 C16 C17 2.58(17) . . . . ?
C15 S3 C17 S5 178.83(12) . . . . ?
C15 S3 C17 C16 -0.23(17) . . . . ?
C5 O2 C4 C3 -176.61(18) . . . . ?
C7 O3 C6 C5 171.64(15) . . . . ?
C6 O3 C7 C8 179.91(15) . . . . ?
C3 O1 C14 C13 175.72(16) . . . . ?
C4 O2 C5 C6 -177.82(18) . . . . ?
C11 O5 C10 C9 168.84(19) . . . . ?
C8 O4 C9 C10 -170.42(17) . . . . ?
C13 O6 C12 C11 -175.11(16) . . . . ?
C12 O6 C13 C14 -176.12(16) . . . . ?
C14 O1 C3 C4 -177.85(16) . . . . ?
C9 O4 C8 C7 -170.63(17) . . . . ?
C10 O5 C11 C12 -177.85(19) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.105
_oxdiff_exptl_absorpt_empirical_full_min 0.357
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_253k
_database_code_depnum_ccdc_archive 'CCDC 2053290'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-19 downloaded from the CCDC.
;
_audit_creation_date             2020-11-11
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C12 H24 O6, C2 H7 F N'
_chemical_formula_sum            'C20 H31 F N Ni O6 S10'
_chemical_formula_weight         779.77
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHNOFNiS
_chemical_oxdiff_usercomment     20_20200608
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.4754(3)
_cell_length_b                   12.6503(4)
_cell_length_c                   12.9637(4)
_cell_angle_alpha                71.385(3)
_cell_angle_beta                 79.802(2)
_cell_angle_gamma                80.550(2)
_cell_volume                     1591.61(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    10478
_cell_measurement_temperature    253
_cell_measurement_theta_max      30.2190
_cell_measurement_theta_min      2.0070
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.308
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70450
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             806
_exptl_crystal_size_max          0.507
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.796
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19688
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.796
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.670
_diffrn_reflns_theta_min         1.989
_diffrn_ambient_temperature      253
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.796
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     26.00  72.00   0.50    0.32    --    5.18  37.00 -30.00   92
  2  ω    -44.00  10.00   0.50    0.32    --   -4.95 -57.00-120.00  108
  3  ω    -18.00  23.00   0.50    0.32    --   -4.95 -99.00-150.00   82
  4  ω    -12.00  39.00   0.50    0.32    --    5.18 -99.00  60.00  102
  5  ω    -74.00   6.00   0.50    0.32    --   -4.95 -37.00 120.00  160
  6  ω    -11.00  68.00   0.50    0.32    --   -4.95  37.00  60.00  158
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0026392000
_diffrn_orient_matrix_UB_12      0.0547622000
_diffrn_orient_matrix_UB_13      0.0045116000
_diffrn_orient_matrix_UB_21      -0.0104241000
_diffrn_orient_matrix_UB_22      -0.0219485000
_diffrn_orient_matrix_UB_23      0.0580682000
_diffrn_orient_matrix_UB_31      0.0684213000
_diffrn_orient_matrix_UB_32      -0.0081922000
_diffrn_orient_matrix_UB_33      0.0011581000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5764
_reflns_number_total             7844
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         7844
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0343
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0325P)²+0.1433P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0872
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
2. Others
 Sof(H1AA)=Sof(H1AB)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(F1)=1-FVAR(1)
 Sof(H1BC)=Sof(H1BD)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(F1A)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C7(H7A,H7B), C6(H6A,H6B), C3(H3A,H3B), C4(H4A,H4B), C11(H11A,
 H11B), C8(H8A,H8B), C13(H13A,H13B), C12(H12A,H12B), C14(H14A,H14B), C1(H1BC,
 H1BD), C1(H1AA,H1AB), C9(H9A,H9B), C10(H10A,H10B), C2(H2A,H2B), C2A(H2AA,H2AB)
3.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.16314(2) 0.40477(2) 0.49172(2) 0.03311(8) Uani 1 1 d . . . . .
S2 S -0.07960(5) 0.26665(4) 0.29622(4) 0.03777(12) Uani 1 1 d . . . . .
S4 S 0.00654(5) 0.31439(4) 0.48688(4) 0.03752(12) Uani 1 1 d . . . . .
S6 S 0.10007(5) 0.36905(4) 0.66646(4) 0.03985(13) Uani 1 1 d . . . . .
S5 S 0.22903(5) 0.43909(4) 0.31733(4) 0.04028(12) Uani 1 1 d . . . . .
S8 S 0.19585(5) 0.43704(4) 0.84134(4) 0.04164(13) Uani 1 1 d . . . . .
S3 S 0.12877(5) 0.37506(5) 0.14193(5) 0.04426(13) Uani 1 1 d . . . . .
S9 S 0.40165(5) 0.54921(5) 0.68627(5) 0.04516(14) Uani 1 1 d . . . . .
S7 S 0.31569(5) 0.49923(5) 0.49612(5) 0.04300(13) Uani 1 1 d . . . . .
S10 S 0.37510(6) 0.54722(5) 0.91799(5) 0.05562(16) Uani 1 1 d . . . . .
S1 S -0.04946(6) 0.26393(6) 0.06480(5) 0.05639(16) Uani 1 1 d . . . . .
O2 O 0.16867(13) 0.89579(11) 0.28469(13) 0.0451(4) Uani 1 1 d . . . . .
O3 O 0.26754(14) 1.06507(12) 0.32985(13) 0.0471(4) Uani 1 1 d . . . . .
N1 N 0.44671(15) 0.89072(13) 0.25371(14) 0.0362(4) Uani 1 1 d . . . . .
H1A H 0.403062 0.876193 0.207734 0.043 Uiso 1 1 calc R U . . .
H1B H 0.515340 0.925537 0.215952 0.043 Uiso 1 1 calc R U . . .
H1C H 0.394582 0.934518 0.289258 0.043 Uiso 1 1 calc R U . . .
O5 O 0.68737(14) 0.98007(13) 0.13997(14) 0.0526(4) Uani 1 1 d . . . . .
O1 O 0.31843(15) 0.80848(11) 0.12221(14) 0.0483(4) Uani 1 1 d . . . . .
O6 O 0.59009(15) 0.81777(13) 0.07799(13) 0.0521(4) Uani 1 1 d . . . . .
O4 O 0.54117(14) 1.07271(12) 0.29769(15) 0.0520(4) Uani 1 1 d . . . . .
C16 C 0.02356(18) 0.32449(15) 0.35022(17) 0.0329(4) Uani 1 1 d . . . . .
C18 C 0.20467(19) 0.43533(15) 0.70608(16) 0.0340(4) Uani 1 1 d . . . . .
C19 C 0.29931(18) 0.49001(16) 0.63272(17) 0.0367(4) Uani 1 1 d . . . . .
C17 C 0.12049(18) 0.37688(15) 0.27668(17) 0.0349(4) Uani 1 1 d . . . . .
C20 C 0.32571(19) 0.51360(16) 0.82048(18) 0.0386(4) Uani 1 1 d . . . . .
C15 C -0.00225(19) 0.29954(17) 0.16272(18) 0.0398(5) Uani 1 1 d . . . . .
C5 C 0.0863(2) 0.98188(18) 0.3205(2) 0.0503(6) Uani 1 1 d . . . . .
H5A H 0.005024 0.954200 0.360418 0.060 Uiso 1 1 calc R U . . .
H5B H 0.066130 1.045370 0.257696 0.060 Uiso 1 1 calc R U . . .
C7 C 0.3317(2) 1.11509(19) 0.3881(2) 0.0526(6) Uani 1 1 d . . . . .
H7A H 0.358695 1.059038 0.453770 0.063 Uiso 1 1 calc R U . . .
H7B H 0.272585 1.174027 0.409987 0.063 Uiso 1 1 calc R U . . .
C6 C 0.1544(2) 1.0173(2) 0.3929(2) 0.0517(6) Uani 1 1 d . . . . .
H6A H 0.097101 1.072124 0.422594 0.062 Uiso 1 1 calc R U . . .
H6B H 0.178885 0.953091 0.453636 0.062 Uiso 1 1 calc R U . . .
C3 C 0.2010(2) 0.76544(18) 0.1838(2) 0.0545(6) Uani 1 1 d . . . . .
H3A H 0.220760 0.706119 0.249846 0.065 Uiso 1 1 calc R U . . .
H3B H 0.159670 0.734499 0.140337 0.065 Uiso 1 1 calc R U . . .
C4 C 0.1119(2) 0.85888(18) 0.2132(2) 0.0504(6) Uani 1 1 d . . . . .
H4A H 0.097407 0.920422 0.147374 0.061 Uiso 1 1 calc R U . . .
H4B H 0.028238 0.833240 0.248924 0.061 Uiso 1 1 calc R U . . .
C11 C 0.7699(2) 0.9031(2) 0.0910(2) 0.0616(7) Uani 1 1 d . . . . .
H11A H 0.796511 0.835337 0.147433 0.074 Uiso 1 1 calc R U . . .
H11B H 0.847615 0.936283 0.049681 0.074 Uiso 1 1 calc R U . . .
C8 C 0.4475(2) 1.16259(18) 0.3147(2) 0.0535(6) Uani 1 1 d . . . . .
H8A H 0.422077 1.210855 0.244914 0.064 Uiso 1 1 calc R U . . .
H8B H 0.484832 1.207118 0.347810 0.064 Uiso 1 1 calc R U . . .
C13 C 0.5194(3) 0.7803(2) 0.0135(2) 0.0612(7) Uani 1 1 d . . . . .
H13A H 0.576173 0.727035 -0.018587 0.073 Uiso 1 1 calc R U . . .
H13B H 0.489419 0.843749 -0.045778 0.073 Uiso 1 1 calc R U . . .
C12 C 0.6961(2) 0.8751(2) 0.0162(2) 0.0630(7) Uani 1 1 d . . . . .
H12A H 0.664407 0.943548 -0.037046 0.076 Uiso 1 1 calc R U . . .
H12B H 0.753474 0.828452 -0.023456 0.076 Uiso 1 1 calc R U . . .
C14 C 0.4063(3) 0.7267(2) 0.0840(2) 0.0611(7) Uani 1 1 d . . . . .
H14A H 0.362665 0.695196 0.042489 0.073 Uiso 1 1 calc R U . . .
H14B H 0.435646 0.666259 0.145876 0.073 Uiso 1 1 calc R U . . .
C1 C 0.4921(3) 0.7836(2) 0.3343(2) 0.0651(7) Uani 1 1 d . . . . .
H1BC H 0.429289 0.730841 0.347013 0.078 Uiso 0.637(8) 1 calc R U P A 2
H1BD H 0.574388 0.752443 0.301812 0.078 Uiso 0.637(8) 1 calc R U P A 2
H1AA H 0.493541 0.722297 0.304157 0.078 Uiso 0.363(8) 1 calc R U P A 1
H1AB H 0.580793 0.786418 0.344663 0.078 Uiso 0.363(8) 1 calc R U P A 1
C9 C 0.6628(2) 1.1099(2) 0.2420(2) 0.0608(7) Uani 1 1 d . . . . .
H9A H 0.704425 1.135987 0.289046 0.073 Uiso 1 1 calc R U . . .
H9B H 0.648984 1.171831 0.176215 0.073 Uiso 1 1 calc R U . . .
C10 C 0.7485(2) 1.0140(2) 0.2118(2) 0.0615(7) Uani 1 1 d . . . . .
H10A H 0.833162 1.037212 0.175874 0.074 Uiso 1 1 calc R U . . .
H10B H 0.761546 0.951743 0.277466 0.074 Uiso 1 1 calc R U . . .
C2 C 0.5095(5) 0.7924(4) 0.4363(4) 0.0630(17) Uani 0.637(8) 1 d . . P A 2
H2A H 0.560169 0.853493 0.425958 0.076 Uiso 0.637(8) 1 calc R U P A 2
H2B H 0.554431 0.723215 0.478916 0.076 Uiso 0.637(8) 1 calc R U P A 2
C2A C 0.4144(9) 0.7614(6) 0.4358(7) 0.054(2) Uani 0.363(8) 1 d . . P A 1
H2AA H 0.449825 0.691056 0.484171 0.065 Uiso 0.363(8) 1 calc R U P A 1
H2AB H 0.327212 0.752754 0.426428 0.065 Uiso 0.363(8) 1 calc R U P A 1
F1A F 0.4063(12) 0.8467(8) 0.4853(8) 0.085(3) Uani 0.637(8) 1 d . . P A 1
F1 F 0.3765(19) 0.8144(14) 0.4923(15) 0.084(4) Uani 0.363(8) 1 d . . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S4 2.1681(5) . ?
Ni1 S6 2.1649(6) . ?
Ni1 S5 2.1669(6) . ?
Ni1 S7 2.1651(5) . ?
S2 C16 1.7457(18) . ?
S2 C15 1.726(2) . ?
S4 C16 1.714(2) . ?
S6 C18 1.7156(18) . ?
S5 C17 1.7205(18) . ?
S8 C18 1.746(2) . ?
S8 C20 1.731(2) . ?
S3 C17 1.741(2) . ?
S3 C15 1.733(2) . ?
S9 C19 1.7468(18) . ?
S9 C20 1.729(2) . ?
S7 C19 1.716(2) . ?
S10 C20 1.641(2) . ?
S1 C15 1.649(2) . ?
O2 C5 1.421(3) . ?
O2 C4 1.411(2) . ?
O3 C7 1.431(2) . ?
O3 C6 1.419(3) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.488(3) . ?
O5 C11 1.423(3) . ?
O5 C10 1.421(3) . ?
O1 C3 1.429(3) . ?
O1 C14 1.420(3) . ?
O6 C13 1.435(3) . ?
O6 C12 1.407(3) . ?
O4 C8 1.421(3) . ?
O4 C9 1.422(3) . ?
C16 C17 1.362(3) . ?
C18 C19 1.355(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.483(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.485(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.488(3) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.496(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.478(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C1 H1BC 0.9700 . ?
C1 H1BD 0.9700 . ?
C1 H1AA 0.9700 . ?
C1 H1AB 0.9700 . ?
C1 C2 1.407(5) . ?
C1 C2A 1.391(9) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.501(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 F1 1.48(2) . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?
C2A F1A 1.405(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S6 Ni1 S4 87.12(2) . . ?
S6 Ni1 S5 179.16(2) . . ?
S6 Ni1 S7 92.75(2) . . ?
S5 Ni1 S4 93.27(2) . . ?
S7 Ni1 S4 178.40(2) . . ?
S7 Ni1 S5 86.89(2) . . ?
C15 S2 C16 97.67(10) . . ?
C16 S4 Ni1 101.83(7) . . ?
C18 S6 Ni1 102.44(7) . . ?
C17 S5 Ni1 102.08(7) . . ?
C20 S8 C18 97.19(10) . . ?
C15 S3 C17 97.29(10) . . ?
C20 S9 C19 97.40(10) . . ?
C19 S7 Ni1 102.37(7) . . ?
C4 O2 C5 112.40(15) . . ?
C6 O3 C7 112.98(18) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
C10 O5 C11 113.43(17) . . ?
C14 O1 C3 112.52(18) . . ?
C12 O6 C13 113.4(2) . . ?
C8 O4 C9 112.25(18) . . ?
S4 C16 S2 122.60(12) . . ?
C17 C16 S2 115.50(15) . . ?
C17 C16 S4 121.89(14) . . ?
S6 C18 S8 122.58(12) . . ?
C19 C18 S6 121.17(15) . . ?
C19 C18 S8 116.25(14) . . ?
S7 C19 S9 122.91(13) . . ?
C18 C19 S9 115.84(16) . . ?
C18 C19 S7 121.26(14) . . ?
S5 C17 S3 122.72(12) . . ?
C16 C17 S5 120.91(15) . . ?
C16 C17 S3 116.36(14) . . ?
S9 C20 S8 113.26(11) . . ?
S10 C20 S8 123.91(14) . . ?
S10 C20 S9 122.81(12) . . ?
S2 C15 S3 113.11(11) . . ?
S1 C15 S2 123.35(12) . . ?
S1 C15 S3 123.54(14) . . ?
O2 C5 H5A 109.9 . . ?
O2 C5 H5B 109.9 . . ?
O2 C5 C6 108.83(16) . . ?
H5A C5 H5B 108.3 . . ?
C6 C5 H5A 109.9 . . ?
C6 C5 H5B 109.9 . . ?
O3 C7 H7A 110.0 . . ?
O3 C7 H7B 110.0 . . ?
O3 C7 C8 108.4(2) . . ?
H7A C7 H7B 108.4 . . ?
C8 C7 H7A 110.0 . . ?
C8 C7 H7B 110.0 . . ?
O3 C6 C5 108.4(2) . . ?
O3 C6 H6A 110.0 . . ?
O3 C6 H6B 110.0 . . ?
C5 C6 H6A 110.0 . . ?
C5 C6 H6B 110.0 . . ?
H6A C6 H6B 108.4 . . ?
O1 C3 H3A 110.0 . . ?
O1 C3 H3B 110.0 . . ?
O1 C3 C4 108.49(17) . . ?
H3A C3 H3B 108.4 . . ?
C4 C3 H3A 110.0 . . ?
C4 C3 H3B 110.0 . . ?
O2 C4 C3 109.10(16) . . ?
O2 C4 H4A 109.9 . . ?
O2 C4 H4B 109.9 . . ?
C3 C4 H4A 109.9 . . ?
C3 C4 H4B 109.9 . . ?
H4A C4 H4B 108.3 . . ?
O5 C11 H11A 110.0 . . ?
O5 C11 H11B 110.0 . . ?
O5 C11 C12 108.58(18) . . ?
H11A C11 H11B 108.4 . . ?
C12 C11 H11A 110.0 . . ?
C12 C11 H11B 110.0 . . ?
O4 C8 C7 108.72(18) . . ?
O4 C8 H8A 109.9 . . ?
O4 C8 H8B 109.9 . . ?
C7 C8 H8A 109.9 . . ?
C7 C8 H8B 109.9 . . ?
H8A C8 H8B 108.3 . . ?
O6 C13 H13A 109.8 . . ?
O6 C13 H13B 109.8 . . ?
O6 C13 C14 109.5(2) . . ?
H13A C13 H13B 108.2 . . ?
C14 C13 H13A 109.8 . . ?
C14 C13 H13B 109.8 . . ?
O6 C12 C11 109.7(2) . . ?
O6 C12 H12A 109.7 . . ?
O6 C12 H12B 109.7 . . ?
C11 C12 H12A 109.7 . . ?
C11 C12 H12B 109.7 . . ?
H12A C12 H12B 108.2 . . ?
O1 C14 C13 109.0(2) . . ?
O1 C14 H14A 109.9 . . ?
O1 C14 H14B 109.9 . . ?
C13 C14 H14A 109.9 . . ?
C13 C14 H14B 109.9 . . ?
H14A C14 H14B 108.3 . . ?
N1 C1 H1BC 108.4 . . ?
N1 C1 H1BD 108.4 . . ?
N1 C1 H1AA 108.9 . . ?
N1 C1 H1AB 108.9 . . ?
H1BC C1 H1BD 107.5 . . ?
H1AA C1 H1AB 107.7 . . ?
C2 C1 N1 115.3(3) . . ?
C2 C1 H1BC 108.4 . . ?
C2 C1 H1BD 108.4 . . ?
C2A C1 N1 113.5(4) . . ?
C2A C1 H1AA 108.9 . . ?
C2A C1 H1AB 108.9 . . ?
O4 C9 H9A 109.9 . . ?
O4 C9 H9B 109.9 . . ?
O4 C9 C10 108.83(18) . . ?
H9A C9 H9B 108.3 . . ?
C10 C9 H9A 109.9 . . ?
C10 C9 H9B 109.9 . . ?
O5 C10 C9 108.72(17) . . ?
O5 C10 H10A 109.9 . . ?
O5 C10 H10B 109.9 . . ?
C9 C10 H10A 109.9 . . ?
C9 C10 H10B 109.9 . . ?
H10A C10 H10B 108.3 . . ?
C1 C2 H2A 110.6 . . ?
C1 C2 H2B 110.6 . . ?
C1 C2 F1 105.6(8) . . ?
H2A C2 H2B 108.7 . . ?
F1 C2 H2A 110.6 . . ?
F1 C2 H2B 110.6 . . ?
C1 C2A H2AA 109.1 . . ?
C1 C2A H2AB 109.1 . . ?
C1 C2A F1A 112.7(6) . . ?
H2AA C2A H2AB 107.8 . . ?
F1A C2A H2AA 109.1 . . ?
F1A C2A H2AB 109.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S4 C16 S2 -179.42(9) . . . . ?
Ni1 S4 C16 C17 1.73(17) . . . . ?
Ni1 S6 C18 S8 178.46(9) . . . . ?
Ni1 S6 C18 C19 -1.33(17) . . . . ?
Ni1 S5 C17 S3 -178.46(10) . . . . ?
Ni1 S5 C17 C16 0.58(17) . . . . ?
Ni1 S7 C19 S9 178.38(10) . . . . ?
Ni1 S7 C19 C18 -1.54(18) . . . . ?
S2 C16 C17 S5 179.41(9) . . . . ?
S2 C16 C17 S3 -1.5(2) . . . . ?
S4 C16 C17 S5 -1.7(2) . . . . ?
S4 C16 C17 S3 177.44(10) . . . . ?
S6 C18 C19 S9 -177.88(10) . . . . ?
S6 C18 C19 S7 2.0(2) . . . . ?
S8 C18 C19 S9 2.3(2) . . . . ?
S8 C18 C19 S7 -177.75(10) . . . . ?
O2 C5 C6 O3 63.9(2) . . . . ?
O3 C7 C8 O4 -68.5(2) . . . . ?
N1 C1 C2 F1 71.1(7) . . . . ?
N1 C1 C2A F1A -58.3(8) . . . . ?
O5 C11 C12 O6 -64.9(3) . . . . ?
O1 C3 C4 O2 -65.0(2) . . . . ?
O6 C13 C14 O1 64.6(3) . . . . ?
O4 C9 C10 O5 61.5(3) . . . . ?
C16 S2 C15 S3 -2.56(13) . . . . ?
C16 S2 C15 S1 178.12(13) . . . . ?
C18 S8 C20 S9 -0.95(12) . . . . ?
C18 S8 C20 S10 -179.64(12) . . . . ?
C19 S9 C20 S8 1.94(12) . . . . ?
C19 S9 C20 S10 -179.36(12) . . . . ?
C17 S3 C15 S2 1.91(13) . . . . ?
C17 S3 C15 S1 -178.76(13) . . . . ?
C20 S8 C18 S6 179.38(12) . . . . ?
C20 S8 C18 C19 -0.82(17) . . . . ?
C20 S9 C19 S7 177.49(12) . . . . ?
C20 S9 C19 C18 -2.59(17) . . . . ?
C15 S2 C16 S4 -176.46(12) . . . . ?
C15 S2 C16 C17 2.47(17) . . . . ?
C15 S3 C17 S5 178.82(12) . . . . ?
C15 S3 C17 C16 -0.26(17) . . . . ?
C5 O2 C4 C3 -177.3(2) . . . . ?
C7 O3 C6 C5 172.53(16) . . . . ?
C6 O3 C7 C8 -179.70(17) . . . . ?
C3 O1 C14 C13 175.15(19) . . . . ?
C4 O2 C5 C6 -178.74(19) . . . . ?
C11 O5 C10 C9 169.6(2) . . . . ?
C8 O4 C9 C10 -171.3(2) . . . . ?
C13 O6 C12 C11 -175.67(18) . . . . ?
C12 O6 C13 C14 -177.02(19) . . . . ?
C14 O1 C3 C4 -176.04(19) . . . . ?
C9 O4 C8 C7 -171.08(19) . . . . ?
C10 O5 C11 C12 -179.1(2) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.303
_oxdiff_exptl_absorpt_empirical_full_min 0.536
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_193
_database_code_depnum_ccdc_archive 'CCDC 2053287'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-19 downloaded from the CCDC.
;
_audit_creation_date             2020-11-11
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C12 H24 O6, C2 H7 F N'
_chemical_formula_sum            'C20 H31 F N Ni O6 S10'
_chemical_formula_weight         779.77
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHNOFNiS
_chemical_oxdiff_usercomment     20_20200608
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.4204(3)
_cell_length_b                   12.6319(4)
_cell_length_c                   12.9511(4)
_cell_angle_alpha                70.735(3)
_cell_angle_beta                 79.898(2)
_cell_angle_gamma                80.250(2)
_cell_volume                     1572.90(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9571
_cell_measurement_temperature    193
_cell_measurement_theta_max      30.3680
_cell_measurement_theta_min      2.0060
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.323
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71505
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             806
_exptl_crystal_size_max          0.507
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_unetI/netI     0.0700
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.789
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19734
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.789
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.850
_diffrn_reflns_theta_min         1.998
_diffrn_ambient_temperature      193
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.789
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     25.00  74.00   0.50    0.23    --    5.18  37.00  60.00   98
  2  ω    -77.00   5.00   0.50    0.23    --   -4.95 -37.00-150.00  164
  3  ω    -17.00  29.00   0.50    0.23    --   -4.95 -99.00 -60.00   92
  4  ω    -38.00  10.00   0.50    0.23    --   -4.95 -57.00 -30.00   96
  5  ω    -13.00  39.00   0.50    0.23    --    5.18 -99.00 150.00  104
  6  ω     -9.00  68.00   0.50    0.23    --   -4.95  37.00 150.00  154
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0022965000
_diffrn_orient_matrix_UB_12      0.0551232000
_diffrn_orient_matrix_UB_13      0.0036178000
_diffrn_orient_matrix_UB_21      -0.0109255000
_diffrn_orient_matrix_UB_22      -0.0217292000
_diffrn_orient_matrix_UB_23      0.0583618000
_diffrn_orient_matrix_UB_31      0.0687427000
_diffrn_orient_matrix_UB_32      -0.0088927000
_diffrn_orient_matrix_UB_33      0.0017820000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5845
_reflns_number_total             7797
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.450
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         7797
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0414
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0440P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1011
_refine_ls_wR_factor_ref         0.1094
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
2. Others
 Sof(H1AA)=Sof(H1AB)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(F1)=1-FVAR(1)
 Sof(H1BC)=Sof(H1BD)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(F1A)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C7(H7A,H7B), C6(H6A,H6B), C3(H3A,H3B), C4(H4A,H4B), C11(H11A,
 H11B), C8(H8A,H8B), C13(H13A,H13B), C12(H12A,H12B), C14(H14A,H14B), C1(H1BC,
 H1BD), C1(H1AA,H1AB), C9(H9A,H9B), C10(H10A,H10B), C2(H2A,H2B), C2A(H2AA,H2AB)
3.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.16414(2) 0.40625(2) 0.49002(2) 0.02443(9) Uani 1 1 d . . . . .
S2 S -0.07861(5) 0.26622(5) 0.29605(5) 0.02778(13) Uani 1 1 d . . . . .
S4 S 0.00857(5) 0.31370(5) 0.48652(5) 0.02762(13) Uani 1 1 d . . . . .
S6 S 0.10156(5) 0.36924(5) 0.66549(5) 0.02967(14) Uani 1 1 d . . . . .
S5 S 0.22989(5) 0.44103(5) 0.31500(5) 0.03011(14) Uani 1 1 d . . . . .
S8 S 0.19760(6) 0.43731(5) 0.84042(5) 0.03074(14) Uani 1 1 d . . . . .
S3 S 0.12902(5) 0.37694(5) 0.13985(5) 0.03273(14) Uani 1 1 d . . . . .
S9 S 0.40139(5) 0.55364(5) 0.68301(5) 0.03323(15) Uani 1 1 d . . . . .
S7 S 0.31450(5) 0.50397(5) 0.49320(5) 0.03135(14) Uani 1 1 d . . . . .
S10 S 0.37677(6) 0.54893(6) 0.91600(6) 0.04113(17) Uani 1 1 d . . . . .
S1 S -0.04949(6) 0.26450(6) 0.06389(6) 0.04148(17) Uani 1 1 d . . . . .
O2 O 0.16706(14) 0.89526(13) 0.28585(14) 0.0314(4) Uani 1 1 d . . . . .
O3 O 0.26676(15) 1.06488(14) 0.32923(14) 0.0343(4) Uani 1 1 d . . . . .
N1 N 0.44520(17) 0.89051(15) 0.25286(16) 0.0270(4) Uani 1 1 d . . . . .
H1A H 0.410838 0.876912 0.200902 0.032 Uiso 1 1 calc R U . . .
H1B H 0.513469 0.929063 0.222000 0.032 Uiso 1 1 calc R U . . .
H1C H 0.384857 0.930729 0.287045 0.032 Uiso 1 1 calc R U . . .
O5 O 0.68795(14) 0.97899(14) 0.13916(15) 0.0380(4) Uani 1 1 d . . . . .
O1 O 0.31603(15) 0.80812(13) 0.12203(15) 0.0340(4) Uani 1 1 d . . . . .
O6 O 0.58971(15) 0.81631(15) 0.07851(15) 0.0378(4) Uani 1 1 d . . . . .
O4 O 0.54288(15) 1.07188(14) 0.29594(16) 0.0386(4) Uani 1 1 d . . . . .
C16 C 0.02489(19) 0.32426(17) 0.34981(19) 0.0244(5) Uani 1 1 d . . . . .
C18 C 0.2059(2) 0.43668(18) 0.70490(19) 0.0265(5) Uani 1 1 d . . . . .
C19 C 0.2988(2) 0.49306(18) 0.6308(2) 0.0264(5) Uani 1 1 d . . . . .
C17 C 0.1211(2) 0.37801(19) 0.27516(19) 0.0269(5) Uani 1 1 d . . . . .
C20 C 0.3268(2) 0.51553(19) 0.8184(2) 0.0299(5) Uani 1 1 d . . . . .
C15 C -0.0015(2) 0.3003(2) 0.1612(2) 0.0305(5) Uani 1 1 d . . . . .
C5 C 0.0840(2) 0.9814(2) 0.3217(2) 0.0360(6) Uani 1 1 d . . . . .
H5A H 0.002789 0.953291 0.362280 0.043 Uiso 1 1 calc R U . . .
H5B H 0.062769 1.045639 0.258536 0.043 Uiso 1 1 calc R U . . .
C7 C 0.3320(2) 1.1144(2) 0.3873(2) 0.0358(6) Uani 1 1 d . . . . .
H7A H 0.360221 1.057531 0.453086 0.043 Uiso 1 1 calc R U . . .
H7B H 0.272621 1.173346 0.409420 0.043 Uiso 1 1 calc R U . . .
C6 C 0.1542(2) 1.0163(2) 0.3940(2) 0.0358(6) Uani 1 1 d . . . . .
H6A H 0.097017 1.070979 0.424182 0.043 Uiso 1 1 calc R U . . .
H6B H 0.180243 0.951284 0.454791 0.043 Uiso 1 1 calc R U . . .
C3 C 0.1992(2) 0.7648(2) 0.1849(2) 0.0367(6) Uani 1 1 d . . . . .
H3A H 0.220149 0.705168 0.251540 0.044 Uiso 1 1 calc R U . . .
H3B H 0.156960 0.733586 0.142308 0.044 Uiso 1 1 calc R U . . .
C4 C 0.1092(2) 0.8596(2) 0.2139(2) 0.0346(5) Uani 1 1 d . . . . .
H4A H 0.094901 0.921994 0.147540 0.042 Uiso 1 1 calc R U . . .
H4B H 0.025003 0.834279 0.249534 0.042 Uiso 1 1 calc R U . . .
C11 C 0.7709(2) 0.9018(2) 0.0898(2) 0.0427(6) Uani 1 1 d . . . . .
H11A H 0.798154 0.833261 0.146575 0.051 Uiso 1 1 calc R U . . .
H11B H 0.848802 0.935333 0.048264 0.051 Uiso 1 1 calc R U . . .
C8 C 0.4482(2) 1.1630(2) 0.3120(2) 0.0381(6) Uani 1 1 d . . . . .
H8A H 0.421700 1.211424 0.241807 0.046 Uiso 1 1 calc R U . . .
H8B H 0.485907 1.207968 0.344311 0.046 Uiso 1 1 calc R U . . .
C13 C 0.5195(2) 0.7796(2) 0.0138(2) 0.0431(7) Uani 1 1 d . . . . .
H13A H 0.576886 0.726397 -0.018148 0.052 Uiso 1 1 calc R U . . .
H13B H 0.488526 0.843641 -0.045684 0.052 Uiso 1 1 calc R U . . .
C12 C 0.6962(2) 0.8746(2) 0.0146(2) 0.0445(7) Uani 1 1 d . . . . .
H12A H 0.663523 0.943747 -0.038910 0.053 Uiso 1 1 calc R U . . .
H12B H 0.753611 0.827983 -0.025065 0.053 Uiso 1 1 calc R U . . .
C14 C 0.4055(3) 0.7243(2) 0.0863(2) 0.0424(6) Uani 1 1 d . . . . .
H14A H 0.362216 0.691444 0.045799 0.051 Uiso 1 1 calc R U . . .
H14B H 0.435522 0.664523 0.149556 0.051 Uiso 1 1 calc R U . . .
C1 C 0.4892(3) 0.7820(2) 0.3338(2) 0.0469(7) Uani 1 1 d . . . . .
H1BC H 0.422738 0.731454 0.350268 0.056 Uiso 0.764(8) 1 calc R U P A 2
H1BD H 0.569071 0.747487 0.300735 0.056 Uiso 0.764(8) 1 calc R U P A 2
H1AA H 0.483770 0.720904 0.305557 0.056 Uiso 0.236(8) 1 calc R U P A 1
H1AB H 0.580742 0.781111 0.340414 0.056 Uiso 0.236(8) 1 calc R U P A 1
C9 C 0.6651(2) 1.1094(2) 0.2395(3) 0.0456(7) Uani 1 1 d . . . . .
H9A H 0.707132 1.135566 0.286127 0.055 Uiso 1 1 calc R U . . .
H9B H 0.650760 1.171534 0.172883 0.055 Uiso 1 1 calc R U . . .
C10 C 0.7510(2) 1.0124(2) 0.2107(3) 0.0437(6) Uani 1 1 d . . . . .
H10A H 0.836009 1.035171 0.174282 0.052 Uiso 1 1 calc R U . . .
H10B H 0.764112 0.949713 0.277121 0.052 Uiso 1 1 calc R U . . .
C2 C 0.5138(4) 0.7934(3) 0.4359(3) 0.0424(11) Uani 0.764(8) 1 d . . P A 2
H2A H 0.559238 0.858535 0.422674 0.051 Uiso 0.764(8) 1 calc R U P A 2
H2B H 0.564173 0.726192 0.478224 0.051 Uiso 0.764(8) 1 calc R U P A 2
C2A C 0.4179(14) 0.7614(10) 0.4380(10) 0.044(4) Uani 0.236(8) 1 d . . P A 1
H2AA H 0.330299 0.748758 0.432899 0.053 Uiso 0.236(8) 1 calc R U P A 1
H2AB H 0.458467 0.691967 0.485944 0.053 Uiso 0.236(8) 1 calc R U P A 1
F1A F 0.4064(6) 0.8449(4) 0.4875(5) 0.0605(14) Uani 0.764(8) 1 d . . P A 1
F1 F 0.3769(18) 0.8089(13) 0.4920(16) 0.048(3) Uani 0.236(8) 1 d . . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S4 2.1678(6) . ?
Ni1 S6 2.1657(7) . ?
Ni1 S5 2.1680(7) . ?
Ni1 S7 2.1661(6) . ?
S2 C16 1.747(2) . ?
S2 C15 1.735(3) . ?
S4 C16 1.711(2) . ?
S6 C18 1.721(2) . ?
S5 C17 1.723(2) . ?
S8 C18 1.745(2) . ?
S8 C20 1.732(2) . ?
S3 C17 1.744(2) . ?
S3 C15 1.732(2) . ?
S9 C19 1.749(2) . ?
S9 C20 1.733(3) . ?
S7 C19 1.722(2) . ?
S10 C20 1.644(2) . ?
S1 C15 1.649(2) . ?
O2 C5 1.422(2) . ?
O2 C4 1.414(3) . ?
O3 C7 1.433(3) . ?
O3 C6 1.419(3) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.482(3) . ?
O5 C11 1.427(3) . ?
O5 C10 1.426(3) . ?
O1 C3 1.424(3) . ?
O1 C14 1.429(3) . ?
O6 C13 1.428(3) . ?
O6 C12 1.418(3) . ?
O4 C8 1.430(3) . ?
O4 C9 1.425(3) . ?
C16 C17 1.363(3) . ?
C18 C19 1.350(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.494(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.496(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.499(3) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.500(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.496(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C1 H1BC 0.9700 . ?
C1 H1BD 0.9700 . ?
C1 H1AA 0.9700 . ?
C1 H1AB 0.9700 . ?
C1 C2 1.445(4) . ?
C1 C2A 1.386(14) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.501(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 F1 1.495(19) . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?
C2A F1A 1.384(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S4 Ni1 S5 93.31(2) . . ?
S6 Ni1 S4 86.98(2) . . ?
S6 Ni1 S5 178.96(2) . . ?
S6 Ni1 S7 92.77(2) . . ?
S7 Ni1 S4 177.96(2) . . ?
S7 Ni1 S5 86.98(2) . . ?
C15 S2 C16 97.78(11) . . ?
C16 S4 Ni1 101.85(8) . . ?
C18 S6 Ni1 102.51(9) . . ?
C17 S5 Ni1 101.98(9) . . ?
C20 S8 C18 97.02(11) . . ?
C15 S3 C17 97.32(11) . . ?
C20 S9 C19 97.04(11) . . ?
C19 S7 Ni1 102.20(8) . . ?
C4 O2 C5 112.12(15) . . ?
C6 O3 C7 112.48(19) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
C10 O5 C11 113.22(17) . . ?
C3 O1 C14 112.20(19) . . ?
C12 O6 C13 112.4(2) . . ?
C9 O4 C8 112.1(2) . . ?
S4 C16 S2 122.76(14) . . ?
C17 C16 S2 115.24(17) . . ?
C17 C16 S4 122.00(16) . . ?
S6 C18 S8 122.64(15) . . ?
C19 C18 S6 120.91(17) . . ?
C19 C18 S8 116.45(16) . . ?
S7 C19 S9 122.39(14) . . ?
C18 C19 S9 116.04(17) . . ?
C18 C19 S7 121.57(16) . . ?
S5 C17 S3 122.53(15) . . ?
C16 C17 S5 120.84(17) . . ?
C16 C17 S3 116.62(16) . . ?
S8 C20 S9 113.38(12) . . ?
S10 C20 S8 123.83(16) . . ?
S10 C20 S9 122.78(15) . . ?
S3 C15 S2 112.96(12) . . ?
S1 C15 S2 123.14(15) . . ?
S1 C15 S3 123.90(16) . . ?
O2 C5 H5A 110.0 . . ?
O2 C5 H5B 110.0 . . ?
O2 C5 C6 108.47(17) . . ?
H5A C5 H5B 108.4 . . ?
C6 C5 H5A 110.0 . . ?
C6 C5 H5B 110.0 . . ?
O3 C7 H7A 110.1 . . ?
O3 C7 H7B 110.1 . . ?
O3 C7 C8 108.1(2) . . ?
H7A C7 H7B 108.4 . . ?
C8 C7 H7A 110.1 . . ?
C8 C7 H7B 110.1 . . ?
O3 C6 C5 108.1(2) . . ?
O3 C6 H6A 110.1 . . ?
O3 C6 H6B 110.1 . . ?
C5 C6 H6A 110.1 . . ?
C5 C6 H6B 110.1 . . ?
H6A C6 H6B 108.4 . . ?
O1 C3 H3A 110.0 . . ?
O1 C3 H3B 110.0 . . ?
O1 C3 C4 108.3(2) . . ?
H3A C3 H3B 108.4 . . ?
C4 C3 H3A 110.0 . . ?
C4 C3 H3B 110.0 . . ?
O2 C4 C3 108.87(17) . . ?
O2 C4 H4A 109.9 . . ?
O2 C4 H4B 109.9 . . ?
C3 C4 H4A 109.9 . . ?
C3 C4 H4B 109.9 . . ?
H4A C4 H4B 108.3 . . ?
O5 C11 H11A 109.9 . . ?
O5 C11 H11B 109.9 . . ?
O5 C11 C12 108.76(18) . . ?
H11A C11 H11B 108.3 . . ?
C12 C11 H11A 109.9 . . ?
C12 C11 H11B 109.9 . . ?
O4 C8 C7 108.3(2) . . ?
O4 C8 H8A 110.0 . . ?
O4 C8 H8B 110.0 . . ?
C7 C8 H8A 110.0 . . ?
C7 C8 H8B 110.0 . . ?
H8A C8 H8B 108.4 . . ?
O6 C13 H13A 109.9 . . ?
O6 C13 H13B 109.9 . . ?
O6 C13 C14 108.9(2) . . ?
H13A C13 H13B 108.3 . . ?
C14 C13 H13A 109.9 . . ?
C14 C13 H13B 109.9 . . ?
O6 C12 C11 108.9(2) . . ?
O6 C12 H12A 109.9 . . ?
O6 C12 H12B 109.9 . . ?
C11 C12 H12A 109.9 . . ?
C11 C12 H12B 109.9 . . ?
H12A C12 H12B 108.3 . . ?
O1 C14 C13 108.3(2) . . ?
O1 C14 H14A 110.0 . . ?
O1 C14 H14B 110.0 . . ?
C13 C14 H14A 110.0 . . ?
C13 C14 H14B 110.0 . . ?
H14A C14 H14B 108.4 . . ?
N1 C1 H1BC 108.8 . . ?
N1 C1 H1BD 108.8 . . ?
N1 C1 H1AA 108.6 . . ?
N1 C1 H1AB 108.6 . . ?
H1BC C1 H1BD 107.7 . . ?
H1AA C1 H1AB 107.6 . . ?
C2 C1 N1 113.7(2) . . ?
C2 C1 H1BC 108.8 . . ?
C2 C1 H1BD 108.8 . . ?
C2A C1 N1 114.6(5) . . ?
C2A C1 H1AA 108.6 . . ?
C2A C1 H1AB 108.6 . . ?
O4 C9 H9A 110.0 . . ?
O4 C9 H9B 110.0 . . ?
O4 C9 C10 108.5(2) . . ?
H9A C9 H9B 108.4 . . ?
C10 C9 H9A 110.0 . . ?
C10 C9 H9B 110.0 . . ?
O5 C10 C9 108.26(18) . . ?
O5 C10 H10A 110.0 . . ?
O5 C10 H10B 110.0 . . ?
C9 C10 H10A 110.0 . . ?
C9 C10 H10B 110.0 . . ?
H10A C10 H10B 108.4 . . ?
C1 C2 H2A 111.5 . . ?
C1 C2 H2B 111.5 . . ?
C1 C2 F1 101.2(8) . . ?
H2A C2 H2B 109.3 . . ?
F1 C2 H2A 111.5 . . ?
F1 C2 H2B 111.5 . . ?
C1 C2A H2AA 108.2 . . ?
C1 C2A H2AB 108.2 . . ?
H2AA C2A H2AB 107.3 . . ?
F1A C2A C1 116.5(9) . . ?
F1A C2A H2AA 108.2 . . ?
F1A C2A H2AB 108.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S4 C16 S2 -178.84(10) . . . . ?
Ni1 S4 C16 C17 1.79(18) . . . . ?
Ni1 S6 C18 S8 178.75(10) . . . . ?
Ni1 S6 C18 C19 -0.80(18) . . . . ?
Ni1 S5 C17 S3 -178.76(11) . . . . ?
Ni1 S5 C17 C16 0.05(18) . . . . ?
Ni1 S7 C19 S9 177.97(10) . . . . ?
Ni1 S7 C19 C18 -1.96(18) . . . . ?
S2 C16 C17 S5 179.27(10) . . . . ?
S2 C16 C17 S3 -1.9(2) . . . . ?
S4 C16 C17 S5 -1.3(3) . . . . ?
S4 C16 C17 S3 177.55(10) . . . . ?
S6 C18 C19 S9 -177.97(10) . . . . ?
S6 C18 C19 S7 2.0(3) . . . . ?
S8 C18 C19 S9 2.5(2) . . . . ?
S8 C18 C19 S7 -177.60(10) . . . . ?
O2 C5 C6 O3 64.1(3) . . . . ?
O3 C7 C8 O4 -69.1(2) . . . . ?
N1 C1 C2 F1 76.9(7) . . . . ?
N1 C1 C2A F1A -53.5(11) . . . . ?
O5 C11 C12 O6 -65.0(3) . . . . ?
O1 C3 C4 O2 -66.0(3) . . . . ?
O6 C13 C14 O1 65.9(3) . . . . ?
O4 C9 C10 O5 61.6(3) . . . . ?
C16 S2 C15 S3 -2.74(13) . . . . ?
C16 S2 C15 S1 177.96(14) . . . . ?
C18 S8 C20 S9 -0.61(13) . . . . ?
C18 S8 C20 S10 -179.51(13) . . . . ?
C19 S9 C20 S8 1.65(13) . . . . ?
C19 S9 C20 S10 -179.44(13) . . . . ?
C17 S3 C15 S2 1.93(14) . . . . ?
C17 S3 C15 S1 -178.78(14) . . . . ?
C20 S8 C18 S6 179.32(13) . . . . ?
C20 S8 C18 C19 -1.12(18) . . . . ?
C20 S9 C19 S7 177.58(13) . . . . ?
C20 S9 C19 C18 -2.49(18) . . . . ?
C15 S2 C16 S4 -176.62(13) . . . . ?
C15 S2 C16 C17 2.79(18) . . . . ?
C15 S3 C17 S5 178.80(13) . . . . ?
C15 S3 C17 C16 -0.06(18) . . . . ?
C5 O2 C4 C3 -176.9(2) . . . . ?
C7 O3 C6 C5 172.48(16) . . . . ?
C6 O3 C7 C8 -179.87(18) . . . . ?
C3 O1 C14 C13 175.5(2) . . . . ?
C4 O2 C5 C6 -178.2(2) . . . . ?
C11 O5 C10 C9 169.0(2) . . . . ?
C8 O4 C9 C10 -171.4(2) . . . . ?
C13 O6 C12 C11 -175.44(17) . . . . ?
C12 O6 C13 C14 -177.19(19) . . . . ?
C14 O1 C3 C4 -177.33(19) . . . . ?
C9 O4 C8 C7 -170.8(2) . . . . ?
C10 O5 C11 C12 -178.7(2) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.654
_oxdiff_exptl_absorpt_empirical_full_min 0.424
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_233k
_database_code_depnum_ccdc_archive 'CCDC 2053289'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-19 downloaded from the CCDC.
;
_audit_creation_date             2020-11-11
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C12 H24 O6, C2 H7 F N'
_chemical_formula_sum            'C20 H31 F N Ni O6 S10'
_chemical_formula_weight         779.77
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHNOFNiS
_chemical_oxdiff_usercomment     20_20200608
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.4520(3)
_cell_length_b                   12.6374(4)
_cell_length_c                   12.9527(4)
_cell_angle_alpha                71.178(3)
_cell_angle_beta                 79.806(2)
_cell_angle_gamma                80.408(2)
_cell_volume                     1582.77(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    10633
_cell_measurement_temperature    233
_cell_measurement_theta_max      30.6840
_cell_measurement_theta_min      2.0020
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.315
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49603
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             806
_exptl_crystal_size_max          0.507
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.775
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19876
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.775
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.035
_diffrn_reflns_theta_min         1.994
_diffrn_ambient_temperature      233
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.775
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      8.00  39.00   0.50    0.30    --    5.18 -99.00 -60.00   62
  2  ω    -18.00  38.00   0.50    0.30    --    5.18 -99.00 -30.00  112
  3  ω    -50.00  -5.00   0.50    0.30    --    5.18 -77.00 -60.00   90
  4  ω     -5.00  78.00   0.50    0.30    --    5.18  37.00  60.00  166
  5  ω    -11.00  77.00   0.50    0.30    --    5.18  77.00 120.00  176
  6  ω    -12.00  14.00   0.50    0.30    --   -4.95 -99.00-150.00   52
  7  ω     -5.00  21.00   0.50    0.30    --   -4.95 -99.00 150.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0026295000
_diffrn_orient_matrix_UB_12      0.0549105000
_diffrn_orient_matrix_UB_13      0.0042537000
_diffrn_orient_matrix_UB_21      -0.0104286000
_diffrn_orient_matrix_UB_22      -0.0219289000
_diffrn_orient_matrix_UB_23      0.0581977000
_diffrn_orient_matrix_UB_31      0.0685944000
_diffrn_orient_matrix_UB_32      -0.0083350000
_diffrn_orient_matrix_UB_33      0.0012107000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5915
_reflns_number_total             7847
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         7847
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0335
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0366P)²+0.1442P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0864
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
2. Others
 Sof(H1AA)=Sof(H1AB)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(F1)=1-FVAR(1)
 Sof(H1BC)=Sof(H1BD)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(F1A)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C7(H7A,H7B), C6(H6A,H6B), C3(H3A,H3B), C4(H4A,H4B), C11(H11A,
 H11B), C8(H8A,H8B), C13(H13A,H13B), C12(H12A,H12B), C14(H14A,H14B), C1(H1BC,
 H1BD), C1(H1AA,H1AB), C9(H9A,H9B), C10(H10A,H10B), C2(H2A,H2B), C2A(H2AA,H2AB)
3.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.16338(2) 0.40515(2) 0.49126(2) 0.03019(7) Uani 1 1 d . . . . .
S2 S -0.07950(4) 0.26657(4) 0.29617(4) 0.03414(12) Uani 1 1 d . . . . .
S4 S 0.00700(5) 0.31407(4) 0.48682(4) 0.03427(11) Uani 1 1 d . . . . .
S6 S 0.10036(5) 0.36910(4) 0.66616(4) 0.03630(12) Uani 1 1 d . . . . .
S5 S 0.22919(5) 0.43961(4) 0.31665(4) 0.03687(12) Uani 1 1 d . . . . .
S8 S 0.19619(5) 0.43696(4) 0.84130(4) 0.03784(12) Uani 1 1 d . . . . .
S3 S 0.12881(5) 0.37559(5) 0.14138(5) 0.04009(13) Uani 1 1 d . . . . .
S9 S 0.40160(5) 0.55041(5) 0.68531(5) 0.04122(13) Uani 1 1 d . . . . .
S7 S 0.31531(5) 0.50046(5) 0.49528(4) 0.03910(13) Uani 1 1 d . . . . .
S10 S 0.37559(6) 0.54765(5) 0.91760(5) 0.05072(15) Uani 1 1 d . . . . .
S1 S -0.04969(6) 0.26398(6) 0.06449(5) 0.05097(15) Uani 1 1 d . . . . .
O2 O 0.16826(12) 0.89577(11) 0.28516(13) 0.0406(3) Uani 1 1 d . . . . .
O3 O 0.26723(13) 1.06532(12) 0.32946(13) 0.0424(3) Uani 1 1 d . . . . .
N1 N 0.44630(15) 0.89072(13) 0.25355(14) 0.0336(4) Uani 1 1 d . . . . .
H1A H 0.410040 0.876290 0.203075 0.040 Uiso 1 1 calc R U . . .
H1B H 0.514276 0.928875 0.220965 0.040 Uiso 1 1 calc R U . . .
H1C H 0.387539 0.931490 0.288343 0.040 Uiso 1 1 calc R U . . .
O5 O 0.68754(13) 0.97983(13) 0.13980(14) 0.0479(4) Uani 1 1 d . . . . .
O1 O 0.31756(14) 0.80836(12) 0.12224(13) 0.0429(4) Uani 1 1 d . . . . .
O6 O 0.59013(14) 0.81744(13) 0.07829(13) 0.0469(4) Uani 1 1 d . . . . .
O4 O 0.54177(14) 1.07247(12) 0.29715(14) 0.0472(4) Uani 1 1 d . . . . .
C16 C 0.02407(17) 0.32421(15) 0.35009(17) 0.0304(4) Uani 1 1 d . . . . .
C18 C 0.20469(18) 0.43541(15) 0.70606(17) 0.0321(4) Uani 1 1 d . . . . .
C19 C 0.29896(17) 0.49094(16) 0.63213(17) 0.0330(4) Uani 1 1 d . . . . .
C17 C 0.12050(18) 0.37718(16) 0.27618(17) 0.0320(4) Uani 1 1 d . . . . .
C20 C 0.32629(19) 0.51412(16) 0.82010(18) 0.0359(4) Uani 1 1 d . . . . .
C15 C -0.00221(19) 0.29989(17) 0.16204(18) 0.0369(4) Uani 1 1 d . . . . .
C5 C 0.08544(19) 0.98216(19) 0.3208(2) 0.0458(5) Uani 1 1 d . . . . .
H5A H 0.004071 0.954501 0.360876 0.055 Uiso 1 1 calc R U . . .
H5B H 0.065131 1.045914 0.257731 0.055 Uiso 1 1 calc R U . . .
C7 C 0.3320(2) 1.11484(19) 0.3880(2) 0.0465(5) Uani 1 1 d . . . . .
H7A H 0.359591 1.058211 0.453477 0.056 Uiso 1 1 calc R U . . .
H7B H 0.272721 1.173611 0.410365 0.056 Uiso 1 1 calc R U . . .
C6 C 0.1546(2) 1.01727(19) 0.3932(2) 0.0454(5) Uani 1 1 d . . . . .
H6A H 0.097409 1.071918 0.423395 0.054 Uiso 1 1 calc R U . . .
H6B H 0.179889 0.952604 0.453830 0.054 Uiso 1 1 calc R U . . .
C3 C 0.2002(2) 0.76483(18) 0.1850(2) 0.0474(5) Uani 1 1 d . . . . .
H3A H 0.220574 0.705820 0.251463 0.057 Uiso 1 1 calc R U . . .
H3B H 0.158471 0.733312 0.142230 0.057 Uiso 1 1 calc R U . . .
C4 C 0.1109(2) 0.85946(18) 0.2136(2) 0.0446(5) Uani 1 1 d . . . . .
H4A H 0.097080 0.921187 0.147298 0.054 Uiso 1 1 calc R U . . .
H4B H 0.026752 0.834460 0.249110 0.054 Uiso 1 1 calc R U . . .
C11 C 0.7705(2) 0.9023(2) 0.0905(2) 0.0545(6) Uani 1 1 d . . . . .
H11A H 0.797097 0.834138 0.147018 0.065 Uiso 1 1 calc R U . . .
H11B H 0.848542 0.935447 0.049221 0.065 Uiso 1 1 calc R U . . .
C8 C 0.4475(2) 1.16286(18) 0.3140(2) 0.0483(6) Uani 1 1 d . . . . .
H8A H 0.421508 1.211179 0.244091 0.058 Uiso 1 1 calc R U . . .
H8B H 0.484839 1.207591 0.346847 0.058 Uiso 1 1 calc R U . . .
C13 C 0.5196(2) 0.7806(2) 0.0135(2) 0.0539(6) Uani 1 1 d . . . . .
H13A H 0.576714 0.727681 -0.019089 0.065 Uiso 1 1 calc R U . . .
H13B H 0.488844 0.844443 -0.045514 0.065 Uiso 1 1 calc R U . . .
C12 C 0.6964(2) 0.8752(2) 0.0154(2) 0.0550(6) Uani 1 1 d . . . . .
H12A H 0.664189 0.944111 -0.037614 0.066 Uiso 1 1 calc R U . . .
H12B H 0.753595 0.828694 -0.024531 0.066 Uiso 1 1 calc R U . . .
C14 C 0.4063(2) 0.7256(2) 0.0849(2) 0.0548(6) Uani 1 1 d . . . . .
H14A H 0.362963 0.693509 0.043726 0.066 Uiso 1 1 calc R U . . .
H14B H 0.436141 0.665540 0.147240 0.066 Uiso 1 1 calc R U . . .
C1 C 0.4913(3) 0.7833(2) 0.3339(2) 0.0591(7) Uani 1 1 d . . . . .
H1BC H 0.427277 0.731259 0.348066 0.071 Uiso 0.668(8) 1 calc R U P A 2
H1BD H 0.572910 0.751066 0.301192 0.071 Uiso 0.668(8) 1 calc R U P A 2
H1AA H 0.490979 0.722251 0.304014 0.071 Uiso 0.332(8) 1 calc R U P A 1
H1AB H 0.581013 0.785232 0.342985 0.071 Uiso 0.332(8) 1 calc R U P A 1
C9 C 0.6636(2) 1.1099(2) 0.2408(2) 0.0569(6) Uani 1 1 d . . . . .
H9A H 0.705361 1.136478 0.287389 0.068 Uiso 1 1 calc R U . . .
H9B H 0.649531 1.171457 0.174458 0.068 Uiso 1 1 calc R U . . .
C10 C 0.7493(2) 1.0131(2) 0.2119(2) 0.0564(6) Uani 1 1 d . . . . .
H10A H 0.834457 1.035694 0.176144 0.068 Uiso 1 1 calc R U . . .
H10B H 0.761601 0.950749 0.277995 0.068 Uiso 1 1 calc R U . . .
C2 C 0.5111(5) 0.7935(3) 0.4361(3) 0.0566(14) Uani 0.668(8) 1 d . . P A 2
H2A H 0.562934 0.854011 0.425307 0.068 Uiso 0.668(8) 1 calc R U P A 2
H2B H 0.553191 0.723801 0.481319 0.068 Uiso 0.668(8) 1 calc R U P A 2
C2A C 0.4169(10) 0.7607(6) 0.4358(6) 0.050(3) Uani 0.332(8) 1 d . . P A 1
H2AA H 0.453396 0.689312 0.482573 0.060 Uiso 0.332(8) 1 calc R U P A 1
H2AB H 0.329049 0.752271 0.427454 0.060 Uiso 0.332(8) 1 calc R U P A 1
F1A F 0.4087(8) 0.8429(8) 0.4889(8) 0.077(2) Uani 0.668(8) 1 d . . P A 1
F1 F 0.3719(16) 0.8197(18) 0.4861(14) 0.073(4) Uani 0.332(8) 1 d . . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S4 2.1686(5) . ?
Ni1 S6 2.1631(6) . ?
Ni1 S5 2.1660(6) . ?
Ni1 S7 2.1638(5) . ?
S2 C16 1.7461(18) . ?
S2 C15 1.730(2) . ?
S4 C16 1.713(2) . ?
S6 C18 1.7152(19) . ?
S5 C17 1.7217(19) . ?
S8 C18 1.744(2) . ?
S8 C20 1.736(2) . ?
S3 C17 1.739(2) . ?
S3 C15 1.733(2) . ?
S9 C19 1.7476(18) . ?
S9 C20 1.731(2) . ?
S7 C19 1.717(2) . ?
S10 C20 1.640(2) . ?
S1 C15 1.648(2) . ?
O2 C5 1.422(2) . ?
O2 C4 1.411(2) . ?
O3 C7 1.433(2) . ?
O3 C6 1.417(3) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.482(3) . ?
O5 C11 1.430(3) . ?
O5 C10 1.422(3) . ?
O1 C3 1.432(3) . ?
O1 C14 1.425(2) . ?
O6 C13 1.433(3) . ?
O6 C12 1.413(3) . ?
O4 C8 1.426(2) . ?
O4 C9 1.424(3) . ?
C16 C17 1.360(3) . ?
C18 C19 1.358(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.489(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.485(3) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.493(3) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.495(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.487(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C1 H1BC 0.9700 . ?
C1 H1BD 0.9700 . ?
C1 H1AA 0.9700 . ?
C1 H1AB 0.9700 . ?
C1 C2 1.423(5) . ?
C1 C2A 1.377(9) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.500(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 F1 1.513(18) . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?
C2A F1A 1.405(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S6 Ni1 S4 87.07(2) . . ?
S6 Ni1 S5 179.14(2) . . ?
S6 Ni1 S7 92.77(2) . . ?
S5 Ni1 S4 93.26(2) . . ?
S7 Ni1 S4 178.30(2) . . ?
S7 Ni1 S5 86.92(2) . . ?
C15 S2 C16 97.70(10) . . ?
C16 S4 Ni1 101.80(7) . . ?
C18 S6 Ni1 102.60(7) . . ?
C17 S5 Ni1 102.09(7) . . ?
C20 S8 C18 97.26(10) . . ?
C15 S3 C17 97.40(10) . . ?
C20 S9 C19 97.41(10) . . ?
C19 S7 Ni1 102.33(7) . . ?
C4 O2 C5 112.08(15) . . ?
C6 O3 C7 112.65(17) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
C10 O5 C11 113.30(17) . . ?
C14 O1 C3 112.37(17) . . ?
C12 O6 C13 112.83(19) . . ?
C9 O4 C8 112.25(17) . . ?
S4 C16 S2 122.57(12) . . ?
C17 C16 S2 115.43(15) . . ?
C17 C16 S4 121.99(14) . . ?
S6 C18 S8 122.84(12) . . ?
C19 C18 S6 120.91(15) . . ?
C19 C18 S8 116.24(14) . . ?
S7 C19 S9 122.75(12) . . ?
C18 C19 S9 115.89(15) . . ?
C18 C19 S7 121.36(14) . . ?
S5 C17 S3 122.65(12) . . ?
C16 C17 S5 120.85(15) . . ?
C16 C17 S3 116.48(14) . . ?
S9 C20 S8 113.14(11) . . ?
S10 C20 S8 123.86(13) . . ?
S10 C20 S9 122.99(13) . . ?
S2 C15 S3 112.91(11) . . ?
S1 C15 S2 123.22(12) . . ?
S1 C15 S3 123.87(13) . . ?
O2 C5 H5A 110.0 . . ?
O2 C5 H5B 110.0 . . ?
O2 C5 C6 108.47(16) . . ?
H5A C5 H5B 108.4 . . ?
C6 C5 H5A 110.0 . . ?
C6 C5 H5B 110.0 . . ?
O3 C7 H7A 110.1 . . ?
O3 C7 H7B 110.1 . . ?
O3 C7 C8 108.24(18) . . ?
H7A C7 H7B 108.4 . . ?
C8 C7 H7A 110.1 . . ?
C8 C7 H7B 110.1 . . ?
O3 C6 C5 108.25(18) . . ?
O3 C6 H6A 110.0 . . ?
O3 C6 H6B 110.0 . . ?
C5 C6 H6A 110.0 . . ?
C5 C6 H6B 110.0 . . ?
H6A C6 H6B 108.4 . . ?
O1 C3 H3A 110.1 . . ?
O1 C3 H3B 110.1 . . ?
O1 C3 C4 108.03(17) . . ?
H3A C3 H3B 108.4 . . ?
C4 C3 H3A 110.1 . . ?
C4 C3 H3B 110.1 . . ?
O2 C4 C3 108.82(16) . . ?
O2 C4 H4A 109.9 . . ?
O2 C4 H4B 109.9 . . ?
C3 C4 H4A 109.9 . . ?
C3 C4 H4B 109.9 . . ?
H4A C4 H4B 108.3 . . ?
O5 C11 H11A 110.0 . . ?
O5 C11 H11B 110.0 . . ?
O5 C11 C12 108.48(17) . . ?
H11A C11 H11B 108.4 . . ?
C12 C11 H11A 110.0 . . ?
C12 C11 H11B 110.0 . . ?
O4 C8 C7 108.51(18) . . ?
O4 C8 H8A 110.0 . . ?
O4 C8 H8B 110.0 . . ?
C7 C8 H8A 110.0 . . ?
C7 C8 H8B 110.0 . . ?
H8A C8 H8B 108.4 . . ?
O6 C13 H13A 109.8 . . ?
O6 C13 H13B 109.8 . . ?
O6 C13 C14 109.2(2) . . ?
H13A C13 H13B 108.3 . . ?
C14 C13 H13A 109.8 . . ?
C14 C13 H13B 109.8 . . ?
O6 C12 C11 109.2(2) . . ?
O6 C12 H12A 109.8 . . ?
O6 C12 H12B 109.8 . . ?
C11 C12 H12A 109.8 . . ?
C11 C12 H12B 109.8 . . ?
H12A C12 H12B 108.3 . . ?
O1 C14 C13 108.48(19) . . ?
O1 C14 H14A 110.0 . . ?
O1 C14 H14B 110.0 . . ?
C13 C14 H14A 110.0 . . ?
C13 C14 H14B 110.0 . . ?
H14A C14 H14B 108.4 . . ?
N1 C1 H1BC 108.6 . . ?
N1 C1 H1BD 108.6 . . ?
N1 C1 H1AA 108.7 . . ?
N1 C1 H1AB 108.7 . . ?
H1BC C1 H1BD 107.6 . . ?
H1AA C1 H1AB 107.6 . . ?
C2 C1 N1 114.6(2) . . ?
C2 C1 H1BC 108.6 . . ?
C2 C1 H1BD 108.6 . . ?
C2A C1 N1 114.4(3) . . ?
C2A C1 H1AA 108.7 . . ?
C2A C1 H1AB 108.7 . . ?
O4 C9 H9A 110.0 . . ?
O4 C9 H9B 110.0 . . ?
O4 C9 C10 108.53(19) . . ?
H9A C9 H9B 108.4 . . ?
C10 C9 H9A 110.0 . . ?
C10 C9 H9B 110.0 . . ?
O5 C10 C9 108.26(17) . . ?
O5 C10 H10A 110.0 . . ?
O5 C10 H10B 110.0 . . ?
C9 C10 H10A 110.0 . . ?
C9 C10 H10B 110.0 . . ?
H10A C10 H10B 108.4 . . ?
C1 C2 H2A 111.5 . . ?
C1 C2 H2B 111.5 . . ?
C1 C2 F1 101.5(6) . . ?
H2A C2 H2B 109.3 . . ?
F1 C2 H2A 111.5 . . ?
F1 C2 H2B 111.5 . . ?
C1 C2A H2AA 108.6 . . ?
C1 C2A H2AB 108.6 . . ?
C1 C2A F1A 114.8(7) . . ?
H2AA C2A H2AB 107.5 . . ?
F1A C2A H2AA 108.6 . . ?
F1A C2A H2AB 108.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S4 C16 S2 -179.05(9) . . . . ?
Ni1 S4 C16 C17 1.53(16) . . . . ?
Ni1 S6 C18 S8 178.53(9) . . . . ?
Ni1 S6 C18 C19 -0.97(16) . . . . ?
Ni1 S5 C17 S3 -178.51(10) . . . . ?
Ni1 S5 C17 C16 0.26(16) . . . . ?
Ni1 S7 C19 S9 178.16(10) . . . . ?
Ni1 S7 C19 C18 -1.44(17) . . . . ?
S2 C16 C17 S5 179.26(9) . . . . ?
S2 C16 C17 S3 -1.9(2) . . . . ?
S4 C16 C17 S5 -1.3(2) . . . . ?
S4 C16 C17 S3 177.56(10) . . . . ?
S6 C18 C19 S9 -177.91(9) . . . . ?
S6 C18 C19 S7 1.7(2) . . . . ?
S8 C18 C19 S9 2.6(2) . . . . ?
S8 C18 C19 S7 -177.81(10) . . . . ?
O2 C5 C6 O3 64.3(2) . . . . ?
O3 C7 C8 O4 -69.0(2) . . . . ?
N1 C1 C2 F1 70.1(9) . . . . ?
N1 C1 C2A F1A -58.3(8) . . . . ?
O5 C11 C12 O6 -65.2(2) . . . . ?
O1 C3 C4 O2 -65.8(2) . . . . ?
O6 C13 C14 O1 65.4(2) . . . . ?
O4 C9 C10 O5 62.2(3) . . . . ?
C16 S2 C15 S3 -2.65(12) . . . . ?
C16 S2 C15 S1 177.84(13) . . . . ?
C18 S8 C20 S9 -0.78(12) . . . . ?
C18 S8 C20 S10 -179.65(12) . . . . ?
C19 S9 C20 S8 1.87(12) . . . . ?
C19 S9 C20 S10 -179.25(12) . . . . ?
C17 S3 C15 S2 1.83(12) . . . . ?
C17 S3 C15 S1 -178.66(13) . . . . ?
C20 S8 C18 S6 179.41(11) . . . . ?
C20 S8 C18 C19 -1.08(16) . . . . ?
C20 S9 C19 S7 177.69(12) . . . . ?
C20 S9 C19 C18 -2.69(16) . . . . ?
C15 S2 C16 S4 -176.69(11) . . . . ?
C15 S2 C16 C17 2.76(16) . . . . ?
C15 S3 C17 S5 178.85(12) . . . . ?
C15 S3 C17 C16 0.03(16) . . . . ?
C5 O2 C4 C3 -176.91(19) . . . . ?
C7 O3 C6 C5 172.60(16) . . . . ?
C6 O3 C7 C8 -179.74(17) . . . . ?
C3 O1 C14 C13 175.49(19) . . . . ?
C4 O2 C5 C6 -178.58(19) . . . . ?
C11 O5 C10 C9 169.1(2) . . . . ?
C8 O4 C9 C10 -171.6(2) . . . . ?
C13 O6 C12 C11 -175.48(17) . . . . ?
C12 O6 C13 C14 -177.35(18) . . . . ?
C14 O1 C3 C4 -176.34(18) . . . . ?
C9 O4 C8 C7 -171.11(19) . . . . ?
C10 O5 C11 C12 -179.0(2) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.665
_oxdiff_exptl_absorpt_empirical_full_min 0.514
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_H293k
_database_code_depnum_ccdc_archive 'CCDC 2053280'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H32 N Ni O6 S10'
_chemical_formula_weight         761.77

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.2486(6)
_cell_length_b                   12.3540(8)
_cell_length_c                   12.7375(8)
_cell_angle_alpha                87.498(5)
_cell_angle_beta                 69.343(6)
_cell_angle_gamma                80.758(5)
_cell_volume                     1634.62(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_F_000             790
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    1.267
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20189
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.959
_diffrn_reflns_theta_max         31.057
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.767
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.767
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.767
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8034
_reflns_number_gt                5879
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0402P)²+0.1497P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8034
_refine_ls_number_parameters     345
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0365
_refine_ls_wR_factor_ref         0.1020
_refine_ls_wR_factor_gt          0.0945
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.35979(2) 0.11846(2) 0.47366(2) 0.03788(8) Uani 1 1 d . . . . .
S2 S 0.31298(5) 0.07183(5) 0.64732(4) 0.05024(14) Uani 1 1 d . . . . .
S1 S 0.50126(5) 0.21526(5) 0.48004(4) 0.04860(14) Uani 1 1 d . . . . .
S9 S 0.13894(5) -0.03269(4) 0.27335(5) 0.04889(14) Uani 1 1 d . . . . .
S4 S 0.41958(5) 0.12526(5) 0.82366(5) 0.05215(15) Uani 1 1 d . . . . .
S6 S 0.40862(5) 0.16333(5) 0.29887(4) 0.04890(14) Uani 1 1 d . . . . .
S7 S 0.21822(5) 0.02150(5) 0.46737(4) 0.04862(14) Uani 1 1 d . . . . .
S8 S 0.31296(6) 0.09829(5) 0.11933(5) 0.05515(16) Uani 1 1 d . . . . .
S5 S 0.58210(6) 0.24074(6) 0.90711(5) 0.06601(19) Uani 1 1 d . . . . .
S3 S 0.58781(6) 0.26132(5) 0.67182(5) 0.05534(15) Uani 1 1 d . . . . .
S10 S 0.14340(7) -0.01039(6) 0.03831(6) 0.06674(19) Uani 1 1 d . . . . .
O4 O 0.00074(15) 0.69556(14) 0.66819(14) 0.0613(4) Uani 1 1 d . . . . .
O3 O 0.20599(14) 0.72674(12) 0.73492(14) 0.0551(4) Uani 1 1 d . . . . .
O6 O -0.01558(16) 0.34954(13) 0.84132(14) 0.0620(4) Uani 1 1 d . . . . .
O5 O -0.07264(16) 0.48666(15) 0.67797(15) 0.0676(5) Uani 1 1 d . . . . .
O2 O 0.26228(15) 0.58497(14) 0.89264(14) 0.0618(4) Uani 1 1 d . . . . .
O1 O 0.18675(16) 0.37617(13) 0.91794(14) 0.0615(4) Uani 1 1 d . . . . .
N1 N 0.14958(16) 0.50826(14) 0.73940(15) 0.0465(4) Uani 1 1 d . . . . .
H1A H 0.078017 0.520523 0.722932 0.056 Uiso 1 1 calc R U . . .
H1B H 0.172693 0.572012 0.747796 0.056 Uiso 1 1 calc R U . . .
H1C H 0.135455 0.470894 0.802862 0.056 Uiso 1 1 calc R U . . .
C19 C 0.23020(18) 0.03247(15) 0.32939(17) 0.0394(4) Uani 1 1 d . . . . .
C16 C 0.41400(19) 0.13599(16) 0.68835(16) 0.0412(4) Uani 1 1 d . . . . .
C20 C 0.1962(2) 0.01654(17) 0.13841(18) 0.0483(5) Uani 1 1 d . . . . .
C6 C 0.2565(2) 0.7608(2) 0.8130(2) 0.0633(6) Uani 1 1 d . . . . .
H6A H 0.186801 0.788584 0.880891 0.076 Uiso 1 1 calc R U . . .
H6B H 0.306302 0.819156 0.781544 0.076 Uiso 1 1 calc R U . . .
C13 C 0.0504(3) 0.2628(2) 0.8889(3) 0.0733(7) Uani 1 1 d . . . . .
H13A H 0.124847 0.225144 0.830112 0.088 Uiso 1 1 calc R U . . .
H13B H -0.006341 0.210044 0.924258 0.088 Uiso 1 1 calc R U . . .
C15 C 0.49430(18) 0.19877(17) 0.61638(17) 0.0417(4) Uani 1 1 d . . . . .
C7 C 0.1271(2) 0.81404(19) 0.7029(2) 0.0644(6) Uani 1 1 d . . . . .
H7A H 0.175936 0.873106 0.671969 0.077 Uiso 1 1 calc R U . . .
H7B H 0.054155 0.842367 0.768346 0.077 Uiso 1 1 calc R U . . .
C5 C 0.3391(2) 0.6665(2) 0.8398(2) 0.0645(7) Uani 1 1 d . . . . .
H5A H 0.406730 0.636632 0.771544 0.077 Uiso 1 1 calc R U . . .
H5B H 0.378947 0.689828 0.889428 0.077 Uiso 1 1 calc R U . . .
C18 C 0.31172(19) 0.09434(17) 0.25657(16) 0.0414(4) Uani 1 1 d . . . . .
C8 C 0.0809(2) 0.7748(2) 0.6184(2) 0.0635(6) Uani 1 1 d . . . . .
H8A H 0.033105 0.835733 0.592226 0.076 Uiso 1 1 calc R U . . .
H8B H 0.153377 0.742636 0.554547 0.076 Uiso 1 1 calc R U . . .
C3 C 0.2367(3) 0.4204(2) 0.9925(2) 0.0691(7) Uani 1 1 d . . . . .
H3A H 0.279812 0.361304 1.025015 0.083 Uiso 1 1 calc R U . . .
H3B H 0.166933 0.460926 1.052909 0.083 Uiso 1 1 calc R U . . .
C11 C -0.1476(3) 0.4047(3) 0.7348(3) 0.0796(8) Uani 1 1 d . . . . .
H11A H -0.187950 0.378746 0.686857 0.096 Uiso 1 1 calc R U . . .
H11B H -0.214986 0.436104 0.802435 0.096 Uiso 1 1 calc R U . . .
C10 C -0.1487(3) 0.5844(3) 0.6622(3) 0.0762(8) Uani 1 1 d . . . . .
H10A H -0.205012 0.616085 0.734404 0.091 Uiso 1 1 calc R U . . .
H10B H -0.201665 0.568504 0.620737 0.091 Uiso 1 1 calc R U . . .
C17 C 0.53187(19) 0.21070(19) 0.80632(18) 0.0488(5) Uani 1 1 d . . . . .
C9 C -0.0638(3) 0.6626(2) 0.5995(2) 0.0701(7) Uani 1 1 d . . . . .
H9A H -0.001383 0.628250 0.530891 0.084 Uiso 1 1 calc R U . . .
H9B H -0.114084 0.726139 0.579734 0.084 Uiso 1 1 calc R U . . .
C4 C 0.3290(3) 0.4943(2) 0.9296(2) 0.0703(7) Uani 1 1 d . . . . .
H4A H 0.369938 0.518855 0.977789 0.084 Uiso 1 1 calc R U . . .
H4B H 0.395363 0.455265 0.865767 0.084 Uiso 1 1 calc R U . . .
C12 C -0.0648(3) 0.3115(2) 0.7644(3) 0.0773(8) Uani 1 1 d . . . . .
H12A H -0.114559 0.253577 0.797818 0.093 Uiso 1 1 calc R U . . .
H12B H 0.005328 0.282217 0.697512 0.093 Uiso 1 1 calc R U . . .
C14 C 0.0918(3) 0.3097(2) 0.9731(2) 0.0695(7) Uani 1 1 d . . . . .
H14A H 0.018647 0.353399 1.027905 0.083 Uiso 1 1 calc R U . . .
H14B H 0.126733 0.251105 1.012143 0.083 Uiso 1 1 calc R U . . .
C1 C 0.2533(3) 0.4442(2) 0.6476(3) 0.0814(8) Uani 1 1 d . . . . .
H1D H 0.317660 0.407742 0.677109 0.098 Uiso 1 1 calc R U . . .
H1E H 0.217621 0.387641 0.623328 0.098 Uiso 1 1 calc R U . . .
C2 C 0.3157(4) 0.5053(3) 0.5518(3) 0.1109(13) Uani 1 1 d . . . . .
H2A H 0.374270 0.455869 0.493683 0.166 Uiso 1 1 calc R U . . .
H2B H 0.362232 0.554448 0.572125 0.166 Uiso 1 1 calc R U . . .
H2C H 0.252400 0.546744 0.525156 0.166 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S2 2.1603(6) . ?
Ni1 S1 2.1633(6) . ?
Ni1 S7 2.1653(6) . ?
Ni1 S6 2.1663(6) . ?
S2 C16 1.7137(19) . ?
S1 C15 1.715(2) . ?
S9 C20 1.730(2) . ?
S9 C19 1.7447(18) . ?
S4 C17 1.723(2) . ?
S4 C16 1.7453(19) . ?
S6 C18 1.7199(19) . ?
S7 C19 1.716(2) . ?
S8 C20 1.727(2) . ?
S8 C18 1.7417(19) . ?
S5 C17 1.651(2) . ?
S3 C17 1.730(2) . ?
S3 C15 1.7422(18) . ?
S10 C20 1.6506(19) . ?
O4 C8 1.414(3) . ?
O4 C9 1.425(3) . ?
O3 C6 1.415(3) . ?
O3 C7 1.424(3) . ?
O6 C12 1.412(3) . ?
O6 C13 1.439(3) . ?
O5 C10 1.414(3) . ?
O5 C11 1.428(3) . ?
O2 C4 1.405(3) . ?
O2 C5 1.423(3) . ?
O1 C14 1.418(3) . ?
O1 C3 1.427(3) . ?
N1 C1 1.476(3) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
C19 C18 1.360(3) . ?
C16 C15 1.355(3) . ?
C6 C5 1.476(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C13 C14 1.482(4) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C7 C8 1.478(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C3 C4 1.486(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C11 C12 1.484(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C10 C9 1.475(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C1 C2 1.427(4) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S2 Ni1 S1 93.13(2) . . ?
S2 Ni1 S7 86.83(2) . . ?
S1 Ni1 S7 179.96(3) . . ?
S2 Ni1 S6 179.25(3) . . ?
S1 Ni1 S6 86.88(2) . . ?
S7 Ni1 S6 93.16(2) . . ?
C16 S2 Ni1 102.19(7) . . ?
C15 S1 Ni1 101.95(7) . . ?
C20 S9 C19 97.50(10) . . ?
C17 S4 C16 97.38(10) . . ?
C18 S6 Ni1 102.05(7) . . ?
C19 S7 Ni1 102.09(7) . . ?
C20 S8 C18 97.32(10) . . ?
C17 S3 C15 97.59(10) . . ?
C8 O4 C9 113.8(2) . . ?
C6 O3 C7 112.54(18) . . ?
C12 O6 C13 113.3(2) . . ?
C10 O5 C11 112.8(2) . . ?
C4 O2 C5 113.93(19) . . ?
C14 O1 C3 112.8(2) . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C18 C19 S7 121.46(14) . . ?
C18 C19 S9 115.61(15) . . ?
S7 C19 S9 122.93(12) . . ?
C15 C16 S2 121.22(15) . . ?
C15 C16 S4 116.21(14) . . ?
S2 C16 S4 122.57(13) . . ?
S10 C20 S8 123.30(14) . . ?
S10 C20 S9 123.49(13) . . ?
S8 C20 S9 113.20(11) . . ?
O3 C6 C5 109.11(19) . . ?
O3 C6 H6A 109.9 . . ?
C5 C6 H6A 109.9 . . ?
O3 C6 H6B 109.9 . . ?
C5 C6 H6B 109.9 . . ?
H6A C6 H6B 108.3 . . ?
O6 C13 C14 109.4(2) . . ?
O6 C13 H13A 109.8 . . ?
C14 C13 H13A 109.8 . . ?
O6 C13 H13B 109.8 . . ?
C14 C13 H13B 109.8 . . ?
H13A C13 H13B 108.2 . . ?
C16 C15 S1 121.49(14) . . ?
C16 C15 S3 115.68(15) . . ?
S1 C15 S3 122.83(13) . . ?
O3 C7 C8 110.20(19) . . ?
O3 C7 H7A 109.6 . . ?
C8 C7 H7A 109.6 . . ?
O3 C7 H7B 109.6 . . ?
C8 C7 H7B 109.6 . . ?
H7A C7 H7B 108.1 . . ?
O2 C5 C6 108.83(19) . . ?
O2 C5 H5A 109.9 . . ?
C6 C5 H5A 109.9 . . ?
O2 C5 H5B 109.9 . . ?
C6 C5 H5B 109.9 . . ?
H5A C5 H5B 108.3 . . ?
C19 C18 S6 121.21(15) . . ?
C19 C18 S8 116.33(14) . . ?
S6 C18 S8 122.47(12) . . ?
O4 C8 C7 108.7(2) . . ?
O4 C8 H8A 109.9 . . ?
C7 C8 H8A 109.9 . . ?
O4 C8 H8B 109.9 . . ?
C7 C8 H8B 109.9 . . ?
H8A C8 H8B 108.3 . . ?
O1 C3 C4 109.4(2) . . ?
O1 C3 H3A 109.8 . . ?
C4 C3 H3A 109.8 . . ?
O1 C3 H3B 109.8 . . ?
C4 C3 H3B 109.8 . . ?
H3A C3 H3B 108.2 . . ?
O5 C11 C12 110.1(2) . . ?
O5 C11 H11A 109.6 . . ?
C12 C11 H11A 109.6 . . ?
O5 C11 H11B 109.6 . . ?
C12 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
O5 C10 C9 109.2(2) . . ?
O5 C10 H10A 109.8 . . ?
C9 C10 H10A 109.8 . . ?
O5 C10 H10B 109.8 . . ?
C9 C10 H10B 109.8 . . ?
H10A C10 H10B 108.3 . . ?
S5 C17 S4 123.65(15) . . ?
S5 C17 S3 123.25(14) . . ?
S4 C17 S3 113.09(11) . . ?
O4 C9 C10 108.8(2) . . ?
O4 C9 H9A 109.9 . . ?
C10 C9 H9A 109.9 . . ?
O4 C9 H9B 109.9 . . ?
C10 C9 H9B 109.9 . . ?
H9A C9 H9B 108.3 . . ?
O2 C4 C3 109.0(2) . . ?
O2 C4 H4A 109.9 . . ?
C3 C4 H4A 109.9 . . ?
O2 C4 H4B 109.9 . . ?
C3 C4 H4B 109.9 . . ?
H4A C4 H4B 108.3 . . ?
O6 C12 C11 108.6(2) . . ?
O6 C12 H12A 110.0 . . ?
C11 C12 H12A 110.0 . . ?
O6 C12 H12B 110.0 . . ?
C11 C12 H12B 110.0 . . ?
H12A C12 H12B 108.4 . . ?
O1 C14 C13 109.2(2) . . ?
O1 C14 H14A 109.8 . . ?
C13 C14 H14A 109.8 . . ?
O1 C14 H14B 109.8 . . ?
C13 C14 H14B 109.8 . . ?
H14A C14 H14B 108.3 . . ?
C2 C1 N1 115.7(2) . . ?
C2 C1 H1D 108.4 . . ?
N1 C1 H1D 108.4 . . ?
C2 C1 H1E 108.4 . . ?
N1 C1 H1E 108.4 . . ?
H1D C1 H1E 107.4 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S7 C19 C18 -1.96(18) . . . . ?
Ni1 S7 C19 S9 178.72(10) . . . . ?
C20 S9 C19 C18 -0.94(18) . . . . ?
C20 S9 C19 S7 178.41(13) . . . . ?
Ni1 S2 C16 C15 1.13(18) . . . . ?
Ni1 S2 C16 S4 -179.11(10) . . . . ?
C17 S4 C16 C15 1.92(18) . . . . ?
C17 S4 C16 S2 -177.84(13) . . . . ?
C18 S8 C20 S10 177.23(14) . . . . ?
C18 S8 C20 S9 -1.99(14) . . . . ?
C19 S9 C20 S10 -177.36(14) . . . . ?
C19 S9 C20 S8 1.86(14) . . . . ?
C7 O3 C6 C5 -178.7(2) . . . . ?
C12 O6 C13 C14 -176.7(2) . . . . ?
S2 C16 C15 S1 -1.2(3) . . . . ?
S4 C16 C15 S1 179.00(11) . . . . ?
S2 C16 C15 S3 178.37(10) . . . . ?
S4 C16 C15 S3 -1.4(2) . . . . ?
Ni1 S1 C15 C16 0.58(18) . . . . ?
Ni1 S1 C15 S3 -178.99(11) . . . . ?
C17 S3 C15 C16 0.14(18) . . . . ?
C17 S3 C15 S1 179.73(13) . . . . ?
C6 O3 C7 C8 178.0(2) . . . . ?
C4 O2 C5 C6 -175.5(2) . . . . ?
O3 C6 C5 O2 -63.4(3) . . . . ?
S7 C19 C18 S6 0.9(3) . . . . ?
S9 C19 C18 S6 -179.76(10) . . . . ?
S7 C19 C18 S8 -179.69(11) . . . . ?
S9 C19 C18 S8 -0.3(2) . . . . ?
Ni1 S6 C18 C19 0.74(18) . . . . ?
Ni1 S6 C18 S8 -178.66(11) . . . . ?
C20 S8 C18 C19 1.42(18) . . . . ?
C20 S8 C18 S6 -179.15(13) . . . . ?
C9 O4 C8 C7 171.9(2) . . . . ?
O3 C7 C8 O4 64.3(3) . . . . ?
C14 O1 C3 C4 -176.4(2) . . . . ?
C10 O5 C11 C12 -171.2(2) . . . . ?
C11 O5 C10 C9 -177.9(2) . . . . ?
C16 S4 C17 S5 178.69(14) . . . . ?
C16 S4 C17 S3 -1.74(13) . . . . ?
C15 S3 C17 S5 -179.28(14) . . . . ?
C15 S3 C17 S4 1.15(14) . . . . ?
C8 O4 C9 C10 -177.3(2) . . . . ?
O5 C10 C9 O4 -66.9(3) . . . . ?
C5 O2 C4 C3 174.7(2) . . . . ?
O1 C3 C4 O2 65.3(3) . . . . ?
C13 O6 C12 C11 171.2(2) . . . . ?
O5 C11 C12 O6 64.0(3) . . . . ?
C3 O1 C14 C13 -177.1(2) . . . . ?
O6 C13 C14 O1 -66.6(3) . . . . ?

_refine_diff_density_max         0.322
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.060

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_373k
_database_code_depnum_ccdc_archive 'CCDC 2053296'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-19 downloaded from the CCDC.
;
_audit_creation_date             2020-11-11
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C12 H24 O6, C2 H7 F N'
_chemical_formula_sum            'C20 H31 F N Ni O6 S10'
_chemical_formula_weight         779.77
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHNOFNiS
_chemical_oxdiff_usercomment     20_20200608
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.5742(7)
_cell_length_b                   12.6426(7)
_cell_length_c                   13.0305(11)
_cell_angle_alpha                72.446(6)
_cell_angle_beta                 79.808(6)
_cell_angle_gamma                81.420(5)
_cell_volume                     1626.1(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7361
_cell_measurement_temperature    373
_cell_measurement_theta_max      27.0440
_cell_measurement_theta_min      1.8190
_shelx_estimated_absorpt_T_max   0.894
_shelx_estimated_absorpt_T_min   0.563
_exptl_absorpt_coefficient_mu    1.280
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52678
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             806
_exptl_crystal_size_max          0.507
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0728
_diffrn_reflns_av_unetI/netI     0.0784
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.855
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18911
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.855
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.027
_diffrn_reflns_theta_min         1.967
_diffrn_ambient_temperature      373
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.855
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -73.00  22.00   0.50    0.90    --   21.69 -74.00  92.00  190
  2  ω     31.00  57.00   0.50    0.90    --   21.69  74.00-139.00   52
  3  ω     49.00  98.00   0.50    0.90    --   21.69 178.00  90.00   98
  4  ω     46.00 103.00   0.50    0.90    --   21.69 178.00 120.00  114
  5  ω    -30.00  44.00   0.50    0.90    --  -21.62  74.00-139.00  148
  6  ω    -26.00  58.00   0.50    0.90    --  -21.62  37.00-150.00  168
  7  ω     13.00  39.00   0.50    0.90    --  -21.62  19.00 -90.00   52
  8  ω    -39.00  12.00   0.50    0.90    --  -21.62  37.00   0.00  102
  9  ω    -35.00  24.00   0.50    0.90    --  -21.62 -74.00  92.00  118
 10  ω    -80.00 -54.00   0.50    0.90    --  -21.62 -74.00  92.00   52
 11  ω   -123.00 -43.00   0.50    0.90    --  -21.62-178.00   0.00  160
 12  ω   -123.00 -44.00   0.50    0.90    --  -21.62-178.00-150.00  158
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0337873000
_diffrn_orient_matrix_UB_12      0.0043644000
_diffrn_orient_matrix_UB_13      -0.0437623000
_diffrn_orient_matrix_UB_21      -0.0492649000
_diffrn_orient_matrix_UB_22      0.0368011000
_diffrn_orient_matrix_UB_23      0.0193153000
_diffrn_orient_matrix_UB_31      0.0335451000
_diffrn_orient_matrix_UB_32      0.0461058000
_diffrn_orient_matrix_UB_33      -0.0321948000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4338
_reflns_number_total             7413
_reflns_odcompleteness_completeness 99.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.911
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         7413
_refine_ls_number_restraints     44
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_gt           0.0514
_refine_ls_restrained_S_all      0.910
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1505
_refine_ls_wR_factor_ref         0.1770
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
2. Rigid bond restraints
 O1, C3, C4, C14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
O1 \\sim C3 \\sim C14: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 C14, O1, C3, C4, O2, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H1AA)=Sof(H1AB)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(F1)=1-FVAR(1)
 Sof(H1BC)=Sof(H1BD)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(F1A)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C7(H7A,H7B), C6(H6A,H6B), C3(H3A,H3B), C4(H4A,H4B), C11(H11A,
 H11B), C8(H8A,H8B), C13(H13A,H13B), C12(H12A,H12B), C14(H14A,H14B), C1(H1BC,
 H1BD), C1(H1AA,H1AB), C9(H9A,H9B), C10(H10A,H10B), C2(H2A,H2B), C2A(H2AA,H2AB)
6.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.16372(4) 0.40481(3) 0.49208(3) 0.05829(17) Uani 1 1 d . . . . .
S2 S -0.07743(9) 0.26631(8) 0.29609(8) 0.0677(3) Uani 1 1 d . . . . .
S4 S 0.00740(9) 0.31495(8) 0.48581(7) 0.0656(3) Uani 1 1 d . . . . .
S6 S 0.10087(10) 0.36953(8) 0.66503(7) 0.0700(3) Uani 1 1 d . . . . .
S5 S 0.22963(9) 0.43853(8) 0.31975(7) 0.0692(3) Uani 1 1 d . . . . .
S8 S 0.19663(11) 0.43793(8) 0.83911(7) 0.0730(3) Uani 1 1 d . . . . .
S3 S 0.12936(10) 0.37505(9) 0.14466(7) 0.0765(3) Uani 1 1 d . . . . .
S9 S 0.40149(10) 0.54921(9) 0.68699(8) 0.0761(3) Uani 1 1 d . . . . .
S7 S 0.31701(10) 0.49765(9) 0.49782(7) 0.0731(3) Uani 1 1 d . . . . .
S10 S 0.37490(14) 0.54778(11) 0.91659(9) 0.0963(4) Uani 1 1 d . . . . .
S1 S -0.04681(13) 0.26340(12) 0.06649(10) 0.0984(4) Uani 1 1 d . . . . .
O2 O 0.1701(3) 0.8955(2) 0.2813(2) 0.0915(8) Uani 1 1 d . . . . .
O3 O 0.2675(3) 1.0634(2) 0.3288(2) 0.0900(8) Uani 1 1 d . . . . .
N1 N 0.4473(3) 0.8881(2) 0.2555(2) 0.0615(7) Uani 1 1 d . . . . .
H1A H 0.404978 0.872943 0.209189 0.074 Uiso 1 1 calc R U . . .
H1B H 0.515849 0.922863 0.219047 0.074 Uiso 1 1 calc R U . . .
H1C H 0.395275 0.931782 0.290851 0.074 Uiso 1 1 calc R U . . .
O5 O 0.6850(3) 0.9826(3) 0.1435(3) 0.1014(9) Uani 1 1 d . . . . .
O1 O 0.3210(3) 0.8062(2) 0.1219(2) 0.0948(8) Uani 1 1 d . U . . .
O6 O 0.5902(4) 0.8196(3) 0.0785(2) 0.1025(10) Uani 1 1 d . . . . .
O4 O 0.5365(3) 1.0736(2) 0.2989(2) 0.0935(8) Uani 1 1 d . . . . .
C16 C 0.0242(3) 0.3246(3) 0.3505(3) 0.0581(8) Uani 1 1 d . . . . .
C18 C 0.2054(4) 0.4352(3) 0.7047(3) 0.0604(8) Uani 1 1 d . . . . .
C19 C 0.3005(3) 0.4894(3) 0.6333(3) 0.0621(8) Uani 1 1 d . . . . .
C17 C 0.1208(4) 0.3770(3) 0.2793(3) 0.0617(8) Uani 1 1 d . . . . .
C20 C 0.3259(4) 0.5148(3) 0.8189(3) 0.0703(10) Uani 1 1 d . . . . .
C15 C 0.0006(4) 0.2996(3) 0.1637(3) 0.0702(9) Uani 1 1 d . . . . .
C5 C 0.0920(5) 0.9808(4) 0.3188(4) 0.1027(15) Uani 1 1 d . . . . .
H5A H 0.011094 0.953556 0.358265 0.123 Uiso 1 1 calc R U . . .
H5B H 0.072659 1.043622 0.257265 0.123 Uiso 1 1 calc R U . . .
C7 C 0.3313(5) 1.1144(4) 0.3867(4) 0.1003(15) Uani 1 1 d . . . . .
H7A H 0.357400 1.059397 0.451335 0.120 Uiso 1 1 calc R U . . .
H7B H 0.273215 1.172976 0.408863 0.120 Uiso 1 1 calc R U . . .
C6 C 0.1575(5) 1.0169(4) 0.3895(4) 0.1046(15) Uani 1 1 d . . . . .
H6A H 0.100914 1.071521 0.419154 0.126 Uiso 1 1 calc R U . . .
H6B H 0.180907 0.953765 0.449371 0.126 Uiso 1 1 calc R U . . .
C3 C 0.2007(5) 0.7662(4) 0.1812(4) 0.1044(14) Uani 1 1 d . U . . .
H3A H 0.217066 0.706021 0.245644 0.125 Uiso 1 1 calc R U . . .
H3B H 0.158541 0.737702 0.136185 0.125 Uiso 1 1 calc R U . . .
C4 C 0.1175(5) 0.8575(4) 0.2123(4) 0.1029(14) Uani 1 1 d . U . . .
H4A H 0.103652 0.918188 0.147592 0.123 Uiso 1 1 calc R U . . .
H4B H 0.034172 0.832167 0.247448 0.123 Uiso 1 1 calc R U . . .
C11 C 0.7686(5) 0.9056(5) 0.0926(5) 0.123(2) Uani 1 1 d . . . . .
H11A H 0.796543 0.839301 0.147521 0.148 Uiso 1 1 calc R U . . .
H11B H 0.844411 0.940165 0.050328 0.148 Uiso 1 1 calc R U . . .
C8 C 0.4443(6) 1.1608(4) 0.3156(4) 0.1016(15) Uani 1 1 d . . . . .
H8A H 0.419794 1.207316 0.246554 0.122 Uiso 1 1 calc R U . . .
H8B H 0.480422 1.206746 0.348546 0.122 Uiso 1 1 calc R U . . .
C13 C 0.5174(6) 0.7774(5) 0.0161(4) 0.117(2) Uani 1 1 d . . . . .
H13A H 0.490970 0.837839 -0.044816 0.140 Uiso 1 1 calc R U . . .
H13B H 0.572121 0.721098 -0.012558 0.140 Uiso 1 1 calc R U . . .
C12 C 0.6936(6) 0.8753(5) 0.0204(4) 0.125(2) Uani 1 1 d . . . . .
H12A H 0.662917 0.942596 -0.032012 0.150 Uiso 1 1 calc R U . . .
H12B H 0.749829 0.828684 -0.019435 0.150 Uiso 1 1 calc R U . . .
C14 C 0.4033(7) 0.7291(5) 0.0851(5) 0.1219(18) Uani 1 1 d . U . . .
H14A H 0.359223 0.697324 0.043839 0.146 Uiso 1 1 calc R U . . .
H14B H 0.430045 0.669396 0.146403 0.146 Uiso 1 1 calc R U . . .
C1 C 0.4898(6) 0.7832(4) 0.3343(4) 0.1023(16) Uani 1 1 d . . . . .
H1BC H 0.426679 0.730999 0.345613 0.123 Uiso 0.69(2) 1 calc R U P A 2
H1BD H 0.570629 0.752069 0.301298 0.123 Uiso 0.69(2) 1 calc R U P A 2
H1AA H 0.493654 0.722035 0.302962 0.123 Uiso 0.31(2) 1 calc R U P A 1
H1AB H 0.576408 0.787349 0.346947 0.123 Uiso 0.31(2) 1 calc R U P A 1
C9 C 0.6578(5) 1.1112(5) 0.2431(5) 0.1137(17) Uani 1 1 d . . . . .
H9A H 0.697888 1.140220 0.289008 0.136 Uiso 1 1 calc R U . . .
H9B H 0.644564 1.170534 0.177337 0.136 Uiso 1 1 calc R U . . .
C10 C 0.7431(5) 1.0164(5) 0.2153(5) 0.124(2) Uani 1 1 d . . . . .
H10A H 0.827663 1.039424 0.181369 0.149 Uiso 1 1 calc R U . . .
H10B H 0.753281 0.955331 0.280489 0.149 Uiso 1 1 calc R U . . .
C2 C 0.508(2) 0.7886(14) 0.4336(7) 0.140(7) Uani 0.69(2) 1 d . . P A 2
H2A H 0.551336 0.852706 0.427964 0.168 Uiso 0.69(2) 1 calc R U P A 2
H2B H 0.554652 0.721159 0.473220 0.168 Uiso 0.69(2) 1 calc R U P A 2
C2A C 0.413(3) 0.7614(16) 0.4289(14) 0.080(6) Uani 0.31(2) 1 d . . P A 1
H2AA H 0.444161 0.689719 0.474834 0.096 Uiso 0.31(2) 1 calc R U P A 1
H2AB H 0.326940 0.755518 0.416347 0.096 Uiso 0.31(2) 1 calc R U P A 1
F1A F 0.4055(18) 0.8420(11) 0.4840(9) 0.142(5) Uani 0.69(2) 1 d . . P A 1
F1 F 0.369(3) 0.800(3) 0.484(3) 0.155(12) Uani 0.31(2) 1 d . . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S4 2.1665(10) . ?
Ni1 S6 2.1614(10) . ?
Ni1 S5 2.1603(9) . ?
Ni1 S7 2.1619(10) . ?
S2 C16 1.739(3) . ?
S2 C15 1.731(4) . ?
S4 C16 1.709(4) . ?
S6 C18 1.707(4) . ?
S5 C17 1.714(4) . ?
S8 C18 1.748(3) . ?
S8 C20 1.731(4) . ?
S3 C17 1.748(3) . ?
S3 C15 1.718(4) . ?
S9 C19 1.740(3) . ?
S9 C20 1.718(4) . ?
S7 C19 1.716(4) . ?
S10 C20 1.637(4) . ?
S1 C15 1.645(4) . ?
O2 C5 1.413(5) . ?
O2 C4 1.366(5) . ?
O3 C7 1.429(5) . ?
O3 C6 1.386(5) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.477(5) . ?
O5 C11 1.447(6) . ?
O5 C10 1.400(6) . ?
O1 C3 1.442(5) . ?
O1 C14 1.348(6) . ?
O6 C13 1.464(6) . ?
O6 C12 1.370(7) . ?
O4 C8 1.401(5) . ?
O4 C9 1.429(6) . ?
C16 C17 1.356(5) . ?
C18 C19 1.355(5) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.452(7) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.456(7) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.457(7) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.494(8) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.464(8) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C1 H1BC 0.9700 . ?
C1 H1BD 0.9700 . ?
C1 H1AA 0.9700 . ?
C1 H1AB 0.9700 . ?
C1 C2 1.363(13) . ?
C1 C2A 1.328(18) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.485(7) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 F1 1.50(3) . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?
C2A F1A 1.40(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S6 Ni1 S4 87.15(4) . . ?
S6 Ni1 S7 92.83(4) . . ?
S5 Ni1 S4 93.32(4) . . ?
S5 Ni1 S6 179.04(5) . . ?
S5 Ni1 S7 86.72(3) . . ?
S7 Ni1 S4 178.81(4) . . ?
C15 S2 C16 97.39(17) . . ?
C16 S4 Ni1 101.93(12) . . ?
C18 S6 Ni1 102.20(11) . . ?
C17 S5 Ni1 101.64(12) . . ?
C20 S8 C18 97.18(17) . . ?
C15 S3 C17 97.41(17) . . ?
C20 S9 C19 97.42(17) . . ?
C19 S7 Ni1 102.40(12) . . ?
C4 O2 C5 114.8(4) . . ?
C6 O3 C7 113.2(4) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
C10 O5 C11 113.7(4) . . ?
C14 O1 C3 114.0(4) . . ?
C12 O6 C13 115.8(4) . . ?
C8 O4 C9 112.9(4) . . ?
S4 C16 S2 122.8(2) . . ?
C17 C16 S2 116.0(3) . . ?
C17 C16 S4 121.2(3) . . ?
S6 C18 S8 122.5(2) . . ?
C19 C18 S6 121.9(3) . . ?
C19 C18 S8 115.6(3) . . ?
S7 C19 S9 123.0(2) . . ?
C18 C19 S9 116.3(3) . . ?
C18 C19 S7 120.7(3) . . ?
S5 C17 S3 122.2(2) . . ?
C16 C17 S5 121.9(3) . . ?
C16 C17 S3 115.9(3) . . ?
S9 C20 S8 113.4(2) . . ?
S10 C20 S8 123.5(2) . . ?
S10 C20 S9 123.1(2) . . ?
S3 C15 S2 113.3(2) . . ?
S1 C15 S2 122.7(2) . . ?
S1 C15 S3 124.1(2) . . ?
O2 C5 H5A 109.6 . . ?
O2 C5 H5B 109.6 . . ?
O2 C5 C6 110.5(4) . . ?
H5A C5 H5B 108.1 . . ?
C6 C5 H5A 109.6 . . ?
C6 C5 H5B 109.6 . . ?
O3 C7 H7A 110.0 . . ?
O3 C7 H7B 110.0 . . ?
O3 C7 C8 108.6(4) . . ?
H7A C7 H7B 108.3 . . ?
C8 C7 H7A 110.0 . . ?
C8 C7 H7B 110.0 . . ?
O3 C6 C5 108.3(4) . . ?
O3 C6 H6A 110.0 . . ?
O3 C6 H6B 110.0 . . ?
C5 C6 H6A 110.0 . . ?
C5 C6 H6B 110.0 . . ?
H6A C6 H6B 108.4 . . ?
O1 C3 H3A 109.8 . . ?
O1 C3 H3B 109.8 . . ?
O1 C3 C4 109.2(4) . . ?
H3A C3 H3B 108.3 . . ?
C4 C3 H3A 109.8 . . ?
C4 C3 H3B 109.8 . . ?
O2 C4 C3 111.6(4) . . ?
O2 C4 H4A 109.3 . . ?
O2 C4 H4B 109.3 . . ?
C3 C4 H4A 109.3 . . ?
C3 C4 H4B 109.3 . . ?
H4A C4 H4B 108.0 . . ?
O5 C11 H11A 110.2 . . ?
O5 C11 H11B 110.2 . . ?
O5 C11 C12 107.7(4) . . ?
H11A C11 H11B 108.5 . . ?
C12 C11 H11A 110.2 . . ?
C12 C11 H11B 110.2 . . ?
O4 C8 C7 109.2(4) . . ?
O4 C8 H8A 109.8 . . ?
O4 C8 H8B 109.8 . . ?
C7 C8 H8A 109.8 . . ?
C7 C8 H8B 109.8 . . ?
H8A C8 H8B 108.3 . . ?
O6 C13 H13A 109.6 . . ?
O6 C13 H13B 109.6 . . ?
H13A C13 H13B 108.1 . . ?
C14 C13 O6 110.4(4) . . ?
C14 C13 H13A 109.6 . . ?
C14 C13 H13B 109.6 . . ?
O6 C12 C11 111.7(4) . . ?
O6 C12 H12A 109.3 . . ?
O6 C12 H12B 109.3 . . ?
C11 C12 H12A 109.3 . . ?
C11 C12 H12B 109.3 . . ?
H12A C12 H12B 107.9 . . ?
O1 C14 C13 111.5(5) . . ?
O1 C14 H14A 109.3 . . ?
O1 C14 H14B 109.3 . . ?
C13 C14 H14A 109.3 . . ?
C13 C14 H14B 109.3 . . ?
H14A C14 H14B 108.0 . . ?
N1 C1 H1BC 107.9 . . ?
N1 C1 H1BD 107.9 . . ?
N1 C1 H1AA 108.9 . . ?
N1 C1 H1AB 108.9 . . ?
H1BC C1 H1BD 107.2 . . ?
H1AA C1 H1AB 107.7 . . ?
C2 C1 N1 117.5(7) . . ?
C2 C1 H1BC 107.9 . . ?
C2 C1 H1BD 107.9 . . ?
C2A C1 N1 113.4(12) . . ?
C2A C1 H1AA 108.9 . . ?
C2A C1 H1AB 108.9 . . ?
O4 C9 H9A 109.8 . . ?
O4 C9 H9B 109.8 . . ?
O4 C9 C10 109.2(4) . . ?
H9A C9 H9B 108.3 . . ?
C10 C9 H9A 109.8 . . ?
C10 C9 H9B 109.8 . . ?
O5 C10 C9 107.5(4) . . ?
O5 C10 H10A 110.2 . . ?
O5 C10 H10B 110.2 . . ?
C9 C10 H10A 110.2 . . ?
C9 C10 H10B 110.2 . . ?
H10A C10 H10B 108.5 . . ?
C1 C2 H2A 111.9 . . ?
C1 C2 H2B 111.9 . . ?
C1 C2 F1 99.3(18) . . ?
H2A C2 H2B 109.6 . . ?
F1 C2 H2A 111.9 . . ?
F1 C2 H2B 111.9 . . ?
C1 C2A H2AA 108.8 . . ?
C1 C2A H2AB 108.8 . . ?
C1 C2A F1A 113.7(13) . . ?
H2AA C2A H2AB 107.7 . . ?
F1A C2A H2AA 108.8 . . ?
F1A C2A H2AB 108.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S4 C16 S2 -179.92(19) . . . . ?
Ni1 S4 C16 C17 1.4(3) . . . . ?
Ni1 S6 C18 S8 178.09(19) . . . . ?
Ni1 S6 C18 C19 -1.5(3) . . . . ?
Ni1 S5 C17 S3 -178.4(2) . . . . ?
Ni1 S5 C17 C16 0.1(3) . . . . ?
Ni1 S7 C19 S9 179.3(2) . . . . ?
Ni1 S7 C19 C18 -1.1(3) . . . . ?
S2 C16 C17 S5 -179.86(19) . . . . ?
S2 C16 C17 S3 -1.2(4) . . . . ?
S4 C16 C17 S5 -1.1(5) . . . . ?
S4 C16 C17 S3 177.49(19) . . . . ?
S6 C18 C19 S9 -178.49(19) . . . . ?
S6 C18 C19 S7 1.9(5) . . . . ?
S8 C18 C19 S9 1.9(4) . . . . ?
S8 C18 C19 S7 -177.74(19) . . . . ?
O2 C5 C6 O3 63.8(5) . . . . ?
O3 C7 C8 O4 -69.3(5) . . . . ?
N1 C1 C2 F1 75.6(16) . . . . ?
N1 C1 C2A F1A -62(2) . . . . ?
O5 C11 C12 O6 -63.8(6) . . . . ?
O1 C3 C4 O2 -63.2(5) . . . . ?
O6 C13 C14 O1 62.6(6) . . . . ?
O4 C9 C10 O5 63.4(5) . . . . ?
C16 S2 C15 S3 -2.6(3) . . . . ?
C16 S2 C15 S1 178.3(3) . . . . ?
C18 S8 C20 S9 -1.2(2) . . . . ?
C18 S8 C20 S10 -179.0(3) . . . . ?
C19 S9 C20 S8 2.0(3) . . . . ?
C19 S9 C20 S10 179.8(3) . . . . ?
C17 S3 C15 S2 2.1(3) . . . . ?
C17 S3 C15 S1 -178.8(3) . . . . ?
C20 S8 C18 S6 180.0(2) . . . . ?
C20 S8 C18 C19 -0.4(3) . . . . ?
C20 S9 C19 S7 177.3(2) . . . . ?
C20 S9 C19 C18 -2.4(3) . . . . ?
C15 S2 C16 S4 -176.4(2) . . . . ?
C15 S2 C16 C17 2.3(3) . . . . ?
C15 S3 C17 S5 178.1(2) . . . . ?
C15 S3 C17 C16 -0.5(3) . . . . ?
C5 O2 C4 C3 -177.3(4) . . . . ?
C7 O3 C6 C5 172.7(4) . . . . ?
C6 O3 C7 C8 -179.7(4) . . . . ?
C3 O1 C14 C13 174.0(4) . . . . ?
C4 O2 C5 C6 -178.8(4) . . . . ?
C11 O5 C10 C9 168.5(4) . . . . ?
C8 O4 C9 C10 -172.1(4) . . . . ?
C13 O6 C12 C11 -174.7(4) . . . . ?
C12 O6 C13 C14 -174.7(4) . . . . ?
C14 O1 C3 C4 -177.3(4) . . . . ?
C9 O4 C8 C7 -171.5(4) . . . . ?
C10 O5 C11 C12 178.9(4) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 5.319
_oxdiff_exptl_absorpt_empirical_full_min 0.192
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_313k
_database_code_depnum_ccdc_archive 'CCDC 2053293'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-19 downloaded from the CCDC.
;
_audit_creation_date             2020-11-11
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C12 H24 O6, C2 H7 F N'
_chemical_formula_sum            'C20 H31 F N Ni O6 S10'
_chemical_formula_weight         779.77
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHNOFNiS
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.5377(3)
_cell_length_b                   12.6697(3)
_cell_length_c                   13.0079(4)
_cell_angle_alpha                71.903(2)
_cell_angle_beta                 79.822(2)
_cell_angle_gamma                80.956(2)
_cell_volume                     1615.05(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9065
_cell_measurement_temperature    313
_cell_measurement_theta_max      27.9340
_cell_measurement_theta_min      1.8490
_shelx_estimated_absorpt_T_max   0.893
_shelx_estimated_absorpt_T_min   0.561
_exptl_absorpt_coefficient_mu    1.289
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73320
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             806
_exptl_crystal_size_max          0.507
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.853
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17913
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.853
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.003
_diffrn_reflns_theta_min         2.403
_diffrn_ambient_temperature      313
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.853
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      9.00  67.00   0.50    0.80    --   21.85  67.00-137.00  116
  2  ω     46.00 104.00   0.50    0.80    --   21.85 178.00   0.00  116
  3  ω     50.00  91.00   0.50    0.80    --   21.85 178.00  90.00   82
  4  ω     51.00 104.00   0.50    0.80    --   21.85 178.00 120.00  106
  5  ω    -67.00  65.00   0.50    0.80    --   21.85 -67.00  87.00  264
  6  ω    -24.00  60.00   0.50    0.80    --  -21.77  19.00-150.00  168
  7  ω     -4.00  36.00   0.50    0.80    --  -21.77 -99.00-150.00   80
  8  ω   -109.00   4.00   0.50    0.80    --  -21.77 -67.00  87.00  226
  9  ω    -40.00  -3.00   0.50    0.80    --  -21.77  37.00   0.00   74
 10  ω    -27.00  -2.00   0.50    0.80    --  -21.77  67.00-137.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0367316000
_diffrn_orient_matrix_UB_12      -0.0010010000
_diffrn_orient_matrix_UB_13      -0.0403605000
_diffrn_orient_matrix_UB_21      -0.0503813000
_diffrn_orient_matrix_UB_22      0.0365112000
_diffrn_orient_matrix_UB_23      0.0188355000
_diffrn_orient_matrix_UB_31      0.0290839000
_diffrn_orient_matrix_UB_32      0.0466565000
_diffrn_orient_matrix_UB_33      -0.0370051000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5289
_reflns_number_total             7336
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         7336
_refine_ls_number_restraints     261
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0354
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0382P)²+0.3111P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0938
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(H1AA)=Sof(H1AB)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(F1)=1-FVAR(1)
 Sof(H1BC)=Sof(H1BD)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(F1A)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C7(H7A,H7B), C6(H6A,H6B), C3(H3A,H3B), C4(H4A,H4B), C11(H11A,
 H11B), C8(H8A,H8B), C13(H13A,H13B), C12(H12A,H12B), C14(H14A,H14B), C1(H1BC,
 H1BD), C1(H1AA,H1AB), C9(H9A,H9B), C10(H10A,H10B), C2(H2A,H2B), C2A(H2AA,H2AB)
4.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.16324(3) 0.40445(2) 0.49232(2) 0.04443(9) Uani 1 1 d . . . . .
S2 S -0.07894(6) 0.26663(5) 0.29639(5) 0.05113(15) Uani 1 1 d . . . . .
S4 S 0.00659(6) 0.31474(5) 0.48664(5) 0.05030(15) Uani 1 1 d . . . . .
S6 S 0.10015(6) 0.36923(5) 0.66624(5) 0.05368(16) Uani 1 1 d . . . . .
S5 S 0.22917(6) 0.43837(5) 0.31878(5) 0.05367(16) Uani 1 1 d . . . . .
S8 S 0.19589(7) 0.43731(5) 0.84078(5) 0.05556(16) Uani 1 1 d . . . . .
S3 S 0.12901(6) 0.37464(6) 0.14351(5) 0.05916(17) Uani 1 1 d . . . . .
S9 S 0.40167(6) 0.54834(6) 0.68721(5) 0.05932(17) Uani 1 1 d . . . . .
S7 S 0.31662(6) 0.49750(6) 0.49745(5) 0.05704(17) Uani 1 1 d . . . . .
S10 S 0.37477(8) 0.54724(7) 0.91783(6) 0.0742(2) Uani 1 1 d . . . . .
S1 S -0.04840(8) 0.26351(7) 0.06592(6) 0.0757(2) Uani 1 1 d . . . . .
O2 O 0.16960(17) 0.89600(14) 0.28319(15) 0.0638(4) Uani 1 1 d . . . . .
O3 O 0.26773(18) 1.06451(15) 0.32957(14) 0.0649(5) Uani 1 1 d . . . . .
N1 N 0.44718(18) 0.89000(14) 0.25488(14) 0.0477(4) Uani 1 1 d . . . . .
H1A H 0.400205 0.875319 0.211443 0.057 Uiso 1 1 calc R U . . .
H1B H 0.515512 0.923110 0.214872 0.057 Uiso 1 1 calc R U . . .
H1C H 0.398876 0.935057 0.290700 0.057 Uiso 1 1 calc R U . . .
O5 O 0.68638(18) 0.98131(16) 0.14147(16) 0.0731(5) Uani 1 1 d . . . . .
O1 O 0.31985(19) 0.80759(14) 0.12190(15) 0.0678(5) Uani 1 1 d . . . . .
O6 O 0.5897(2) 0.81856(16) 0.07840(14) 0.0730(5) Uani 1 1 d . . . . .
O4 O 0.53886(19) 1.07335(15) 0.29865(16) 0.0708(5) Uani 1 1 d . . . . .
C16 C 0.0238(2) 0.32446(17) 0.35047(18) 0.0445(5) Uani 1 1 d . . . . .
C18 C 0.2051(2) 0.43474(17) 0.70636(18) 0.0459(5) Uani 1 1 d . . . . .
C19 C 0.2996(2) 0.48933(19) 0.63370(19) 0.0481(5) Uani 1 1 d . . . . .
C17 C 0.1207(2) 0.37646(18) 0.27836(18) 0.0468(5) Uani 1 1 d . . . . .
C20 C 0.3253(2) 0.51355(19) 0.82062(19) 0.0523(6) Uani 1 1 d . . . . .
C15 C -0.0011(2) 0.2993(2) 0.16352(19) 0.0542(6) Uani 1 1 d . . . . .
C5 C 0.0884(3) 0.9814(2) 0.3194(2) 0.0715(7) Uani 1 1 d . . . . .
H5A H 0.007541 0.953716 0.358911 0.086 Uiso 1 1 calc R U . . .
H5B H 0.068658 1.044337 0.257140 0.086 Uiso 1 1 calc R U . . .
C7 C 0.3320(3) 1.1145(2) 0.3877(2) 0.0738(8) Uani 1 1 d . . . . .
H7A H 0.358959 1.058758 0.452495 0.089 Uiso 1 1 calc R U . . .
H7B H 0.273403 1.172796 0.410393 0.089 Uiso 1 1 calc R U . . .
C6 C 0.1556(3) 1.0172(2) 0.3913(2) 0.0731(8) Uani 1 1 d . . . . .
H6A H 0.098724 1.071756 0.421017 0.088 Uiso 1 1 calc R U . . .
H6B H 0.179478 0.953543 0.451551 0.088 Uiso 1 1 calc R U . . .
C3 C 0.2012(3) 0.7660(2) 0.1827(2) 0.0747(8) Uani 1 1 d . . . . .
H3A H 0.219581 0.706646 0.248094 0.090 Uiso 1 1 calc R U . . .
H3B H 0.159604 0.735795 0.138856 0.090 Uiso 1 1 calc R U . . .
C4 C 0.1144(3) 0.8586(2) 0.2127(2) 0.0720(8) Uani 1 1 d . . . . .
H4A H 0.100381 0.919580 0.147424 0.086 Uiso 1 1 calc R U . . .
H4B H 0.031072 0.833198 0.248082 0.086 Uiso 1 1 calc R U . . .
C11 C 0.7687(3) 0.9043(3) 0.0915(3) 0.0876(9) Uani 1 1 d . . . . .
H11A H 0.795704 0.837286 0.147234 0.105 Uiso 1 1 calc R U . . .
H11B H 0.845594 0.937819 0.049932 0.105 Uiso 1 1 calc R U . . .
C8 C 0.4463(3) 1.1623(2) 0.3154(3) 0.0755(8) Uani 1 1 d . . . . .
H8A H 0.421350 1.209841 0.246158 0.091 Uiso 1 1 calc R U . . .
H8B H 0.483037 1.207177 0.348726 0.091 Uiso 1 1 calc R U . . .
C13 C 0.5189(3) 0.7799(3) 0.0144(2) 0.0855(9) Uani 1 1 d . . . . .
H13A H 0.574826 0.726034 -0.016854 0.103 Uiso 1 1 calc R U . . .
H13B H 0.489988 0.842318 -0.044873 0.103 Uiso 1 1 calc R U . . .
C12 C 0.6948(3) 0.8754(3) 0.0180(3) 0.0875(9) Uani 1 1 d . . . . .
H12A H 0.663612 0.943165 -0.034712 0.105 Uiso 1 1 calc R U . . .
H12B H 0.751643 0.828882 -0.021671 0.105 Uiso 1 1 calc R U . . .
C14 C 0.4056(4) 0.7276(3) 0.0845(3) 0.0858(9) Uani 1 1 d . . . . .
H14A H 0.362186 0.695678 0.043257 0.103 Uiso 1 1 calc R U . . .
H14B H 0.434099 0.667948 0.146099 0.103 Uiso 1 1 calc R U . . .
C1 C 0.4921(4) 0.7843(2) 0.3342(2) 0.0835(9) Uani 1 1 d . . . . .
H1BC H 0.430503 0.731049 0.345300 0.100 Uiso 0.620(11) 1 calc R U P A 2
H1BD H 0.574468 0.754401 0.301814 0.100 Uiso 0.620(11) 1 calc R U P A 2
H1AA H 0.495613 0.723491 0.302903 0.100 Uiso 0.380(11) 1 calc R U P A 1
H1AB H 0.579589 0.788579 0.345230 0.100 Uiso 0.380(11) 1 calc R U P A 1
C9 C 0.6605(3) 1.1104(3) 0.2433(3) 0.0855(9) Uani 1 1 d . . . . .
H9A H 0.701503 1.137111 0.290291 0.103 Uiso 1 1 calc R U . . .
H9B H 0.647252 1.171562 0.177986 0.103 Uiso 1 1 calc R U . . .
C10 C 0.7456(3) 1.0157(3) 0.2135(3) 0.0875(9) Uani 1 1 d . . . . .
H10A H 0.829912 1.039011 0.178505 0.105 Uiso 1 1 calc R U . . .
H10B H 0.757658 0.953987 0.278685 0.105 Uiso 1 1 calc R U . . .
C2 C 0.5075(9) 0.7910(6) 0.4348(4) 0.092(3) Uani 0.620(11) 1 d . . P A 2
H2A H 0.557945 0.851523 0.426979 0.111 Uiso 0.620(11) 1 calc R U P A 2
H2B H 0.550741 0.721680 0.476709 0.111 Uiso 0.620(11) 1 calc R U P A 2
C2A C 0.4164(14) 0.7596(7) 0.4333(7) 0.070(3) Uani 0.380(11) 1 d . . P A 1
H2AA H 0.452580 0.689731 0.480099 0.085 Uiso 0.380(11) 1 calc R U P A 1
H2AB H 0.330136 0.749958 0.423758 0.085 Uiso 0.380(11) 1 calc R U P A 1
F1A F 0.4075(14) 0.8453(9) 0.4847(8) 0.108(3) Uani 0.620(11) 1 d . . P A 1
F1 F 0.372(2) 0.8128(17) 0.4888(15) 0.114(5) Uani 0.380(11) 1 d . . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S4 2.1697(6) . ?
Ni1 S6 2.1665(6) . ?
Ni1 S5 2.1680(6) . ?
Ni1 S7 2.1662(6) . ?
S2 C16 1.744(2) . ?
S2 C15 1.730(2) . ?
S4 C16 1.716(2) . ?
S6 C18 1.716(2) . ?
S5 C17 1.717(2) . ?
S8 C18 1.744(2) . ?
S8 C20 1.730(2) . ?
S3 C17 1.748(2) . ?
S3 C15 1.729(2) . ?
S9 C19 1.744(2) . ?
S9 C20 1.731(2) . ?
S7 C19 1.721(2) . ?
S10 C20 1.641(2) . ?
S1 C15 1.649(2) . ?
O2 C5 1.417(3) . ?
O2 C4 1.395(3) . ?
O3 C7 1.431(3) . ?
O3 C6 1.410(3) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.483(3) . ?
O5 C11 1.434(3) . ?
O5 C10 1.415(4) . ?
O1 C3 1.437(3) . ?
O1 C14 1.394(3) . ?
O6 C13 1.441(4) . ?
O6 C12 1.398(4) . ?
O4 C8 1.415(3) . ?
O4 C9 1.427(3) . ?
C16 C17 1.359(3) . ?
C18 C19 1.357(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.477(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.476(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.479(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.492(5) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.478(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C1 H1BC 0.9700 . ?
C1 H1BD 0.9700 . ?
C1 H1AA 0.9700 . ?
C1 H1AB 0.9700 . ?
C1 C2 1.376(7) . ?
C1 C2A 1.364(11) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.491(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 F1 1.50(2) . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?
C2A F1A 1.425(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S6 Ni1 S4 87.16(2) . . ?
S6 Ni1 S5 179.15(3) . . ?
S5 Ni1 S4 93.26(2) . . ?
S7 Ni1 S4 178.69(3) . . ?
S7 Ni1 S6 92.80(2) . . ?
S7 Ni1 S5 86.80(2) . . ?
C15 S2 C16 97.44(11) . . ?
C16 S4 Ni1 101.84(7) . . ?
C18 S6 Ni1 102.46(8) . . ?
C17 S5 Ni1 101.85(8) . . ?
C20 S8 C18 97.25(11) . . ?
C15 S3 C17 97.33(11) . . ?
C20 S9 C19 97.26(11) . . ?
C19 S7 Ni1 102.34(8) . . ?
C4 O2 C5 112.9(2) . . ?
C6 O3 C7 113.3(2) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
C10 O5 C11 114.1(2) . . ?
C14 O1 C3 113.3(2) . . ?
C12 O6 C13 114.1(2) . . ?
C8 O4 C9 112.4(2) . . ?
S4 C16 S2 122.54(13) . . ?
C17 C16 S2 115.94(17) . . ?
C17 C16 S4 121.52(17) . . ?
S6 C18 S8 122.63(13) . . ?
C19 C18 S6 121.23(17) . . ?
C19 C18 S8 116.13(17) . . ?
S7 C19 S9 122.84(14) . . ?
C18 C19 S9 115.99(17) . . ?
C18 C19 S7 121.17(17) . . ?
S5 C17 S3 122.48(13) . . ?
C16 C17 S5 121.52(17) . . ?
C16 C17 S3 116.00(17) . . ?
S8 C20 S9 113.27(13) . . ?
S10 C20 S8 124.02(15) . . ?
S10 C20 S9 122.68(15) . . ?
S3 C15 S2 113.22(13) . . ?
S1 C15 S2 123.04(14) . . ?
S1 C15 S3 123.74(15) . . ?
O2 C5 H5A 109.9 . . ?
O2 C5 H5B 109.9 . . ?
O2 C5 C6 109.0(2) . . ?
H5A C5 H5B 108.3 . . ?
C6 C5 H5A 109.9 . . ?
C6 C5 H5B 109.9 . . ?
O3 C7 H7A 109.9 . . ?
O3 C7 H7B 109.9 . . ?
O3 C7 C8 108.7(2) . . ?
H7A C7 H7B 108.3 . . ?
C8 C7 H7A 109.9 . . ?
C8 C7 H7B 109.9 . . ?
O3 C6 C5 108.6(2) . . ?
O3 C6 H6A 110.0 . . ?
O3 C6 H6B 110.0 . . ?
C5 C6 H6A 110.0 . . ?
C5 C6 H6B 110.0 . . ?
H6A C6 H6B 108.4 . . ?
O1 C3 H3A 109.9 . . ?
O1 C3 H3B 109.9 . . ?
O1 C3 C4 108.9(2) . . ?
H3A C3 H3B 108.3 . . ?
C4 C3 H3A 109.9 . . ?
C4 C3 H3B 109.9 . . ?
O2 C4 C3 110.0(2) . . ?
O2 C4 H4A 109.7 . . ?
O2 C4 H4B 109.7 . . ?
C3 C4 H4A 109.7 . . ?
C3 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
O5 C11 H11A 110.0 . . ?
O5 C11 H11B 110.0 . . ?
O5 C11 C12 108.5(2) . . ?
H11A C11 H11B 108.4 . . ?
C12 C11 H11A 110.0 . . ?
C12 C11 H11B 110.0 . . ?
O4 C8 C7 108.3(2) . . ?
O4 C8 H8A 110.0 . . ?
O4 C8 H8B 110.0 . . ?
C7 C8 H8A 110.0 . . ?
C7 C8 H8B 110.0 . . ?
H8A C8 H8B 108.4 . . ?
O6 C13 H13A 109.7 . . ?
O6 C13 H13B 109.7 . . ?
O6 C13 C14 109.6(2) . . ?
H13A C13 H13B 108.2 . . ?
C14 C13 H13A 109.7 . . ?
C14 C13 H13B 109.7 . . ?
O6 C12 C11 110.5(2) . . ?
O6 C12 H12A 109.6 . . ?
O6 C12 H12B 109.6 . . ?
C11 C12 H12A 109.6 . . ?
C11 C12 H12B 109.6 . . ?
H12A C12 H12B 108.1 . . ?
O1 C14 C13 109.7(3) . . ?
O1 C14 H14A 109.7 . . ?
O1 C14 H14B 109.7 . . ?
C13 C14 H14A 109.7 . . ?
C13 C14 H14B 109.7 . . ?
H14A C14 H14B 108.2 . . ?
N1 C1 H1BC 108.2 . . ?
N1 C1 H1BD 108.2 . . ?
N1 C1 H1AA 108.6 . . ?
N1 C1 H1AB 108.6 . . ?
H1BC C1 H1BD 107.3 . . ?
H1AA C1 H1AB 107.6 . . ?
C2 C1 N1 116.4(4) . . ?
C2 C1 H1BC 108.2 . . ?
C2 C1 H1BD 108.2 . . ?
C2A C1 N1 114.6(5) . . ?
C2A C1 H1AA 108.6 . . ?
C2A C1 H1AB 108.6 . . ?
O4 C9 H9A 109.9 . . ?
O4 C9 H9B 109.9 . . ?
O4 C9 C10 109.1(2) . . ?
H9A C9 H9B 108.3 . . ?
C10 C9 H9A 109.9 . . ?
C10 C9 H9B 109.9 . . ?
O5 C10 C9 108.8(2) . . ?
O5 C10 H10A 109.9 . . ?
O5 C10 H10B 109.9 . . ?
C9 C10 H10A 109.9 . . ?
C9 C10 H10B 109.9 . . ?
H10A C10 H10B 108.3 . . ?
C1 C2 H2A 110.9 . . ?
C1 C2 H2B 110.9 . . ?
C1 C2 F1 104.5(9) . . ?
H2A C2 H2B 108.9 . . ?
F1 C2 H2A 110.9 . . ?
F1 C2 H2B 110.9 . . ?
C1 C2A H2AA 109.3 . . ?
C1 C2A H2AB 109.3 . . ?
C1 C2A F1A 111.7(8) . . ?
H2AA C2A H2AB 107.9 . . ?
F1A C2A H2AA 109.3 . . ?
F1A C2A H2AB 109.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S4 C16 S2 -179.60(12) . . . . ?
Ni1 S4 C16 C17 1.6(2) . . . . ?
Ni1 S6 C18 S8 178.05(12) . . . . ?
Ni1 S6 C18 C19 -1.0(2) . . . . ?
Ni1 S5 C17 S3 -178.54(13) . . . . ?
Ni1 S5 C17 C16 0.6(2) . . . . ?
Ni1 S7 C19 S9 178.64(13) . . . . ?
Ni1 S7 C19 C18 -0.7(2) . . . . ?
S2 C16 C17 S5 179.54(12) . . . . ?
S2 C16 C17 S3 -1.3(3) . . . . ?
S4 C16 C17 S5 -1.6(3) . . . . ?
S4 C16 C17 S3 177.61(12) . . . . ?
S6 C18 C19 S9 -178.21(12) . . . . ?
S6 C18 C19 S7 1.2(3) . . . . ?
S8 C18 C19 S9 2.7(3) . . . . ?
S8 C18 C19 S7 -177.89(13) . . . . ?
O2 C5 C6 O3 63.8(3) . . . . ?
O3 C7 C8 O4 -69.1(3) . . . . ?
N1 C1 C2 F1 70.2(9) . . . . ?
N1 C1 C2A F1A -58.7(11) . . . . ?
O5 C11 C12 O6 -64.6(3) . . . . ?
O1 C3 C4 O2 -64.4(3) . . . . ?
O6 C13 C14 O1 64.4(3) . . . . ?
O4 C9 C10 O5 61.9(3) . . . . ?
C16 S2 C15 S3 -2.74(16) . . . . ?
C16 S2 C15 S1 178.23(17) . . . . ?
C18 S8 C20 S9 -0.97(15) . . . . ?
C18 S8 C20 S10 -179.31(16) . . . . ?
C19 S9 C20 S8 2.13(15) . . . . ?
C19 S9 C20 S10 -179.50(16) . . . . ?
C17 S3 C15 S2 2.20(16) . . . . ?
C17 S3 C15 S1 -178.78(17) . . . . ?
C20 S8 C18 S6 179.90(15) . . . . ?
C20 S8 C18 C19 -1.1(2) . . . . ?
C20 S9 C19 S7 177.68(15) . . . . ?
C20 S9 C19 C18 -3.0(2) . . . . ?
C15 S2 C16 S4 -176.42(15) . . . . ?
C15 S2 C16 C17 2.4(2) . . . . ?
C15 S3 C17 S5 178.61(16) . . . . ?
C15 S3 C17 C16 -0.6(2) . . . . ?
C5 O2 C4 C3 -177.2(2) . . . . ?
C7 O3 C6 C5 172.8(2) . . . . ?
C6 O3 C7 C8 -179.3(2) . . . . ?
C3 O1 C14 C13 174.7(2) . . . . ?
C4 O2 C5 C6 -178.8(2) . . . . ?
C11 O5 C10 C9 169.5(2) . . . . ?
C8 O4 C9 C10 -171.3(2) . . . . ?
C13 O6 C12 C11 -175.5(2) . . . . ?
C12 O6 C13 C14 -176.4(2) . . . . ?
C14 O1 C3 C4 -176.6(2) . . . . ?
C9 O4 C8 C7 -171.1(2) . . . . ?
C10 O5 C11 C12 -179.9(3) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.098
_oxdiff_exptl_absorpt_empirical_full_min 0.693
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_333k
_database_code_depnum_ccdc_archive 'CCDC 2053294'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-19 downloaded from the CCDC.
;
_audit_creation_date             2020-11-11
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C12 H24 O6, C2 H7 F N'
_chemical_formula_sum            'C20 H31 F N Ni O6 S10'
_chemical_formula_weight         779.77
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHNOFNiS
_chemical_oxdiff_usercomment     20_20200608
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.5475(3)
_cell_length_b                   12.6632(3)
_cell_length_c                   13.0124(4)
_cell_angle_alpha                72.091(3)
_cell_angle_beta                 79.842(3)
_cell_angle_gamma                81.154(2)
_cell_volume                     1618.65(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9333
_cell_measurement_temperature    333
_cell_measurement_theta_max      28.0200
_cell_measurement_theta_min      1.9690
_shelx_estimated_absorpt_T_max   0.893
_shelx_estimated_absorpt_T_min   0.562
_exptl_absorpt_coefficient_mu    1.286
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             806
_exptl_crystal_size_max          0.507
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.857
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19117
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.857
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.906
_diffrn_reflns_theta_min         1.973
_diffrn_ambient_temperature      333
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.857
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -22.00  81.00   0.50    0.73    --   21.69  70.00-138.00  206
  2  ω     49.00  92.00   0.50    0.73    --   21.69 178.00  90.00   86
  3  ω     60.00 102.00   0.50    0.73    --   21.69 178.00 120.00   84
  4  ω    -51.00  51.00   0.50    0.73    --   21.69 -70.00  89.00  204
  5  ω    -71.00  -3.00   0.50    0.73    --  -21.62 -70.00  89.00  136
  6  ω      6.00  35.00   0.50    0.73    --  -21.62 -99.00  90.00   58
  7  ω      9.00  35.00   0.50    0.73    --  -21.62 -99.00-150.00   52
  8  ω     15.00  61.00   0.50    0.73    --  -21.62  57.00 -30.00   92
  9  ω    -35.00  59.00   0.50    0.73    --  -21.62  37.00   0.00  188
 10  ω    -46.00 -10.00   0.50    0.73    --  -21.62  57.00 -30.00   72
 11  ω    -36.00  61.00   0.50    0.73    --  -21.62  70.00-138.00  194
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0353241000
_diffrn_orient_matrix_UB_12      0.0004338000
_diffrn_orient_matrix_UB_13      -0.0417621000
_diffrn_orient_matrix_UB_21      -0.0503409000
_diffrn_orient_matrix_UB_22      0.0366016000
_diffrn_orient_matrix_UB_23      0.0185733000
_diffrn_orient_matrix_UB_31      0.0306400000
_diffrn_orient_matrix_UB_32      0.0465272000
_diffrn_orient_matrix_UB_33      -0.0354341000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5151
_reflns_number_total             7320
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         7320
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0383
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0478P)²+0.1865P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1077
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
2. Rigid body (RIGU) restrains
 C13, O6, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, C14, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(H1AA)=Sof(H1AB)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(F1)=1-FVAR(1)
 Sof(H1BC)=Sof(H1BD)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(F1A)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C7(H7A,H7B), C6(H6A,H6B), C3(H3A,H3B), C4(H4A,H4B), C11(H11A,
 H11B), C8(H8A,H8B), C13(H13A,H13B), C12(H12A,H12B), C14(H14A,H14B), C1(H1BC,
 H1BD), C1(H1AA,H1AB), C9(H9A,H9B), C10(H10A,H10B), C2(H2A,H2B), C2A(H2AA,H2AB)
4.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.16338(3) 0.40455(2) 0.49230(2) 0.04868(10) Uani 1 1 d . . . . .
S2 S -0.07852(7) 0.26657(5) 0.29638(5) 0.05604(17) Uani 1 1 d . . . . .
S4 S 0.00693(7) 0.31486(5) 0.48650(5) 0.05502(17) Uani 1 1 d . . . . .
S6 S 0.10043(7) 0.36929(5) 0.66592(5) 0.05857(18) Uani 1 1 d . . . . .
S5 S 0.22929(7) 0.43854(6) 0.31906(5) 0.05867(18) Uani 1 1 d . . . . .
S8 S 0.19612(8) 0.43748(5) 0.84027(5) 0.06111(18) Uani 1 1 d . . . . .
S3 S 0.12899(7) 0.37483(6) 0.14391(5) 0.06477(19) Uani 1 1 d . . . . .
S9 S 0.40158(7) 0.54856(6) 0.68715(6) 0.06457(19) Uani 1 1 d . . . . .
S7 S 0.31668(7) 0.49744(6) 0.49769(5) 0.06225(19) Uani 1 1 d . . . . .
S10 S 0.37490(9) 0.54743(7) 0.91747(6) 0.0812(2) Uani 1 1 d . . . . .
S1 S -0.04805(9) 0.26347(8) 0.06606(7) 0.0830(3) Uani 1 1 d . . . . .
O2 O 0.16967(19) 0.89590(16) 0.28240(16) 0.0717(5) Uani 1 1 d . . . . .
O3 O 0.2678(2) 1.06411(16) 0.32938(16) 0.0722(5) Uani 1 1 d . . . . .
N1 N 0.4479(2) 0.88943(15) 0.25497(15) 0.0513(5) Uani 1 1 d . . . . .
H1A H 0.362524 0.894517 0.256628 0.062 Uiso 1 1 calc R U . . .
H1B H 0.486966 0.890267 0.188300 0.062 Uiso 1 1 calc R U . . .
H1C H 0.468049 0.946942 0.272335 0.062 Uiso 1 1 calc R U . . .
O5 O 0.6860(2) 0.98174(18) 0.14252(18) 0.0810(6) Uani 1 1 d . . . . .
O1 O 0.3199(2) 0.80721(15) 0.12205(16) 0.0766(6) Uani 1 1 d . . . . .
O6 O 0.5898(2) 0.81910(18) 0.07851(16) 0.0828(6) Uani 1 1 d . . . . .
O4 O 0.5385(2) 1.07361(16) 0.29850(17) 0.0779(6) Uani 1 1 d . . . . .
C16 C 0.0236(2) 0.32470(19) 0.35058(19) 0.0494(5) Uani 1 1 d . . . . .
C18 C 0.2048(3) 0.43518(19) 0.70588(19) 0.0508(6) Uani 1 1 d . . . . .
C19 C 0.2996(2) 0.4891(2) 0.6337(2) 0.0528(6) Uani 1 1 d . . . . .
C17 C 0.1208(2) 0.37664(19) 0.27864(19) 0.0511(6) Uani 1 1 d . . . . .
C20 C 0.3252(3) 0.5134(2) 0.8203(2) 0.0574(6) Uani 1 1 d . . . . .
C15 C -0.0007(3) 0.2998(2) 0.1632(2) 0.0599(6) Uani 1 1 d . . . . .
C5 C 0.0900(3) 0.9814(3) 0.3195(3) 0.0797(9) Uani 1 1 d . . . . .
H5A H 0.009015 0.953926 0.359056 0.096 Uiso 1 1 calc R U . . .
H5B H 0.070309 1.044382 0.257626 0.096 Uiso 1 1 calc R U . . .
C7 C 0.3315(4) 1.1143(3) 0.3876(3) 0.0803(9) Uani 1 1 d . . . . .
H7A H 0.357564 1.058860 0.452570 0.096 Uiso 1 1 calc R U . . .
H7B H 0.273030 1.172838 0.409736 0.096 Uiso 1 1 calc R U . . .
C6 C 0.1565(3) 1.0172(3) 0.3910(3) 0.0833(9) Uani 1 1 d . . . . .
H6A H 0.099813 1.071768 0.420715 0.100 Uiso 1 1 calc R U . . .
H6B H 0.180240 0.953717 0.451145 0.100 Uiso 1 1 calc R U . . .
C3 C 0.2009(3) 0.7659(3) 0.1823(3) 0.0853(10) Uani 1 1 d . . . . .
H3A H 0.218599 0.706327 0.247412 0.102 Uiso 1 1 calc R U . . .
H3B H 0.159041 0.736255 0.138036 0.102 Uiso 1 1 calc R U . . .
C4 C 0.1156(3) 0.8586(3) 0.2124(3) 0.0804(9) Uani 1 1 d . . . . .
H4A H 0.102199 0.919450 0.147218 0.096 Uiso 1 1 calc R U . . .
H4B H 0.032009 0.833603 0.247454 0.096 Uiso 1 1 calc R U . . .
C11 C 0.7679(3) 0.9043(3) 0.0921(3) 0.1000(12) Uani 1 1 d . . . . .
H11A H 0.794484 0.837414 0.147611 0.120 Uiso 1 1 calc R U . . .
H11B H 0.844943 0.937720 0.050738 0.120 Uiso 1 1 calc R U . . .
C8 C 0.4464(4) 1.1615(3) 0.3160(3) 0.0840(10) Uani 1 1 d . . . . .
H8A H 0.421817 1.209296 0.246904 0.101 Uiso 1 1 calc R U . . .
H8B H 0.483035 1.206059 0.349754 0.101 Uiso 1 1 calc R U . . .
C13 C 0.5191(4) 0.7795(3) 0.0148(3) 0.0945(12) Uani 1 1 d . . . . .
H13A H 0.574786 0.724680 -0.015368 0.113 Uiso 1 1 calc R U . . .
H13B H 0.491404 0.841181 -0.045232 0.113 Uiso 1 1 calc R U . . .
C12 C 0.6950(4) 0.8753(3) 0.0185(3) 0.0993(12) Uani 1 1 d . . . . .
H12A H 0.664539 0.942799 -0.034461 0.119 Uiso 1 1 calc R U . . .
H12B H 0.751833 0.828378 -0.020697 0.119 Uiso 1 1 calc R U . . .
C14 C 0.4049(4) 0.7286(3) 0.0845(3) 0.0979(12) Uani 1 1 d . . . . .
H14A H 0.361404 0.696796 0.043023 0.117 Uiso 1 1 calc R U . . .
H14B H 0.432722 0.668749 0.145932 0.117 Uiso 1 1 calc R U . . .
C1 C 0.4916(4) 0.7839(3) 0.3343(3) 0.0883(10) Uani 1 1 d . . . . .
H1BC H 0.428509 0.731595 0.346203 0.106 Uiso 0.614(15) 1 calc R U P A 2
H1BD H 0.572702 0.752836 0.301424 0.106 Uiso 0.614(15) 1 calc R U P A 2
H1AA H 0.492725 0.722977 0.303510 0.106 Uiso 0.386(15) 1 calc R U P A 1
H1AB H 0.579757 0.787229 0.344085 0.106 Uiso 0.386(15) 1 calc R U P A 1
C9 C 0.6590(4) 1.1103(3) 0.2442(3) 0.0940(11) Uani 1 1 d . . . . .
H9A H 0.699332 1.137521 0.291188 0.113 Uiso 1 1 calc R U . . .
H9B H 0.645994 1.171086 0.178802 0.113 Uiso 1 1 calc R U . . .
C10 C 0.7449(3) 1.0159(3) 0.2146(3) 0.1009(12) Uani 1 1 d . . . . .
H10A H 0.829103 1.039739 0.179749 0.121 Uiso 1 1 calc R U . . .
H10B H 0.756892 0.954393 0.279554 0.121 Uiso 1 1 calc R U . . .
C2 C 0.5094(13) 0.7907(8) 0.4347(5) 0.101(4) Uani 0.614(15) 1 d . . P A 2
H2A H 0.560540 0.850940 0.426589 0.122 Uiso 0.614(15) 1 calc R U P A 2
H2B H 0.552065 0.721242 0.476465 0.122 Uiso 0.614(15) 1 calc R U P A 2
C2A C 0.4187(18) 0.7607(8) 0.4325(8) 0.077(4) Uani 0.386(15) 1 d . . P A 1
H2AA H 0.456050 0.691456 0.478915 0.093 Uiso 0.386(15) 1 calc R U P A 1
H2AB H 0.332656 0.749458 0.424038 0.093 Uiso 0.386(15) 1 calc R U P A 1
F1A F 0.4083(15) 0.8439(10) 0.4834(7) 0.120(4) Uani 0.614(15) 1 d . . P A 1
F1 F 0.371(2) 0.814(2) 0.4894(14) 0.136(7) Uani 0.386(15) 1 d . . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S4 2.1660(7) . ?
Ni1 S6 2.1647(7) . ?
Ni1 S5 2.1663(7) . ?
Ni1 S7 2.1631(7) . ?
S2 C16 1.741(2) . ?
S2 C15 1.735(3) . ?
S4 C16 1.713(2) . ?
S6 C18 1.712(2) . ?
S5 C17 1.716(2) . ?
S8 C18 1.744(2) . ?
S8 C20 1.723(3) . ?
S3 C17 1.747(2) . ?
S3 C15 1.723(3) . ?
S9 C19 1.744(2) . ?
S9 C20 1.730(3) . ?
S7 C19 1.719(3) . ?
S10 C20 1.643(2) . ?
S1 C15 1.647(3) . ?
O2 C5 1.418(3) . ?
O2 C4 1.381(3) . ?
O3 C7 1.427(3) . ?
O3 C6 1.401(4) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.481(3) . ?
O5 C11 1.440(4) . ?
O5 C10 1.410(4) . ?
O1 C3 1.437(4) . ?
O1 C14 1.381(4) . ?
O6 C13 1.444(4) . ?
O6 C12 1.394(4) . ?
O4 C8 1.407(4) . ?
O4 C9 1.412(4) . ?
C16 C17 1.360(3) . ?
C18 C19 1.354(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.467(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.475(5) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.475(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.485(5) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.477(5) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C1 H1BC 0.9700 . ?
C1 H1BD 0.9700 . ?
C1 H1AA 0.9700 . ?
C1 H1AB 0.9700 . ?
C1 C2 1.383(9) . ?
C1 C2A 1.342(13) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.491(5) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 F1 1.53(2) . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?
C2A F1A 1.390(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S4 Ni1 S5 93.33(3) . . ?
S6 Ni1 S4 87.14(3) . . ?
S6 Ni1 S5 179.12(3) . . ?
S7 Ni1 S4 178.73(3) . . ?
S7 Ni1 S6 92.79(3) . . ?
S7 Ni1 S5 86.76(3) . . ?
C15 S2 C16 97.47(12) . . ?
C16 S4 Ni1 101.92(8) . . ?
C18 S6 Ni1 102.41(8) . . ?
C17 S5 Ni1 101.75(8) . . ?
C20 S8 C18 97.26(12) . . ?
C15 S3 C17 97.47(12) . . ?
C20 S9 C19 97.09(12) . . ?
C19 S7 Ni1 102.29(9) . . ?
C4 O2 C5 113.9(2) . . ?
C6 O3 C7 112.9(2) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
C10 O5 C11 114.4(3) . . ?
C14 O1 C3 113.7(3) . . ?
C12 O6 C13 114.2(3) . . ?
C8 O4 C9 112.7(3) . . ?
S4 C16 S2 122.73(15) . . ?
C17 C16 S2 115.87(18) . . ?
C17 C16 S4 121.38(19) . . ?
S6 C18 S8 122.64(15) . . ?
C19 C18 S6 121.30(18) . . ?
C19 C18 S8 116.06(19) . . ?
S7 C19 S9 122.73(15) . . ?
C18 C19 S9 116.08(19) . . ?
C18 C19 S7 121.19(19) . . ?
S5 C17 S3 122.40(15) . . ?
C16 C17 S5 121.59(18) . . ?
C16 C17 S3 116.00(18) . . ?
S8 C20 S9 113.46(14) . . ?
S10 C20 S8 124.08(16) . . ?
S10 C20 S9 122.44(17) . . ?
S3 C15 S2 113.13(14) . . ?
S1 C15 S2 122.80(16) . . ?
S1 C15 S3 124.07(16) . . ?
O2 C5 H5A 109.7 . . ?
O2 C5 H5B 109.7 . . ?
O2 C5 C6 109.9(3) . . ?
H5A C5 H5B 108.2 . . ?
C6 C5 H5A 109.7 . . ?
C6 C5 H5B 109.7 . . ?
O3 C7 H7A 109.9 . . ?
O3 C7 H7B 109.9 . . ?
O3 C7 C8 108.8(2) . . ?
H7A C7 H7B 108.3 . . ?
C8 C7 H7A 109.9 . . ?
C8 C7 H7B 109.9 . . ?
O3 C6 C5 108.3(3) . . ?
O3 C6 H6A 110.0 . . ?
O3 C6 H6B 110.0 . . ?
C5 C6 H6A 110.0 . . ?
C5 C6 H6B 110.0 . . ?
H6A C6 H6B 108.4 . . ?
O1 C3 H3A 110.0 . . ?
O1 C3 H3B 110.0 . . ?
O1 C3 C4 108.6(2) . . ?
H3A C3 H3B 108.4 . . ?
C4 C3 H3A 110.0 . . ?
C4 C3 H3B 110.0 . . ?
O2 C4 C3 110.6(3) . . ?
O2 C4 H4A 109.5 . . ?
O2 C4 H4B 109.5 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
O5 C11 H11A 109.9 . . ?
O5 C11 H11B 109.9 . . ?
O5 C11 C12 109.1(3) . . ?
H11A C11 H11B 108.3 . . ?
C12 C11 H11A 109.9 . . ?
C12 C11 H11B 109.9 . . ?
O4 C8 C7 109.0(3) . . ?
O4 C8 H8A 109.9 . . ?
O4 C8 H8B 109.9 . . ?
C7 C8 H8A 109.9 . . ?
C7 C8 H8B 109.9 . . ?
H8A C8 H8B 108.3 . . ?
O6 C13 H13A 109.7 . . ?
O6 C13 H13B 109.7 . . ?
O6 C13 C14 109.7(3) . . ?
H13A C13 H13B 108.2 . . ?
C14 C13 H13A 109.7 . . ?
C14 C13 H13B 109.7 . . ?
O6 C12 C11 110.2(3) . . ?
O6 C12 H12A 109.6 . . ?
O6 C12 H12B 109.6 . . ?
C11 C12 H12A 109.6 . . ?
C11 C12 H12B 109.6 . . ?
H12A C12 H12B 108.1 . . ?
O1 C14 C13 110.7(3) . . ?
O1 C14 H14A 109.5 . . ?
O1 C14 H14B 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 108.1 . . ?
N1 C1 H1BC 108.1 . . ?
N1 C1 H1BD 108.1 . . ?
N1 C1 H1AA 108.5 . . ?
N1 C1 H1AB 108.5 . . ?
H1BC C1 H1BD 107.3 . . ?
H1AA C1 H1AB 107.5 . . ?
C2 C1 N1 116.7(4) . . ?
C2 C1 H1BC 108.1 . . ?
C2 C1 H1BD 108.1 . . ?
C2A C1 N1 115.0(6) . . ?
C2A C1 H1AA 108.5 . . ?
C2A C1 H1AB 108.5 . . ?
O4 C9 H9A 109.8 . . ?
O4 C9 H9B 109.8 . . ?
O4 C9 C10 109.6(3) . . ?
H9A C9 H9B 108.2 . . ?
C10 C9 H9A 109.8 . . ?
C10 C9 H9B 109.8 . . ?
O5 C10 C9 108.2(3) . . ?
O5 C10 H10A 110.1 . . ?
O5 C10 H10B 110.1 . . ?
C9 C10 H10A 110.1 . . ?
C9 C10 H10B 110.1 . . ?
H10A C10 H10B 108.4 . . ?
C1 C2 H2A 111.1 . . ?
C1 C2 H2B 111.1 . . ?
C1 C2 F1 103.4(10) . . ?
H2A C2 H2B 109.0 . . ?
F1 C2 H2A 111.1 . . ?
F1 C2 H2B 111.1 . . ?
C1 C2A H2AA 108.9 . . ?
C1 C2A H2AB 108.9 . . ?
C1 C2A F1A 113.4(10) . . ?
H2AA C2A H2AB 107.7 . . ?
F1A C2A H2AA 108.9 . . ?
F1A C2A H2AB 108.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S4 C16 S2 -179.88(13) . . . . ?
Ni1 S4 C16 C17 1.8(2) . . . . ?
Ni1 S6 C18 S8 178.32(13) . . . . ?
Ni1 S6 C18 C19 -1.6(2) . . . . ?
Ni1 S5 C17 S3 -178.52(13) . . . . ?
Ni1 S5 C17 C16 0.7(2) . . . . ?
Ni1 S7 C19 S9 178.87(13) . . . . ?
Ni1 S7 C19 C18 -1.1(2) . . . . ?
S2 C16 C17 S5 179.77(13) . . . . ?
S2 C16 C17 S3 -1.0(3) . . . . ?
S4 C16 C17 S5 -1.8(3) . . . . ?
S4 C16 C17 S3 177.45(13) . . . . ?
S6 C18 C19 S9 -178.06(13) . . . . ?
S6 C18 C19 S7 1.9(3) . . . . ?
S8 C18 C19 S9 2.0(3) . . . . ?
S8 C18 C19 S7 -177.99(14) . . . . ?
O2 C5 C6 O3 63.8(3) . . . . ?
O3 C7 C8 O4 -68.5(3) . . . . ?
N1 C1 C2 F1 70.8(11) . . . . ?
N1 C1 C2A F1A -57.2(15) . . . . ?
O5 C11 C12 O6 -64.3(4) . . . . ?
O1 C3 C4 O2 -64.3(3) . . . . ?
O6 C13 C14 O1 63.6(4) . . . . ?
O4 C9 C10 O5 61.9(4) . . . . ?
C16 S2 C15 S3 -2.39(17) . . . . ?
C16 S2 C15 S1 178.10(18) . . . . ?
C18 S8 C20 S9 -1.05(16) . . . . ?
C18 S8 C20 S10 -179.55(17) . . . . ?
C19 S9 C20 S8 1.92(17) . . . . ?
C19 S9 C20 S10 -179.56(17) . . . . ?
C17 S3 C15 S2 1.98(17) . . . . ?
C17 S3 C15 S1 -178.52(19) . . . . ?
C20 S8 C18 S6 179.52(16) . . . . ?
C20 S8 C18 C19 -0.6(2) . . . . ?
C20 S9 C19 S7 177.63(16) . . . . ?
C20 S9 C19 C18 -2.4(2) . . . . ?
C15 S2 C16 S4 -176.34(16) . . . . ?
C15 S2 C16 C17 2.0(2) . . . . ?
C15 S3 C17 S5 178.62(16) . . . . ?
C15 S3 C17 C16 -0.6(2) . . . . ?
C5 O2 C4 C3 -176.9(2) . . . . ?
C7 O3 C6 C5 172.7(2) . . . . ?
C6 O3 C7 C8 -179.7(2) . . . . ?
C3 O1 C14 C13 174.6(3) . . . . ?
C4 O2 C5 C6 -178.7(3) . . . . ?
C11 O5 C10 C9 169.8(3) . . . . ?
C8 O4 C9 C10 -172.0(3) . . . . ?
C13 O6 C12 C11 -175.3(3) . . . . ?
C12 O6 C13 C14 -176.0(3) . . . . ?
C14 O1 C3 C4 -176.8(3) . . . . ?
C9 O4 C8 C7 -171.2(3) . . . . ?
C10 O5 C11 C12 -179.9(3) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.207
_oxdiff_exptl_absorpt_empirical_full_min 0.589
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_353k
_database_code_depnum_ccdc_archive 'CCDC 2053295'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-19 downloaded from the CCDC.
;
_audit_creation_date             2020-11-11
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C12 H24 O6, C2 H7 F N'
_chemical_formula_sum            'C20 H31 F N Ni O6 S10'
_chemical_formula_weight         779.77
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHNOFNiS
_chemical_oxdiff_usercomment     20_20200608
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.5673(4)
_cell_length_b                   12.6724(4)
_cell_length_c                   13.0358(6)
_cell_angle_alpha                72.219(4)
_cell_angle_beta                 79.801(4)
_cell_angle_gamma                81.293(3)
_cell_volume                     1627.17(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8566
_cell_measurement_temperature    353
_cell_measurement_theta_max      27.9830
_cell_measurement_theta_min      1.7880
_shelx_estimated_absorpt_T_max   0.894
_shelx_estimated_absorpt_T_min   0.563
_exptl_absorpt_coefficient_mu    1.279
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35053
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             806
_exptl_crystal_size_max          0.507
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.840
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18534
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.840
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.081
_diffrn_reflns_theta_min         2.391
_diffrn_ambient_temperature      353
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.840
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     48.00 102.00   0.50    0.76    --   21.85 178.00 120.00  108
  2  ω     67.00  93.00   0.50    0.76    --   21.85 178.00  90.00   52
  3  ω      8.00  57.00   0.50    0.76    --   21.85  72.00-138.00   98
  4  ω    -72.00  23.00   0.50    0.76    --  -21.77 -72.00  91.00  190
  5  ω    -40.00  59.00   0.50    0.76    --  -21.77  37.00   0.00  198
  6  ω    -44.00  59.00   0.50    0.76    --  -21.77  72.00-138.00  206
  7  ω     -7.00  37.00   0.50    0.76    --  -21.77 -99.00-180.00   88
  8  ω     -1.00  24.00   0.50    0.76    --  -21.77 -99.00-150.00   50
  9  ω    -66.00 -38.00   0.50    0.76    --   21.85 -19.00 -60.00   56
 10  ω    -72.00  63.00   0.50    0.76    --   21.85 -72.00  91.00  270
 11  ω    -29.00  26.00   0.50    0.76    --   21.85 -19.00 -60.00  110
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0341380000
_diffrn_orient_matrix_UB_12      0.0023686000
_diffrn_orient_matrix_UB_13      -0.0429880000
_diffrn_orient_matrix_UB_21      -0.0500207000
_diffrn_orient_matrix_UB_22      0.0365955000
_diffrn_orient_matrix_UB_23      0.0187024000
_diffrn_orient_matrix_UB_31      0.0321623000
_diffrn_orient_matrix_UB_32      0.0463454000
_diffrn_orient_matrix_UB_33      -0.0336404000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4815
_reflns_number_total             7331
_reflns_odcompleteness_completeness 99.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.911
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         7331
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0459
_refine_ls_restrained_S_all      0.911
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1373
_refine_ls_wR_factor_ref         0.1559
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
2. Rigid body (RIGU) restrains
 O1, C3, C4, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(H1AA)=Sof(H1AB)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(F1)=1-FVAR(1)
 Sof(H1BC)=Sof(H1BD)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(F1A)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C7(H7A,H7B), C6(H6A,H6B), C3(H3A,H3B), C4(H4A,H4B), C11(H11A,
 H11B), C8(H8A,H8B), C13(H13A,H13B), C12(H12A,H12B), C14(H14A,H14B), C1(H1BC,
 H1BD), C1(H1AA,H1AB), C9(H9A,H9B), C10(H10A,H10B), C2(H2A,H2B), C2A(H2AA,H2AB)
4.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.16351(3) 0.40468(3) 0.49223(3) 0.05417(14) Uani 1 1 d . . . . .
S2 S -0.07792(8) 0.26641(7) 0.29624(7) 0.0625(2) Uani 1 1 d . . . . .
S4 S 0.00716(8) 0.31487(6) 0.48615(6) 0.0612(2) Uani 1 1 d . . . . .
S6 S 0.10079(8) 0.36942(7) 0.66557(6) 0.0648(2) Uani 1 1 d . . . . .
S5 S 0.22941(8) 0.43853(7) 0.31948(6) 0.0645(2) Uani 1 1 d . . . . .
S8 S 0.19638(9) 0.43768(7) 0.83979(6) 0.0674(2) Uani 1 1 d . . . . .
S3 S 0.12918(8) 0.37484(8) 0.14430(7) 0.0712(2) Uani 1 1 d . . . . .
S9 S 0.40154(8) 0.54871(8) 0.68724(7) 0.0710(2) Uani 1 1 d . . . . .
S7 S 0.31689(8) 0.49758(7) 0.49784(7) 0.0682(2) Uani 1 1 d . . . . .
S10 S 0.37476(11) 0.54777(9) 0.91704(8) 0.0895(3) Uani 1 1 d . . . . .
S1 S -0.04744(11) 0.26339(10) 0.06637(8) 0.0920(3) Uani 1 1 d . . . . .
O2 O 0.1705(2) 0.89516(19) 0.2816(2) 0.0820(6) Uani 1 1 d . . . . .
O3 O 0.2679(2) 1.06388(19) 0.3291(2) 0.0813(7) Uani 1 1 d . . . . .
N1 N 0.4474(2) 0.88855(18) 0.25506(18) 0.0570(6) Uani 1 1 d . . . . .
H1A H 0.396116 0.873859 0.214952 0.068 Uiso 1 1 calc R U . . .
H1B H 0.515601 0.919052 0.212029 0.068 Uiso 1 1 calc R U . . .
H1C H 0.403980 0.935699 0.290539 0.068 Uiso 1 1 calc R U . . .
O5 O 0.6858(2) 0.9823(2) 0.1428(2) 0.0930(8) Uani 1 1 d . . . . .
O1 O 0.3209(3) 0.80689(19) 0.1217(2) 0.0864(7) Uani 1 1 d . . . . .
O6 O 0.5898(3) 0.8190(2) 0.0789(2) 0.0929(8) Uani 1 1 d . . . . .
O4 O 0.5375(3) 1.07355(19) 0.2988(2) 0.0869(7) Uani 1 1 d . . . . .
C16 C 0.0243(3) 0.3250(2) 0.3504(2) 0.0555(7) Uani 1 1 d . . . . .
C18 C 0.2049(3) 0.4353(2) 0.7058(2) 0.0549(7) Uani 1 1 d . . . . .
C19 C 0.3001(3) 0.4892(2) 0.6336(3) 0.0587(7) Uani 1 1 d . . . . .
C17 C 0.1207(3) 0.3767(2) 0.2792(2) 0.0567(7) Uani 1 1 d . . . . .
C20 C 0.3251(3) 0.5139(2) 0.8198(3) 0.0632(7) Uani 1 1 d . . . . .
C15 C -0.0001(3) 0.2996(3) 0.1633(3) 0.0663(8) Uani 1 1 d . . . . .
C5 C 0.0898(4) 0.9806(3) 0.3188(4) 0.0909(11) Uani 1 1 d . . . . .
H5A H 0.009343 0.952635 0.358686 0.109 Uiso 1 1 calc R U . . .
H5B H 0.069674 1.043192 0.257141 0.109 Uiso 1 1 calc R U . . .
C7 C 0.3323(4) 1.1146(3) 0.3866(3) 0.0920(12) Uani 1 1 d . . . . .
H7A H 0.358606 1.059514 0.451240 0.110 Uiso 1 1 calc R U . . .
H7B H 0.274011 1.172979 0.408912 0.110 Uiso 1 1 calc R U . . .
C6 C 0.1564(4) 1.0171(4) 0.3896(4) 0.0945(12) Uani 1 1 d . . . . .
H6A H 0.099726 1.071742 0.419025 0.113 Uiso 1 1 calc R U . . .
H6B H 0.179578 0.954006 0.449869 0.113 Uiso 1 1 calc R U . . .
C3 C 0.2013(4) 0.7657(3) 0.1821(3) 0.0950(12) Uani 1 1 d . . . . .
H3A H 0.218722 0.706673 0.247233 0.114 Uiso 1 1 calc R U . . .
H3B H 0.159906 0.735557 0.138050 0.114 Uiso 1 1 calc R U . . .
C4 C 0.1156(4) 0.8579(3) 0.2118(4) 0.0933(11) Uani 1 1 d . . . . .
H4A H 0.102071 0.918478 0.146785 0.112 Uiso 1 1 calc R U . . .
H4B H 0.032281 0.832590 0.247037 0.112 Uiso 1 1 calc R U . . .
C11 C 0.7686(4) 0.9054(4) 0.0922(4) 0.1137(16) Uani 1 1 d . . . . .
H11A H 0.796649 0.839141 0.147389 0.136 Uiso 1 1 calc R U . . .
H11B H 0.844566 0.939683 0.049773 0.136 Uiso 1 1 calc R U . . .
C8 C 0.4455(5) 1.1617(3) 0.3156(4) 0.0950(13) Uani 1 1 d . . . . .
H8A H 0.421102 1.208826 0.246598 0.114 Uiso 1 1 calc R U . . .
H8B H 0.481939 1.206686 0.349045 0.114 Uiso 1 1 calc R U . . .
C13 C 0.5172(5) 0.7783(4) 0.0162(4) 0.1047(15) Uani 1 1 d . . . . .
H13A H 0.572328 0.723695 -0.014288 0.126 Uiso 1 1 calc R U . . .
H13B H 0.488844 0.839679 -0.043429 0.126 Uiso 1 1 calc R U . . .
C12 C 0.6933(5) 0.8748(4) 0.0197(4) 0.1136(16) Uani 1 1 d . . . . .
H12A H 0.662424 0.941904 -0.033000 0.136 Uiso 1 1 calc R U . . .
H12B H 0.749650 0.828038 -0.019757 0.136 Uiso 1 1 calc R U . . .
C14 C 0.4048(6) 0.7276(4) 0.0859(4) 0.1092(15) Uani 1 1 d . . . . .
H14A H 0.361366 0.694768 0.045367 0.131 Uiso 1 1 calc R U . . .
H14B H 0.432707 0.668953 0.147672 0.131 Uiso 1 1 calc R U . . .
C1 C 0.4915(5) 0.7839(3) 0.3343(3) 0.0959(13) Uani 1 1 d . . . . .
H1BC H 0.429619 0.730908 0.345090 0.115 Uiso 0.667(18) 1 calc R U P A 2
H1BD H 0.573139 0.753992 0.301414 0.115 Uiso 0.667(18) 1 calc R U P A 2
H1AA H 0.496620 0.722867 0.302913 0.115 Uiso 0.333(18) 1 calc R U P A 1
H1AB H 0.577854 0.789144 0.346692 0.115 Uiso 0.333(18) 1 calc R U P A 1
C9 C 0.6579(4) 1.1111(4) 0.2436(4) 0.1030(13) Uani 1 1 d . . . . .
H9A H 0.697956 1.139500 0.289808 0.124 Uiso 1 1 calc R U . . .
H9B H 0.644551 1.170902 0.177971 0.124 Uiso 1 1 calc R U . . .
C10 C 0.7447(4) 1.0158(4) 0.2148(4) 0.1109(15) Uani 1 1 d . . . . .
H10A H 0.829067 1.039166 0.180494 0.133 Uiso 1 1 calc R U . . .
H10B H 0.755648 0.954414 0.279827 0.133 Uiso 1 1 calc R U . . .
C2 C 0.5079(16) 0.7886(9) 0.4336(6) 0.129(6) Uani 0.667(18) 1 d . . P A 2
H2A H 0.558202 0.848846 0.427213 0.155 Uiso 0.667(18) 1 calc R U P A 2
H2B H 0.550482 0.718999 0.474322 0.155 Uiso 0.667(18) 1 calc R U P A 2
C2A C 0.4139(18) 0.7601(10) 0.4312(11) 0.070(4) Uani 0.333(18) 1 d . . P A 1
H2AA H 0.447277 0.689499 0.477661 0.084 Uiso 0.333(18) 1 calc R U P A 1
H2AB H 0.328052 0.752119 0.419545 0.084 Uiso 0.333(18) 1 calc R U P A 1
F1A F 0.4051(15) 0.8426(10) 0.4837(7) 0.137(4) Uani 0.667(18) 1 d . . P A 1
F1 F 0.372(2) 0.809(3) 0.487(2) 0.153(10) Uani 0.333(18) 1 d . . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S4 2.1685(8) . ?
Ni1 S6 2.1652(8) . ?
Ni1 S5 2.1645(8) . ?
Ni1 S7 2.1658(8) . ?
S2 C16 1.746(3) . ?
S2 C15 1.735(3) . ?
S4 C16 1.713(3) . ?
S6 C18 1.713(3) . ?
S5 C17 1.716(3) . ?
S8 C18 1.742(3) . ?
S8 C20 1.723(3) . ?
S3 C17 1.752(3) . ?
S3 C15 1.722(3) . ?
S9 C19 1.743(3) . ?
S9 C20 1.726(3) . ?
S7 C19 1.719(3) . ?
S10 C20 1.645(3) . ?
S1 C15 1.645(3) . ?
O2 C5 1.425(4) . ?
O2 C4 1.386(4) . ?
O3 C7 1.430(4) . ?
O3 C6 1.400(4) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.479(4) . ?
O5 C11 1.443(5) . ?
O5 C10 1.406(5) . ?
O1 C3 1.444(4) . ?
O1 C14 1.372(5) . ?
O6 C13 1.456(5) . ?
O6 C12 1.376(6) . ?
O4 C8 1.409(5) . ?
O4 C9 1.419(5) . ?
C16 C17 1.351(4) . ?
C18 C19 1.358(4) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.466(5) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.459(6) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.472(6) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.503(7) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.463(6) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C1 H1BC 0.9700 . ?
C1 H1BD 0.9700 . ?
C1 H1AA 0.9700 . ?
C1 H1AB 0.9700 . ?
C1 C2 1.356(11) . ?
C1 C2A 1.355(15) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.503(6) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 F1 1.50(3) . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?
C2A F1A 1.398(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S6 Ni1 S4 87.26(3) . . ?
S6 Ni1 S7 92.69(3) . . ?
S5 Ni1 S4 93.25(3) . . ?
S5 Ni1 S6 179.03(4) . . ?
S5 Ni1 S7 86.81(3) . . ?
S7 Ni1 S4 178.79(3) . . ?
C15 S2 C16 97.42(14) . . ?
C16 S4 Ni1 101.78(10) . . ?
C18 S6 Ni1 102.60(10) . . ?
C17 S5 Ni1 101.68(10) . . ?
C20 S8 C18 97.29(14) . . ?
C15 S3 C17 97.54(14) . . ?
C20 S9 C19 97.16(15) . . ?
C19 S7 Ni1 102.37(10) . . ?
C4 O2 C5 113.1(3) . . ?
C6 O3 C7 113.8(3) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
C10 O5 C11 113.7(3) . . ?
C14 O1 C3 113.2(3) . . ?
C12 O6 C13 115.1(3) . . ?
C8 O4 C9 112.3(3) . . ?
S4 C16 S2 122.47(17) . . ?
C17 C16 S2 116.0(2) . . ?
C17 C16 S4 121.5(2) . . ?
S6 C18 S8 122.84(17) . . ?
C19 C18 S6 121.1(2) . . ?
C19 C18 S8 116.0(2) . . ?
S7 C19 S9 122.88(18) . . ?
C18 C19 S9 116.0(2) . . ?
C18 C19 S7 121.2(2) . . ?
S5 C17 S3 122.29(17) . . ?
C16 C17 S5 121.8(2) . . ?
C16 C17 S3 115.9(2) . . ?
S8 C20 S9 113.53(17) . . ?
S10 C20 S8 124.0(2) . . ?
S10 C20 S9 122.46(19) . . ?
S3 C15 S2 113.03(17) . . ?
S1 C15 S2 122.77(18) . . ?
S1 C15 S3 124.19(19) . . ?
O2 C5 H5A 109.8 . . ?
O2 C5 H5B 109.8 . . ?
O2 C5 C6 109.5(3) . . ?
H5A C5 H5B 108.2 . . ?
C6 C5 H5A 109.8 . . ?
C6 C5 H5B 109.8 . . ?
O3 C7 H7A 109.9 . . ?
O3 C7 H7B 109.9 . . ?
O3 C7 C8 109.1(3) . . ?
H7A C7 H7B 108.3 . . ?
C8 C7 H7A 109.9 . . ?
C8 C7 H7B 109.9 . . ?
O3 C6 C5 109.1(3) . . ?
O3 C6 H6A 109.9 . . ?
O3 C6 H6B 109.9 . . ?
C5 C6 H6A 109.9 . . ?
C5 C6 H6B 109.9 . . ?
H6A C6 H6B 108.3 . . ?
O1 C3 H3A 109.9 . . ?
O1 C3 H3B 109.9 . . ?
O1 C3 C4 109.1(3) . . ?
H3A C3 H3B 108.3 . . ?
C4 C3 H3A 109.9 . . ?
C4 C3 H3B 109.9 . . ?
O2 C4 C3 109.8(3) . . ?
O2 C4 H4A 109.7 . . ?
O2 C4 H4B 109.7 . . ?
C3 C4 H4A 109.7 . . ?
C3 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
O5 C11 H11A 110.1 . . ?
O5 C11 H11B 110.1 . . ?
O5 C11 C12 108.2(3) . . ?
H11A C11 H11B 108.4 . . ?
C12 C11 H11A 110.1 . . ?
C12 C11 H11B 110.1 . . ?
O4 C8 C7 108.6(3) . . ?
O4 C8 H8A 110.0 . . ?
O4 C8 H8B 110.0 . . ?
C7 C8 H8A 110.0 . . ?
C7 C8 H8B 110.0 . . ?
H8A C8 H8B 108.3 . . ?
O6 C13 H13A 109.6 . . ?
O6 C13 H13B 109.6 . . ?
O6 C13 C14 110.1(3) . . ?
H13A C13 H13B 108.1 . . ?
C14 C13 H13A 109.6 . . ?
C14 C13 H13B 109.6 . . ?
O6 C12 C11 111.3(4) . . ?
O6 C12 H12A 109.4 . . ?
O6 C12 H12B 109.4 . . ?
C11 C12 H12A 109.4 . . ?
C11 C12 H12B 109.4 . . ?
H12A C12 H12B 108.0 . . ?
O1 C14 C13 109.9(4) . . ?
O1 C14 H14A 109.7 . . ?
O1 C14 H14B 109.7 . . ?
C13 C14 H14A 109.7 . . ?
C13 C14 H14B 109.7 . . ?
H14A C14 H14B 108.2 . . ?
N1 C1 H1BC 107.8 . . ?
N1 C1 H1BD 107.8 . . ?
N1 C1 H1AA 108.8 . . ?
N1 C1 H1AB 108.8 . . ?
H1BC C1 H1BD 107.2 . . ?
H1AA C1 H1AB 107.7 . . ?
C2 C1 N1 118.0(5) . . ?
C2 C1 H1BC 107.8 . . ?
C2 C1 H1BD 107.8 . . ?
C2A C1 N1 114.0(7) . . ?
C2A C1 H1AA 108.8 . . ?
C2A C1 H1AB 108.8 . . ?
O4 C9 H9A 109.8 . . ?
O4 C9 H9B 109.8 . . ?
O4 C9 C10 109.3(3) . . ?
H9A C9 H9B 108.3 . . ?
C10 C9 H9A 109.8 . . ?
C10 C9 H9B 109.8 . . ?
O5 C10 C9 107.4(3) . . ?
O5 C10 H10A 110.2 . . ?
O5 C10 H10B 110.2 . . ?
C9 C10 H10A 110.2 . . ?
C9 C10 H10B 110.2 . . ?
H10A C10 H10B 108.5 . . ?
C1 C2 H2A 111.1 . . ?
C1 C2 H2B 111.1 . . ?
C1 C2 F1 103.1(14) . . ?
H2A C2 H2B 109.1 . . ?
F1 C2 H2A 111.1 . . ?
F1 C2 H2B 111.1 . . ?
C1 C2A H2AA 109.1 . . ?
C1 C2A H2AB 109.1 . . ?
C1 C2A F1A 112.3(10) . . ?
H2AA C2A H2AB 107.9 . . ?
F1A C2A H2AA 109.1 . . ?
F1A C2A H2AB 109.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S4 C16 S2 -179.98(15) . . . . ?
Ni1 S4 C16 C17 1.8(3) . . . . ?
Ni1 S6 C18 S8 178.33(16) . . . . ?
Ni1 S6 C18 C19 -1.8(3) . . . . ?
Ni1 S5 C17 S3 -178.47(17) . . . . ?
Ni1 S5 C17 C16 0.5(3) . . . . ?
Ni1 S7 C19 S9 179.05(16) . . . . ?
Ni1 S7 C19 C18 -1.3(3) . . . . ?
S2 C16 C17 S5 179.98(16) . . . . ?
S2 C16 C17 S3 -0.9(3) . . . . ?
S4 C16 C17 S5 -1.7(4) . . . . ?
S4 C16 C17 S3 177.38(16) . . . . ?
S6 C18 C19 S9 -178.10(16) . . . . ?
S6 C18 C19 S7 2.2(4) . . . . ?
S8 C18 C19 S9 1.8(3) . . . . ?
S8 C18 C19 S7 -177.91(17) . . . . ?
O2 C5 C6 O3 63.3(4) . . . . ?
O3 C7 C8 O4 -68.9(4) . . . . ?
N1 C1 C2 F1 70.5(15) . . . . ?
N1 C1 C2A F1A -60.7(15) . . . . ?
O5 C11 C12 O6 -63.8(5) . . . . ?
O1 C3 C4 O2 -64.1(4) . . . . ?
O6 C13 C14 O1 64.5(5) . . . . ?
O4 C9 C10 O5 62.9(4) . . . . ?
C16 S2 C15 S3 -2.4(2) . . . . ?
C16 S2 C15 S1 178.2(2) . . . . ?
C18 S8 C20 S9 -1.2(2) . . . . ?
C18 S8 C20 S10 -179.5(2) . . . . ?
C19 S9 C20 S8 2.0(2) . . . . ?
C19 S9 C20 S10 -179.7(2) . . . . ?
C17 S3 C15 S2 2.0(2) . . . . ?
C17 S3 C15 S1 -178.7(2) . . . . ?
C20 S8 C18 S6 179.56(19) . . . . ?
C20 S8 C18 C19 -0.3(3) . . . . ?
C20 S9 C19 S7 177.4(2) . . . . ?
C20 S9 C19 C18 -2.3(3) . . . . ?
C15 S2 C16 S4 -176.3(2) . . . . ?
C15 S2 C16 C17 2.0(3) . . . . ?
C15 S3 C17 S5 178.4(2) . . . . ?
C15 S3 C17 C16 -0.7(3) . . . . ?
C5 O2 C4 C3 -176.8(3) . . . . ?
C7 O3 C6 C5 172.8(3) . . . . ?
C6 O3 C7 C8 -179.3(3) . . . . ?
C3 O1 C14 C13 174.1(3) . . . . ?
C4 O2 C5 C6 -178.5(3) . . . . ?
C11 O5 C10 C9 169.2(3) . . . . ?
C8 O4 C9 C10 -172.2(3) . . . . ?
C13 O6 C12 C11 -175.4(3) . . . . ?
C12 O6 C13 C14 -176.1(3) . . . . ?
C14 O1 C3 C4 -177.0(3) . . . . ?
C9 O4 C8 C7 -171.5(3) . . . . ?
C10 O5 C11 C12 178.8(4) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 5.929
_oxdiff_exptl_absorpt_empirical_full_min 0.264
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_106k
_database_code_depnum_ccdc_archive 'CCDC 2053298'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-18 downloaded from the CCDC.
;
_audit_creation_date             2020-11-10
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C2 H7 Br1 N, C12 H24 O6'
_chemical_formula_sum            'C20 H31 Br N Ni O6 S10'
_chemical_formula_weight         840.68
_chemical_melting_point          ?
_chemical_oxdiff_formula         BrCHNONiS
_chemical_oxdiff_usercomment     223K
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.9869(3)
_cell_length_b                   12.0485(4)
_cell_length_c                   13.7559(5)
_cell_angle_alpha                115.833(4)
_cell_angle_beta                 91.587(3)
_cell_angle_gamma                100.906(3)
_cell_volume                     1596.83(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    10627
_cell_measurement_temperature    106
_cell_measurement_theta_max      30.5700
_cell_measurement_theta_min      1.9220
_shelx_estimated_absorpt_T_max   0.842
_shelx_estimated_absorpt_T_min   0.429
_exptl_absorpt_coefficient_mu    2.549
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85539
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             858
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_unetI/netI     0.0694
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.779
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19669
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.779
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.957
_diffrn_reflns_theta_min         1.895
_diffrn_ambient_temperature      106
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.779
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -11.00  39.00   0.50    0.67    --    5.18 -99.00   0.00  100
  2  ω    -17.00  26.00   0.50    0.67    --   -4.95 -99.00 150.00   86
  3  ω    -76.00   1.00   0.50    0.67    --   -4.95 -37.00  60.00  154
  4  ω    -10.00  68.00   0.50    0.67    --   -4.95  37.00   0.00  156
  5  ω     25.00  74.00   0.50    0.67    --    5.18  37.00 -90.00   98
  6  ω    -43.00  10.00   0.50    0.67    --   -4.95 -57.00-180.00  106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0310318000
_diffrn_orient_matrix_UB_12      -0.0436389000
_diffrn_orient_matrix_UB_13      -0.0378793000
_diffrn_orient_matrix_UB_21      -0.0300486000
_diffrn_orient_matrix_UB_22      0.0064051000
_diffrn_orient_matrix_UB_23      -0.0429805000
_diffrn_orient_matrix_UB_31      0.0502480000
_diffrn_orient_matrix_UB_32      0.0505765000
_diffrn_orient_matrix_UB_33      0.0071785000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5867
_reflns_number_total             7891
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT n/a (Sheldrick, 2015)'
_refine_diff_density_max         0.460
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         7891
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0356
_refine_ls_restrained_S_all      0.994
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0155P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0757
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
N1 \\sim C1A \\sim C2A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.01 within 2A
3. Others
 1*[Sof(Br1B)]+1*[Sof(Br1A)]+1*[Sof(Br1)]=1 with esd of 0.0001
 Sof(H1BD)=Sof(H1BE)=Sof(H1BF)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C1A)=Sof(H1AD)=
 Sof(H1AE)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C1)=Sof(H1A)=
 Sof(H1B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C3(H3A,H3B), C12(H12A,H12B), C8(H8A,H8B), C9(H9A,H9B),
 C33(H33A,H33B), C32(H32A,H32B), C10(H10A,H10B), C7(H7A,H7B), C4(H4A,H4B),
 C2(H2A,H2B), C6(H6A,H6B), C5(H5A,H5B), C1(H1A,H1B), C2A(H2AA,H2AB), C1A(H1AD,
 H1AE)
4.b Idealised Me refined as rotating group:
 N1(H1AA,H1AB,H1AC), N1(H1BD,H1BE,H1BF)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.13912(3) 0.14919(3) 0.11364(3) 0.01407(8) Uani 1 1 d . . . . .
Br1B Br 0.10533(3) 0.80471(3) 0.52744(3) 0.02529(13) Uani 0.9342(17) 1 d . . P
A 1
S1 S 0.10558(5) 0.33876(6) 0.17838(5) 0.01549(13) Uani 1 1 d . . . . .
S2 S 0.26828(5) 0.18041(6) 0.00725(5) 0.01748(14) Uani 1 1 d . . . . .
S3 S 0.21065(5) 0.55675(6) 0.12782(5) 0.01556(13) Uani 1 1 d . . . . .
S4 S 0.35799(5) 0.41139(6) -0.02987(5) 0.01561(13) Uani 1 1 d . . . . .
S7 S 0.16695(5) -0.04112(6) 0.04134(5) 0.01761(14) Uani 1 1 d . . . . .
S5 S 0.36464(6) 0.67560(6) 0.00815(5) 0.02007(14) Uani 1 1 d . . . . .
S9 S 0.05954(5) -0.26736(6) 0.07860(5) 0.01671(14) Uani 1 1 d . . . . .
S8 S -0.07420(6) -0.12304(6) 0.25119(6) 0.02051(15) Uani 1 1 d . . . . .
S6 S 0.01396(6) 0.11463(6) 0.22152(5) 0.01914(14) Uani 1 1 d . . . . .
S10 S -0.08302(6) -0.39320(6) 0.19788(6) 0.02263(15) Uani 1 1 d . . . . .
O6 O 0.57826(15) 0.65134(17) 0.37307(14) 0.0192(4) Uani 1 1 d . . . . .
O5 O 0.36637(15) 0.48494(16) 0.37809(14) 0.0191(4) Uani 1 1 d . . . . .
O1 O 0.64542(14) 0.89979(17) 0.53634(15) 0.0201(4) Uani 1 1 d . . . . .
O4 O 0.25652(15) 0.54176(17) 0.57149(15) 0.0217(4) Uani 1 1 d . . . . .
O2 O 0.54360(16) 0.93365(17) 0.72982(15) 0.0254(4) Uani 1 1 d . . . . .
O3 O 0.31399(15) 0.78431(18) 0.73465(15) 0.0245(4) Uani 1 1 d . . . . .
N1 N 0.39491(18) 0.7446(2) 0.52465(18) 0.0198(5) Uani 1 1 d . U . . .
H1AA H 0.391579 0.661949 0.490085 0.024 Uiso 0.949(5) 1 calc R U P B 1
H1AB H 0.350518 0.760804 0.580493 0.024 Uiso 0.949(5) 1 calc R U P B 1
H1AC H 0.473979 0.786425 0.549079 0.024 Uiso 0.949(5) 1 calc R U P B 1
H1BD H 0.344020 0.674272 0.475050 0.024 Uiso 0.051(5) 1 calc R U P B 2
H1BE H 0.387988 0.749013 0.590479 0.024 Uiso 0.051(5) 1 calc R U P B 2
H1BF H 0.473352 0.743616 0.510496 0.024 Uiso 0.051(5) 1 calc R U P B 2
C13 C 0.2013(2) 0.4031(2) 0.1104(2) 0.0136(5) Uani 1 1 d . . . . .
C15 C 0.3132(2) 0.5537(2) 0.0333(2) 0.0147(5) Uani 1 1 d . . . . .
C14 C 0.2699(2) 0.3347(2) 0.0358(2) 0.0142(5) Uani 1 1 d . . . . .
C17 C 0.0737(2) -0.1098(2) 0.1072(2) 0.0158(5) Uani 1 1 d . . . . .
C18 C -0.0355(2) -0.2678(2) 0.1771(2) 0.0170(5) Uani 1 1 d . . . . .
C11 C 0.4564(2) 0.4417(2) 0.3055(2) 0.0214(6) Uani 1 1 d . . . . .
H11A H 0.416025 0.366372 0.240338 0.026 Uiso 1 1 calc R U . . .
H11B H 0.520056 0.420273 0.340248 0.026 Uiso 1 1 calc R U . . .
C16 C 0.0092(2) -0.0411(2) 0.1868(2) 0.0166(5) Uani 1 1 d . . . . .
C3 C 0.7142(2) 0.9767(3) 0.6421(2) 0.0225(6) Uani 1 1 d . . . . .
H3A H 0.777978 1.043209 0.640171 0.027 Uiso 1 1 calc R U . . .
H3B H 0.755010 0.925619 0.664762 0.027 Uiso 1 1 calc R U . . .
C12 C 0.5153(2) 0.5439(2) 0.2760(2) 0.0208(6) Uani 1 1 d . . . . .
H12A H 0.574194 0.514322 0.224466 0.025 Uiso 1 1 calc R U . . .
H12B H 0.451623 0.566606 0.242444 0.025 Uiso 1 1 calc R U . . .
C8 C 0.1681(2) 0.5861(3) 0.6442(2) 0.0236(6) Uani 1 1 d . . . . .
H8A H 0.117557 0.516763 0.653238 0.028 Uiso 1 1 calc R U . . .
H8B H 0.113326 0.622272 0.615726 0.028 Uiso 1 1 calc R U . . .
C9 C 0.2048(2) 0.4327(3) 0.4736(2) 0.0232(6) Uani 1 1 d . . . . .
H9A H 0.146491 0.452086 0.432218 0.028 Uiso 1 1 calc R U . . .
H9B H 0.159901 0.366340 0.489617 0.028 Uiso 1 1 calc R U . . .
C33 C 0.7255(2) 0.8460(3) 0.4569(2) 0.0247(6) Uani 1 1 d . . . . .
H33A H 0.779117 0.806757 0.482962 0.030 Uiso 1 1 calc R U . . .
H33B H 0.778041 0.911869 0.444595 0.030 Uiso 1 1 calc R U . . .
C32 C 0.6483(2) 0.7494(3) 0.3529(2) 0.0225(6) Uani 1 1 d . . . . .
H32A H 0.592552 0.787482 0.327633 0.027 Uiso 1 1 calc R U . . .
H32B H 0.701832 0.715369 0.297308 0.027 Uiso 1 1 calc R U . . .
C10 C 0.3090(2) 0.3894(3) 0.4088(2) 0.0228(6) Uani 1 1 d . . . . .
H10A H 0.370319 0.375755 0.452189 0.027 Uiso 1 1 calc R U . . .
H10B H 0.276469 0.310210 0.344334 0.027 Uiso 1 1 calc R U . . .
C7 C 0.2385(2) 0.6844(3) 0.7511(2) 0.0235(6) Uani 1 1 d . . . . .
H7A H 0.180497 0.717705 0.802473 0.028 Uiso 1 1 calc R U . . .
H7B H 0.291074 0.647306 0.780597 0.028 Uiso 1 1 calc R U . . .
C4 C 0.6266(2) 1.0332(3) 0.7206(2) 0.0250(6) Uani 1 1 d . . . . .
H4A H 0.672895 1.092816 0.791005 0.030 Uiso 1 1 calc R U . . .
H4B H 0.580131 1.078046 0.694697 0.030 Uiso 1 1 calc R U . . .
C2 C 0.2057(3) 0.7291(3) 0.4114(2) 0.0217(7) Uani 0.949(5) 1 d . . P A 1
H2A H 0.190325 0.638799 0.388522 0.026 Uiso 0.949(5) 1 calc R U P B 1
H2B H 0.180838 0.741582 0.349345 0.026 Uiso 0.949(5) 1 calc R U P B 1
C6 C 0.3970(3) 0.8715(3) 0.8306(2) 0.0310(7) Uani 1 1 d . . . . .
H6A H 0.455819 0.829300 0.846718 0.037 Uiso 1 1 calc R U . . .
H6B H 0.349909 0.902617 0.891858 0.037 Uiso 1 1 calc R U . . .
C5 C 0.4661(3) 0.9799(3) 0.8133(3) 0.0350(7) Uani 1 1 d . . . . .
H5A H 0.407305 1.018628 0.792287 0.042 Uiso 1 1 calc R U . . .
H5B H 0.516882 1.043324 0.880297 0.042 Uiso 1 1 calc R U . . .
C1 C 0.3422(2) 0.7861(3) 0.4479(2) 0.0203(7) Uani 0.949(5) 1 d . . P A 1
H1A H 0.386962 0.762450 0.384604 0.024 Uiso 0.949(5) 1 calc R U P B 1
H1B H 0.355173 0.877556 0.483322 0.024 Uiso 0.949(5) 1 calc R U P B 1
Br1A Br 0.0702(14) 0.8288(19) 0.4736(19) 0.072(8) Uani 0.0294(18) 1 d . . P C 3
C2A C 0.214(5) 0.846(6) 0.553(5) 0.030(8) Uani 0.051(5) 1 d . U P B 2
H2AA H 0.187749 0.925648 0.574936 0.036 Uiso 0.051(5) 1 calc R U P B 2
H2AB H 0.207297 0.822829 0.612066 0.036 Uiso 0.051(5) 1 calc R U P B 2
Br1 Br 0.1198(13) 0.7259(15) 0.4326(13) 0.078(6) Uani 0.0364(15) 1 d . . P B 2
C1A C 0.359(5) 0.860(6) 0.521(5) 0.029(6) Uani 0.051(5) 1 d . U P B 2
H1AD H 0.362161 0.855315 0.449173 0.034 Uiso 0.051(5) 1 calc R U P B 2
H1AE H 0.413957 0.937811 0.573935 0.034 Uiso 0.051(5) 1 calc R U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S1 2.1702(7) . ?
Ni1 S2 2.1656(6) . ?
Ni1 S7 2.1528(7) . ?
Ni1 S6 2.1684(6) . ?
Br1B C2 1.950(3) . ?
S1 C13 1.720(2) . ?
S2 C14 1.721(2) . ?
S3 C13 1.742(2) . ?
S3 C15 1.737(2) . ?
S4 C15 1.726(3) . ?
S4 C14 1.744(2) . ?
S7 C17 1.714(2) . ?
S5 C15 1.654(2) . ?
S9 C17 1.737(2) . ?
S9 C18 1.734(2) . ?
S8 C18 1.737(3) . ?
S8 C16 1.750(2) . ?
S6 C16 1.713(3) . ?
S10 C18 1.650(2) . ?
O6 C12 1.429(3) . ?
O6 C32 1.421(3) . ?
O5 C11 1.429(3) . ?
O5 C10 1.437(3) . ?
O1 C3 1.430(3) . ?
O1 C33 1.428(3) . ?
O4 C8 1.419(3) . ?
O4 C9 1.413(3) . ?
O2 C4 1.419(3) . ?
O2 C5 1.425(3) . ?
O3 C7 1.435(3) . ?
O3 C6 1.428(3) . ?
N1 H1AA 0.8900 . ?
N1 H1AB 0.8900 . ?
N1 H1AC 0.8900 . ?
N1 H1BD 0.8900 . ?
N1 H1BE 0.8900 . ?
N1 H1BF 0.8900 . ?
N1 C1 1.495(3) . ?
N1 C1A 1.53(6) . ?
C13 C14 1.358(3) . ?
C17 C16 1.365(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.500(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.490(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C7 1.495(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.502(4) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 C32 1.493(4) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C1 1.497(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C5 1.497(4) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?
C2A Br1 1.78(6) . ?
C2A C1A 1.67(7) . ?
C1A H1AD 0.9700 . ?
C1A H1AE 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S2 Ni1 S1 93.58(2) . . ?
S2 Ni1 S6 178.07(3) . . ?
S7 Ni1 S1 176.96(3) . . ?
S7 Ni1 S2 85.41(2) . . ?
S7 Ni1 S6 93.22(2) . . ?
S6 Ni1 S1 87.85(2) . . ?
C13 S1 Ni1 101.51(9) . . ?
C14 S2 Ni1 101.72(8) . . ?
C15 S3 C13 97.43(11) . . ?
C15 S4 C14 97.35(11) . . ?
C17 S7 Ni1 102.50(9) . . ?
C18 S9 C17 97.25(12) . . ?
C18 S8 C16 97.65(12) . . ?
C16 S6 Ni1 101.87(8) . . ?
C32 O6 C12 113.02(18) . . ?
C11 O5 C10 110.68(19) . . ?
C33 O1 C3 111.47(18) . . ?
C9 O4 C8 113.98(18) . . ?
C4 O2 C5 112.1(2) . . ?
C6 O3 C7 111.1(2) . . ?
H1AA N1 H1AB 109.5 . . ?
H1AA N1 H1AC 109.5 . . ?
H1AB N1 H1AC 109.5 . . ?
H1BD N1 H1BE 109.5 . . ?
H1BD N1 H1BF 109.5 . . ?
H1BE N1 H1BF 109.5 . . ?
C1 N1 H1AA 109.5 . . ?
C1 N1 H1AB 109.5 . . ?
C1 N1 H1AC 109.5 . . ?
C1A N1 H1BD 109.5 . . ?
C1A N1 H1BE 109.5 . . ?
C1A N1 H1BF 109.5 . . ?
S1 C13 S3 122.39(14) . . ?
C14 C13 S1 121.70(18) . . ?
C14 C13 S3 115.83(16) . . ?
S4 C15 S3 113.08(12) . . ?
S5 C15 S3 123.37(15) . . ?
S5 C15 S4 123.54(14) . . ?
S2 C14 S4 122.23(14) . . ?
C13 C14 S2 121.47(16) . . ?
C13 C14 S4 116.29(18) . . ?
S7 C17 S9 122.13(15) . . ?
C16 C17 S7 120.85(19) . . ?
C16 C17 S9 117.01(16) . . ?
S9 C18 S8 113.00(13) . . ?
S10 C18 S9 123.10(16) . . ?
S10 C18 S8 123.90(14) . . ?
O5 C11 H11A 109.8 . . ?
O5 C11 H11B 109.8 . . ?
O5 C11 C12 109.3(2) . . ?
H11A C11 H11B 108.3 . . ?
C12 C11 H11A 109.8 . . ?
C12 C11 H11B 109.8 . . ?
S6 C16 S8 123.41(15) . . ?
C17 C16 S8 115.04(18) . . ?
C17 C16 S6 121.53(17) . . ?
O1 C3 H3A 109.9 . . ?
O1 C3 H3B 109.9 . . ?
O1 C3 C4 109.0(2) . . ?
H3A C3 H3B 108.3 . . ?
C4 C3 H3A 109.9 . . ?
C4 C3 H3B 109.9 . . ?
O6 C12 C11 108.4(2) . . ?
O6 C12 H12A 110.0 . . ?
O6 C12 H12B 110.0 . . ?
C11 C12 H12A 110.0 . . ?
C11 C12 H12B 110.0 . . ?
H12A C12 H12B 108.4 . . ?
O4 C8 H8A 110.1 . . ?
O4 C8 H8B 110.1 . . ?
O4 C8 C7 107.90(19) . . ?
H8A C8 H8B 108.4 . . ?
C7 C8 H8A 110.1 . . ?
C7 C8 H8B 110.1 . . ?
O4 C9 H9A 110.0 . . ?
O4 C9 H9B 110.0 . . ?
O4 C9 C10 108.54(19) . . ?
H9A C9 H9B 108.4 . . ?
C10 C9 H9A 110.0 . . ?
C10 C9 H9B 110.0 . . ?
O1 C33 H33A 109.8 . . ?
O1 C33 H33B 109.8 . . ?
O1 C33 C32 109.54(19) . . ?
H33A C33 H33B 108.2 . . ?
C32 C33 H33A 109.8 . . ?
C32 C33 H33B 109.8 . . ?
O6 C32 C33 107.9(2) . . ?
O6 C32 H32A 110.1 . . ?
O6 C32 H32B 110.1 . . ?
C33 C32 H32A 110.1 . . ?
C33 C32 H32B 110.1 . . ?
H32A C32 H32B 108.4 . . ?
O5 C10 C9 108.6(2) . . ?
O5 C10 H10A 110.0 . . ?
O5 C10 H10B 110.0 . . ?
C9 C10 H10A 110.0 . . ?
C9 C10 H10B 110.0 . . ?
H10A C10 H10B 108.3 . . ?
O3 C7 C8 108.7(2) . . ?
O3 C7 H7A 109.9 . . ?
O3 C7 H7B 109.9 . . ?
C8 C7 H7A 109.9 . . ?
C8 C7 H7B 109.9 . . ?
H7A C7 H7B 108.3 . . ?
O2 C4 C3 108.0(2) . . ?
O2 C4 H4A 110.1 . . ?
O2 C4 H4B 110.1 . . ?
C3 C4 H4A 110.1 . . ?
C3 C4 H4B 110.1 . . ?
H4A C4 H4B 108.4 . . ?
Br1B C2 H2A 109.3 . . ?
Br1B C2 H2B 109.3 . . ?
H2A C2 H2B 108.0 . . ?
C1 C2 Br1B 111.5(2) . . ?
C1 C2 H2A 109.3 . . ?
C1 C2 H2B 109.3 . . ?
O3 C6 H6A 109.8 . . ?
O3 C6 H6B 109.8 . . ?
O3 C6 C5 109.4(2) . . ?
H6A C6 H6B 108.2 . . ?
C5 C6 H6A 109.8 . . ?
C5 C6 H6B 109.8 . . ?
O2 C5 C6 108.8(2) . . ?
O2 C5 H5A 109.9 . . ?
O2 C5 H5B 109.9 . . ?
C6 C5 H5A 109.9 . . ?
C6 C5 H5B 109.9 . . ?
H5A C5 H5B 108.3 . . ?
N1 C1 C2 112.7(2) . . ?
N1 C1 H1A 109.1 . . ?
N1 C1 H1B 109.1 . . ?
C2 C1 H1A 109.1 . . ?
C2 C1 H1B 109.1 . . ?
H1A C1 H1B 107.8 . . ?
H2AA C2A H2AB 108.8 . . ?
Br1 C2A H2AA 110.7 . . ?
Br1 C2A H2AB 110.7 . . ?
C1A C2A H2AA 110.7 . . ?
C1A C2A H2AB 110.7 . . ?
C1A C2A Br1 105(4) . . ?
N1 C1A C2A 102(4) . . ?
N1 C1A H1AD 111.4 . . ?
N1 C1A H1AE 111.4 . . ?
C2A C1A H1AD 111.4 . . ?
C2A C1A H1AE 111.4 . . ?
H1AD C1A H1AE 109.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S1 C13 S3 178.48(13) . . . . ?
Ni1 S1 C13 C14 1.7(2) . . . . ?
Ni1 S2 C14 S4 -178.68(13) . . . . ?
Ni1 S2 C14 C13 0.7(2) . . . . ?
Ni1 S7 C17 S9 179.37(13) . . . . ?
Ni1 S7 C17 C16 -2.1(2) . . . . ?
Ni1 S6 C16 S8 177.55(13) . . . . ?
Ni1 S6 C16 C17 -0.9(2) . . . . ?
Br1B C2 C1 N1 72.9(3) . . . . ?
S1 C13 C14 S2 -1.7(3) . . . . ?
S1 C13 C14 S4 177.71(12) . . . . ?
S3 C13 C14 S2 -178.70(13) . . . . ?
S3 C13 C14 S4 0.7(3) . . . . ?
S7 C17 C16 S8 -176.41(13) . . . . ?
S7 C17 C16 S6 2.2(3) . . . . ?
S9 C17 C16 S8 2.2(3) . . . . ?
S9 C17 C16 S6 -179.24(13) . . . . ?
O5 C11 C12 O6 61.9(3) . . . . ?
O1 C3 C4 O2 65.9(3) . . . . ?
O1 C33 C32 O6 -62.7(3) . . . . ?
O4 C8 C7 O3 58.7(3) . . . . ?
O4 C9 C10 O5 -64.8(3) . . . . ?
O3 C6 C5 O2 -64.9(3) . . . . ?
C13 S3 C15 S4 -0.61(15) . . . . ?
C13 S3 C15 S5 -179.50(16) . . . . ?
C15 S3 C13 S1 -177.04(16) . . . . ?
C15 S3 C13 C14 0.0(2) . . . . ?
C15 S4 C14 S2 178.41(16) . . . . ?
C15 S4 C14 C13 -1.0(2) . . . . ?
C14 S4 C15 S3 0.90(16) . . . . ?
C14 S4 C15 S5 179.79(16) . . . . ?
C17 S9 C18 S8 1.70(15) . . . . ?
C17 S9 C18 S10 -178.06(16) . . . . ?
C18 S9 C17 S7 176.19(16) . . . . ?
C18 S9 C17 C16 -2.4(2) . . . . ?
C18 S8 C16 S6 -179.37(16) . . . . ?
C18 S8 C16 C17 -0.8(2) . . . . ?
C11 O5 C10 C9 -173.2(2) . . . . ?
C16 S8 C18 S9 -0.78(15) . . . . ?
C16 S8 C18 S10 178.98(16) . . . . ?
C3 O1 C33 C32 170.1(2) . . . . ?
C12 O6 C32 C33 -170.9(2) . . . . ?
C8 O4 C9 C10 -175.1(2) . . . . ?
C9 O4 C8 C7 169.1(2) . . . . ?
C33 O1 C3 C4 178.3(2) . . . . ?
C32 O6 C12 C11 173.9(2) . . . . ?
C10 O5 C11 C12 -179.5(2) . . . . ?
C7 O3 C6 C5 -175.2(2) . . . . ?
C4 O2 C5 C6 -170.7(2) . . . . ?
C6 O3 C7 C8 -171.4(2) . . . . ?
C5 O2 C4 C3 172.7(2) . . . . ?
Br1 C2A C1A N1 -77(4) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.239
_oxdiff_exptl_absorpt_empirical_full_min 0.447
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_193k
_database_code_depnum_ccdc_archive 'CCDC 2053303'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-18 downloaded from the CCDC.
;
_audit_creation_date             2020-11-10
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C2 H7 Br1 N, C12 H24 O6'
_chemical_formula_sum            'C20 H31 Br N Ni O6 S10'
_chemical_formula_weight         840.68
_chemical_melting_point          ?
_chemical_oxdiff_formula         BrCHNONiS
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.0467(3)
_cell_length_b                   12.0603(3)
_cell_length_c                   13.7505(4)
_cell_angle_alpha                64.635(3)
_cell_angle_beta                 79.967(2)
_cell_angle_gamma                78.865(2)
_cell_volume                     1615.49(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    16920
_cell_measurement_temperature    193
_cell_measurement_theta_max      30.9320
_cell_measurement_theta_min      1.9180
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.520
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60481
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             858
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0721
_diffrn_reflns_av_unetI/netI     0.0605
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.834
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            40000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.834
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.024
_diffrn_reflns_theta_min         1.886
_diffrn_ambient_temperature      193
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.834
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -13.00  18.00   0.50    1.08    --    5.18 -30.00  -9.70   62
  2  ω    -10.00  77.00   0.50    1.08    --    5.18  57.00  60.00  174
  3  ω    -54.00  19.00   0.50    1.08    --    5.18 -28.00  90.96  146
  4  ω    -49.00 -20.00   0.50    1.08    --    5.18 -37.00 -30.00   58
  5  ω    -59.00 -33.00   0.50    1.08    --    5.18 -30.00  -9.70   52
  6  ω    -53.00  19.00   0.50    1.08    --    5.18 -28.00  51.36  144
  7  ω    -16.00  18.00   0.50    1.08    --    5.18 -37.00 -30.00   68
  8  ω    -67.00  19.00   0.50    1.08    --    5.18 -33.00 -92.28  172
  9  ω    -69.00  19.00   0.50    1.08    --    5.18 -28.00-143.18  176
 10  ω    -76.00   8.00   0.50    1.08    --   -4.95 -19.00 150.00  168
 11  ω    -18.00  25.00   0.50    1.08    --   -4.95 -99.00  90.00   86
 12  ω    -17.00  26.00   0.50    1.08    --   -4.95 -99.00 -90.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0297751000
_diffrn_orient_matrix_UB_12      0.0038818000
_diffrn_orient_matrix_UB_13      0.0399517000
_diffrn_orient_matrix_UB_21      -0.0300184000
_diffrn_orient_matrix_UB_22      -0.0493836000
_diffrn_orient_matrix_UB_23      0.0405775000
_diffrn_orient_matrix_UB_31      0.0504082000
_diffrn_orient_matrix_UB_32      -0.0431166000
_diffrn_orient_matrix_UB_33      -0.0071639000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6231
_reflns_number_total             8603
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT n/a (Sheldrick, 2015)'
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         8603
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0375
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0315P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0851
_refine_ls_wR_factor_ref         0.0918
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C9 \\sim C16 \\sim N1: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C2 \\sim C1 \\sim N1: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
C1A \\sim N1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
3. Others
 1*[Sof(Br1)]+1*[Sof(Br1B)]+1*[Sof(Br1A)]=1 with esd of 0.0001
 Sof(H1BD)=Sof(H1BE)=Sof(H1BF)=Sof(C1A)=Sof(H1AD)=Sof(H1AE)=Sof(C2A)=Sof(H2AA)=
 Sof(H2AB)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=
 Sof(H2B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C8(H8A,H8B), C11(H11A,H11B), C12(H12A,H12B), C9(H9A,H9B),
 C14(H14A,H14B), C3(H3A,H3B), C13(H13A,H13B), C7(H7A,H7B), C4(H4A,H4B), C6(H6A,
 H6B), C5(H5A,H5B), C1A(H1AD,H1AE), C1(H1A,H1B), C2(H2A,H2B), C2A(H2AA,H2AB)
4.b Idealised Me refined as rotating group:
 N1(H1BD,H1BE,H1BF), N1(H1AA,H1AB,H1AC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.13628(2) 0.46475(2) 0.88474(2) 0.02513(8) Uani 1 1 d . . . . .
S1 S 0.10313(5) 0.33981(4) 0.81939(4) 0.02762(12) Uani 1 1 d . . . . .
S3 S 0.20946(5) 0.07169(4) 0.86941(5) 0.02895(13) Uani 1 1 d . . . . .
S9 S 0.05659(5) 0.84515(4) 0.92192(5) 0.02984(13) Uani 1 1 d . . . . .
S4 S 0.35742(5) 0.06091(4) 1.02737(5) 0.03028(13) Uani 1 1 d . . . . .
S2 S 0.26655(5) 0.32805(5) 0.99056(5) 0.03198(13) Uani 1 1 d . . . . .
S7 S 0.16326(5) 0.58210(5) 0.95868(5) 0.03152(13) Uani 1 1 d . . . . .
S6 S 0.01272(5) 0.60801(5) 0.77500(5) 0.03332(14) Uani 1 1 d . . . . .
S8 S -0.07708(6) 0.87356(5) 0.74821(5) 0.03793(15) Uani 1 1 d . . . . .
S5 S 0.36385(6) -0.16546(5) 0.99049(5) 0.03888(15) Uani 1 1 d . . . . .
S10 S -0.08814(6) 1.08849(5) 0.80506(6) 0.04478(17) Uani 1 1 d . . . . .
Br1A Br 0.07563(10) 0.14559(13) 0.53577(12) 0.0548(5) Uani 0.2654(14) 1 d . . P
A 3
O5 O 0.36268(14) 0.39229(14) 0.62043(13) 0.0357(4) Uani 1 1 d . . . . .
O6 O 0.57435(14) 0.22194(13) 0.62546(12) 0.0363(4) Uani 1 1 d . . . . .
O4 O 0.25704(13) 0.53098(14) 0.42406(13) 0.0376(4) Uani 1 1 d . . . . .
O1 O 0.64679(14) 0.13925(14) 0.46025(13) 0.0386(4) Uani 1 1 d . . . . .
N1 N 0.39912(17) 0.28537(17) 0.46695(16) 0.0368(5) Uani 1 1 d . U . . .
H1BD H 0.349067 0.329520 0.415341 0.044 Uiso 0.604(6) 1 calc R U P B 2
H1BE H 0.473897 0.266533 0.437059 0.044 Uiso 0.604(6) 1 calc R U P B 2
H1BF H 0.405250 0.329399 0.503426 0.044 Uiso 0.604(6) 1 calc R U P B 2
H1AA H 0.407564 0.338281 0.397811 0.044 Uiso 0.396(6) 1 calc R U P B 1
H1AB H 0.473651 0.249645 0.488811 0.044 Uiso 0.396(6) 1 calc R U P B 1
H1AC H 0.360622 0.325909 0.507006 0.044 Uiso 0.396(6) 1 calc R U P B 1
O3 O 0.31796(15) 0.45520(15) 0.25902(14) 0.0454(4) Uani 1 1 d . . . . .
O2 O 0.54590(17) 0.30047(17) 0.26678(14) 0.0506(5) Uani 1 1 d . . . . .
C19 C 0.07149(19) 0.71626(17) 0.89175(17) 0.0267(4) Uani 1 1 d . . . . .
C15 C 0.19948(18) 0.20836(17) 0.88716(17) 0.0249(4) Uani 1 1 d . . . . .
C16 C 0.26898(19) 0.20227(17) 0.96139(17) 0.0264(4) Uani 1 1 d . . . . .
C18 C 0.00708(19) 0.72841(17) 0.81135(18) 0.0285(5) Uani 1 1 d . . . . .
C20 C -0.03888(19) 0.94315(18) 0.82435(19) 0.0305(5) Uani 1 1 d . . . . .
C17 C 0.31217(19) -0.01866(17) 0.96405(17) 0.0276(4) Uani 1 1 d . . . . .
C10 C 0.3048(2) 0.5176(2) 0.5893(2) 0.0393(6) Uani 1 1 d . . . . .
H10A H 0.365569 0.573602 0.548292 0.047 Uiso 1 1 calc R U . . .
H10B H 0.271449 0.532731 0.653205 0.047 Uiso 1 1 calc R U . . .
C8 C 0.1709(2) 0.5615(2) 0.3478(2) 0.0421(6) Uani 1 1 d . . . . .
H8A H 0.120419 0.639946 0.338842 0.050 Uiso 1 1 calc R U . . .
H8B H 0.116625 0.498228 0.373009 0.050 Uiso 1 1 calc R U . . .
C11 C 0.4527(2) 0.3619(2) 0.69398(19) 0.0384(5) Uani 1 1 d . . . . .
H11A H 0.413198 0.371509 0.759190 0.046 Uiso 1 1 calc R U . . .
H11B H 0.515501 0.417212 0.661109 0.046 Uiso 1 1 calc R U . . .
C12 C 0.5114(2) 0.2312(2) 0.72156(19) 0.0421(6) Uani 1 1 d . . . . .
H12A H 0.569593 0.207654 0.774608 0.051 Uiso 1 1 calc R U . . .
H12B H 0.448443 0.176009 0.752120 0.051 Uiso 1 1 calc R U . . .
C9 C 0.2035(2) 0.5403(2) 0.5222(2) 0.0424(6) Uani 1 1 d . . . . .
H9A H 0.146463 0.479685 0.560475 0.051 Uiso 1 1 calc R U . . .
H9B H 0.157724 0.622115 0.507211 0.051 Uiso 1 1 calc R U . . .
C14 C 0.7250(2) 0.1156(2) 0.5411(2) 0.0465(6) Uani 1 1 d . . . . .
H14A H 0.774626 0.182488 0.517577 0.056 Uiso 1 1 calc R U . . .
H14B H 0.780720 0.039293 0.552717 0.056 Uiso 1 1 calc R U . . .
C3 C 0.7147(2) 0.1691(2) 0.3561(2) 0.0429(6) Uani 1 1 d . . . . .
H3A H 0.779007 0.101202 0.357751 0.052 Uiso 1 1 calc R U . . .
H3B H 0.753999 0.242239 0.336048 0.052 Uiso 1 1 calc R U . . .
C13 C 0.6465(3) 0.1052(2) 0.6441(2) 0.0470(6) Uani 1 1 d . . . . .
H13A H 0.592850 0.041969 0.665505 0.056 Uiso 1 1 calc R U . . .
H13B H 0.698495 0.082669 0.701472 0.056 Uiso 1 1 calc R U . . .
C7 C 0.2425(2) 0.5703(2) 0.2429(2) 0.0428(6) Uani 1 1 d . . . . .
H7A H 0.185920 0.589267 0.189557 0.051 Uiso 1 1 calc R U . . .
H7B H 0.294057 0.636028 0.216385 0.051 Uiso 1 1 calc R U . . .
C4 C 0.6292(3) 0.1922(3) 0.2757(2) 0.0501(7) Uani 1 1 d . . . . .
H4A H 0.675705 0.203396 0.206141 0.060 Uiso 1 1 calc R U . . .
H4B H 0.583847 0.122264 0.298897 0.060 Uiso 1 1 calc R U . . .
C6 C 0.4011(3) 0.4648(3) 0.1647(2) 0.0626(9) Uani 1 1 d . . . . .
H6A H 0.459102 0.521825 0.151716 0.075 Uiso 1 1 calc R U . . .
H6B H 0.354963 0.496268 0.102164 0.075 Uiso 1 1 calc R U . . .
C5 C 0.4699(3) 0.3397(3) 0.1812(3) 0.0731(10) Uani 1 1 d . . . . .
H5A H 0.411783 0.281276 0.199182 0.088 Uiso 1 1 calc R U . . .
H5B H 0.521055 0.343281 0.115190 0.088 Uiso 1 1 calc R U . . .
C1A C 0.3445(4) 0.1627(4) 0.5466(4) 0.0447(12) Uani 0.604(6) 1 d . U P B 2
H1AD H 0.355680 0.107322 0.510377 0.054 Uiso 0.604(6) 1 calc R U P B 2
H1AE H 0.391619 0.122434 0.608859 0.054 Uiso 0.604(6) 1 calc R U P B 2
C1 C 0.3320(12) 0.1982(10) 0.4779(15) 0.142(6) Uani 0.396(6) 1 d . U P B 1
H1A H 0.386246 0.147474 0.444859 0.170 Uiso 0.396(6) 1 calc R U P B 1
H1B H 0.323354 0.146619 0.554879 0.170 Uiso 0.396(6) 1 calc R U P B 1
Br1B Br 0.10581(5) 0.22508(6) 0.47368(5) 0.0455(2) Uani 0.5480(13) 1 d . . P B
2
Br1 Br 0.11819(18) 0.20427(19) 0.56954(18) 0.0701(9) Uani 0.1866(13) 1 d . . P
B 1
C2 C 0.2232(9) 0.2109(9) 0.4465(8) 0.082(3) Uani 0.396(6) 1 d . U P B 1
H2A H 0.216096 0.144080 0.427178 0.098 Uiso 0.396(6) 1 calc R U P B 1
H2B H 0.206397 0.289472 0.385577 0.098 Uiso 0.396(6) 1 calc R U P B 1
C2A C 0.2118(4) 0.1815(4) 0.5848(4) 0.0427(12) Uani 0.604(6) 1 d . . P B 2
H2AA H 0.197800 0.246639 0.610695 0.051 Uiso 0.604(6) 1 calc R U P B 2
H2AB H 0.190195 0.106075 0.645165 0.051 Uiso 0.604(6) 1 calc R U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S1 2.1680(6) . ?
Ni1 S2 2.1597(6) . ?
Ni1 S7 2.1510(6) . ?
Ni1 S6 2.1675(6) . ?
S1 C15 1.7154(19) . ?
S3 C15 1.7475(19) . ?
S3 C17 1.729(2) . ?
S9 C19 1.7451(19) . ?
S9 C20 1.721(2) . ?
S4 C16 1.7391(19) . ?
S4 C17 1.727(2) . ?
S2 C16 1.722(2) . ?
S7 C19 1.7053(19) . ?
S6 C18 1.714(2) . ?
S8 C18 1.7416(19) . ?
S8 C20 1.738(2) . ?
S5 C17 1.6502(19) . ?
S10 C20 1.6499(19) . ?
O5 C10 1.429(3) . ?
O5 C11 1.428(3) . ?
O6 C12 1.420(3) . ?
O6 C13 1.418(3) . ?
O4 C8 1.421(3) . ?
O4 C9 1.418(3) . ?
O1 C14 1.426(3) . ?
O1 C3 1.425(3) . ?
N1 H1BD 0.8900 . ?
N1 H1BE 0.8900 . ?
N1 H1BF 0.8900 . ?
N1 H1AA 0.8900 . ?
N1 H1AB 0.8900 . ?
N1 H1AC 0.8900 . ?
N1 C1A 1.574(5) . ?
N1 C1 1.344(10) . ?
O3 C7 1.423(3) . ?
O3 C6 1.427(3) . ?
O2 C4 1.417(3) . ?
O2 C5 1.424(3) . ?
C19 C18 1.358(3) . ?
C15 C16 1.350(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C9 1.485(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C7 1.491(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.493(3) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C13 1.495(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.480(4) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C5 1.493(4) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C1A H1AD 0.9700 . ?
C1A H1AE 0.9700 . ?
C1A C2A 1.478(7) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.306(14) . ?
Br1B C2A 1.918(4) . ?
Br1 C2 1.857(10) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S2 Ni1 S1 93.37(2) . . ?
S2 Ni1 S6 177.12(3) . . ?
S7 Ni1 S1 176.53(3) . . ?
S7 Ni1 S2 85.46(2) . . ?
S7 Ni1 S6 93.10(2) . . ?
S6 Ni1 S1 88.21(2) . . ?
C15 S1 Ni1 101.58(7) . . ?
C17 S3 C15 97.43(10) . . ?
C20 S9 C19 97.25(10) . . ?
C17 S4 C16 97.21(10) . . ?
C16 S2 Ni1 101.95(7) . . ?
C19 S7 Ni1 102.39(7) . . ?
C18 S6 Ni1 101.87(7) . . ?
C20 S8 C18 97.58(10) . . ?
C11 O5 C10 111.61(17) . . ?
C13 O6 C12 113.36(18) . . ?
C9 O4 C8 114.20(17) . . ?
C3 O1 C14 111.72(19) . . ?
H1BD N1 H1BE 109.5 . . ?
H1BD N1 H1BF 109.5 . . ?
H1BE N1 H1BF 109.5 . . ?
H1AA N1 H1AB 109.5 . . ?
H1AA N1 H1AC 109.5 . . ?
H1AB N1 H1AC 109.5 . . ?
C1A N1 H1BD 109.5 . . ?
C1A N1 H1BE 109.5 . . ?
C1A N1 H1BF 109.5 . . ?
C1 N1 H1AA 109.5 . . ?
C1 N1 H1AB 109.5 . . ?
C1 N1 H1AC 109.5 . . ?
C7 O3 C6 110.7(2) . . ?
C4 O2 C5 112.2(2) . . ?
S7 C19 S9 121.89(13) . . ?
C18 C19 S9 116.61(14) . . ?
C18 C19 S7 121.50(15) . . ?
S1 C15 S3 122.50(12) . . ?
C16 C15 S1 121.96(15) . . ?
C16 C15 S3 115.49(14) . . ?
S2 C16 S4 122.14(12) . . ?
C15 C16 S4 116.71(15) . . ?
C15 C16 S2 121.13(14) . . ?
S6 C18 S8 123.49(13) . . ?
C19 C18 S6 121.11(14) . . ?
C19 C18 S8 115.39(15) . . ?
S9 C20 S8 113.13(11) . . ?
S10 C20 S9 123.19(14) . . ?
S10 C20 S8 123.67(13) . . ?
S4 C17 S3 113.15(10) . . ?
S5 C17 S3 123.77(13) . . ?
S5 C17 S4 123.08(13) . . ?
O5 C10 H10A 109.8 . . ?
O5 C10 H10B 109.8 . . ?
O5 C10 C9 109.34(19) . . ?
H10A C10 H10B 108.3 . . ?
C9 C10 H10A 109.8 . . ?
C9 C10 H10B 109.8 . . ?
O4 C8 H8A 110.1 . . ?
O4 C8 H8B 110.1 . . ?
O4 C8 C7 108.04(18) . . ?
H8A C8 H8B 108.4 . . ?
C7 C8 H8A 110.1 . . ?
C7 C8 H8B 110.1 . . ?
O5 C11 H11A 109.9 . . ?
O5 C11 H11B 109.9 . . ?
O5 C11 C12 109.01(18) . . ?
H11A C11 H11B 108.3 . . ?
C12 C11 H11A 109.9 . . ?
C12 C11 H11B 109.9 . . ?
O6 C12 C11 108.44(19) . . ?
O6 C12 H12A 110.0 . . ?
O6 C12 H12B 110.0 . . ?
C11 C12 H12A 110.0 . . ?
C11 C12 H12B 110.0 . . ?
H12A C12 H12B 108.4 . . ?
O4 C9 C10 108.30(18) . . ?
O4 C9 H9A 110.0 . . ?
O4 C9 H9B 110.0 . . ?
C10 C9 H9A 110.0 . . ?
C10 C9 H9B 110.0 . . ?
H9A C9 H9B 108.4 . . ?
O1 C14 H14A 109.8 . . ?
O1 C14 H14B 109.8 . . ?
O1 C14 C13 109.2(2) . . ?
H14A C14 H14B 108.3 . . ?
C13 C14 H14A 109.8 . . ?
C13 C14 H14B 109.8 . . ?
O1 C3 H3A 109.8 . . ?
O1 C3 H3B 109.8 . . ?
O1 C3 C4 109.4(2) . . ?
H3A C3 H3B 108.2 . . ?
C4 C3 H3A 109.8 . . ?
C4 C3 H3B 109.8 . . ?
O6 C13 C14 107.7(2) . . ?
O6 C13 H13A 110.2 . . ?
O6 C13 H13B 110.2 . . ?
C14 C13 H13A 110.2 . . ?
C14 C13 H13B 110.2 . . ?
H13A C13 H13B 108.5 . . ?
O3 C7 C8 108.9(2) . . ?
O3 C7 H7A 109.9 . . ?
O3 C7 H7B 109.9 . . ?
C8 C7 H7A 109.9 . . ?
C8 C7 H7B 109.9 . . ?
H7A C7 H7B 108.3 . . ?
O2 C4 C3 107.9(2) . . ?
O2 C4 H4A 110.1 . . ?
O2 C4 H4B 110.1 . . ?
C3 C4 H4A 110.1 . . ?
C3 C4 H4B 110.1 . . ?
H4A C4 H4B 108.4 . . ?
O3 C6 H6A 109.9 . . ?
O3 C6 H6B 109.9 . . ?
O3 C6 C5 109.0(3) . . ?
H6A C6 H6B 108.3 . . ?
C5 C6 H6A 109.9 . . ?
C5 C6 H6B 109.9 . . ?
O2 C5 C6 108.9(2) . . ?
O2 C5 H5A 109.9 . . ?
O2 C5 H5B 109.9 . . ?
C6 C5 H5A 109.9 . . ?
C6 C5 H5B 109.9 . . ?
H5A C5 H5B 108.3 . . ?
N1 C1A H1AD 108.7 . . ?
N1 C1A H1AE 108.7 . . ?
H1AD C1A H1AE 107.6 . . ?
C2A C1A N1 114.3(4) . . ?
C2A C1A H1AD 108.7 . . ?
C2A C1A H1AE 108.7 . . ?
N1 C1 H1A 104.9 . . ?
N1 C1 H1B 104.9 . . ?
H1A C1 H1B 105.8 . . ?
C2 C1 N1 129.5(10) . . ?
C2 C1 H1A 104.9 . . ?
C2 C1 H1B 104.9 . . ?
C1 C2 Br1 101.8(11) . . ?
C1 C2 H2A 111.4 . . ?
C1 C2 H2B 111.4 . . ?
Br1 C2 H2A 111.4 . . ?
Br1 C2 H2B 111.4 . . ?
H2A C2 H2B 109.3 . . ?
C1A C2A Br1B 112.5(3) . . ?
C1A C2A H2AA 109.1 . . ?
C1A C2A H2AB 109.1 . . ?
Br1B C2A H2AA 109.1 . . ?
Br1B C2A H2AB 109.1 . . ?
H2AA C2A H2AB 107.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S1 C15 S3 178.41(11) . . . . ?
Ni1 S1 C15 C16 1.2(2) . . . . ?
Ni1 S2 C16 S4 -178.22(11) . . . . ?
Ni1 S2 C16 C15 0.3(2) . . . . ?
Ni1 S7 C19 S9 179.00(11) . . . . ?
Ni1 S7 C19 C18 -1.6(2) . . . . ?
Ni1 S6 C18 S8 178.60(12) . . . . ?
Ni1 S6 C18 C19 -0.2(2) . . . . ?
S1 C15 C16 S4 177.48(11) . . . . ?
S1 C15 C16 S2 -1.1(3) . . . . ?
S3 C15 C16 S4 0.1(2) . . . . ?
S3 C15 C16 S2 -178.47(11) . . . . ?
S9 C19 C18 S6 -179.33(12) . . . . ?
S9 C19 C18 S8 1.8(2) . . . . ?
S7 C19 C18 S6 1.3(3) . . . . ?
S7 C19 C18 S8 -177.59(12) . . . . ?
O5 C10 C9 O4 -65.9(2) . . . . ?
O5 C11 C12 O6 62.8(2) . . . . ?
O4 C8 C7 O3 58.3(3) . . . . ?
O1 C14 C13 O6 -64.3(3) . . . . ?
O1 C3 C4 O2 66.2(3) . . . . ?
N1 C1A C2A Br1B 71.8(4) . . . . ?
N1 C1 C2 Br1 -93.2(19) . . . . ?
O3 C6 C5 O2 -64.9(4) . . . . ?
C19 S9 C20 S8 1.34(14) . . . . ?
C19 S9 C20 S10 -178.33(15) . . . . ?
C15 S3 C17 S4 -0.90(14) . . . . ?
C15 S3 C17 S5 179.95(15) . . . . ?
C16 S4 C17 S3 0.95(14) . . . . ?
C16 S4 C17 S5 -179.89(15) . . . . ?
C18 S8 C20 S9 -0.57(15) . . . . ?
C18 S8 C20 S10 179.10(16) . . . . ?
C20 S9 C19 S7 177.47(14) . . . . ?
C20 S9 C19 C18 -1.9(2) . . . . ?
C20 S8 C18 S6 -179.56(15) . . . . ?
C20 S8 C18 C19 -0.7(2) . . . . ?
C17 S3 C15 S1 -176.86(14) . . . . ?
C17 S3 C15 C16 0.47(19) . . . . ?
C17 S4 C16 S2 177.92(14) . . . . ?
C17 S4 C16 C15 -0.67(19) . . . . ?
C10 O5 C11 C12 -178.84(19) . . . . ?
C8 O4 C9 C10 -174.73(19) . . . . ?
C11 O5 C10 C9 -174.19(19) . . . . ?
C12 O6 C13 C14 -169.7(2) . . . . ?
C9 O4 C8 C7 169.74(19) . . . . ?
C14 O1 C3 C4 179.8(2) . . . . ?
C3 O1 C14 C13 170.93(19) . . . . ?
C13 O6 C12 C11 172.7(2) . . . . ?
C7 O3 C6 C5 -174.7(2) . . . . ?
C4 O2 C5 C6 -170.3(3) . . . . ?
C6 O3 C7 C8 -171.7(2) . . . . ?
C5 O2 C4 C3 172.4(3) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.102
_oxdiff_exptl_absorpt_empirical_full_min 0.270
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_213k
_database_code_depnum_ccdc_archive 'CCDC 2053304'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-18 downloaded from the CCDC.
;
_audit_creation_date             2020-11-10
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C2 H7 Br1 N, C12 H24 O6'
_chemical_formula_sum            'C20 H31 Br N Ni O6 S10'
_chemical_formula_weight         840.68
_chemical_melting_point          ?
_chemical_oxdiff_formula         BrCHNONiS
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.0537(3)
_cell_length_b                   12.0557(3)
_cell_length_c                   13.7262(4)
_cell_angle_alpha                64.890(3)
_cell_angle_beta                 80.331(2)
_cell_angle_gamma                78.815(2)
_cell_volume                     1617.26(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    16151
_cell_measurement_temperature    213
_cell_measurement_theta_max      30.6460
_cell_measurement_theta_min      1.9100
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.517
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60214
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             858
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0762
_diffrn_reflns_av_unetI/netI     0.0663
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.829
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            40716
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.829
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.061
_diffrn_reflns_theta_min         1.883
_diffrn_ambient_temperature      213
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.829
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -69.00  18.00   0.50    1.08    --    5.18 -31.00  -9.29  174
  2  ω    -66.00  19.00   0.50    1.08    --    5.18 -33.00-142.75  170
  3  ω    -50.00  19.00   0.50    1.08    --    5.18 -28.00 -90.37  138
  4  ω    -66.00  19.00   0.50    1.08    --    5.18 -28.00  51.09  170
  5  ω    -66.00  18.00   0.50    1.08    --    5.18 -37.00 120.00  168
  6  ω    -61.00  18.00   0.50    1.08    --    5.18 -29.00 169.50  158
  7  ω    -17.00  26.00   0.50    1.08    --   -4.95 -99.00 -90.00   86
  8  ω    -14.00  26.00   0.50    1.08    --   -4.95 -99.00-150.00   80
  9  ω    -16.00  25.00   0.50    1.08    --   -4.95 -99.00  30.00   82
 10  ω    -15.00  29.00   0.50    1.08    --   -4.95 -99.00  90.00   88
 11  ω    -18.00  29.00   0.50    1.08    --   -4.95 -99.00 150.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0299132000
_diffrn_orient_matrix_UB_12      0.0037741000
_diffrn_orient_matrix_UB_13      0.0401298000
_diffrn_orient_matrix_UB_21      -0.0298253000
_diffrn_orient_matrix_UB_22      -0.0492357000
_diffrn_orient_matrix_UB_23      0.0403168000
_diffrn_orient_matrix_UB_31      0.0503427000
_diffrn_orient_matrix_UB_32      -0.0431829000
_diffrn_orient_matrix_UB_33      -0.0071757000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5863
_reflns_number_total             8593
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT n/a (Sheldrick, 2015)'
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         8593
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0391
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0223P)²+0.2340P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0903
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C9 \\sim C16 \\sim N1: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C2 \\sim C1 \\sim N1: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
C1A \\sim N1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
3. Others
 1*[Sof(Br1)]+1*[Sof(Br1B)]+1*[Sof(Br1A)]=1 with esd of 0.0001
 Sof(H1BD)=Sof(H1BE)=Sof(H1BF)=Sof(C1A)=Sof(H1AD)=Sof(H1AE)=Sof(C2A)=Sof(H2AA)=
 Sof(H2AB)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=
 Sof(H2B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C8(H8A,H8B), C11(H11A,H11B), C12(H12A,H12B), C9(H9A,H9B),
 C14(H14A,H14B), C3(H3A,H3B), C13(H13A,H13B), C7(H7A,H7B), C4(H4A,H4B), C6(H6A,
 H6B), C5(H5A,H5B), C1A(H1AD,H1AE), C1(H1A,H1B), C2(H2A,H2B), C2A(H2AA,H2AB)
4.b Idealised Me refined as rotating group:
 N1(H1BD,H1BE,H1BF), N1(H1AA,H1AB,H1AC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.13547(3) 0.46464(2) 0.88421(2) 0.02810(8) Uani 1 1 d . . . . .
S1 S 0.10234(5) 0.33970(5) 0.81848(5) 0.03076(13) Uani 1 1 d . . . . .
S3 S 0.20908(5) 0.07179(5) 0.86835(5) 0.03274(14) Uani 1 1 d . . . . .
S9 S 0.05566(5) 0.84481(5) 0.92221(5) 0.03329(14) Uani 1 1 d . . . . .
S4 S 0.35731(5) 0.06152(5) 1.02654(5) 0.03392(14) Uani 1 1 d . . . . .
S2 S 0.26604(6) 0.32821(5) 0.99000(5) 0.03527(15) Uani 1 1 d . . . . .
S7 S 0.16234(6) 0.58184(5) 0.95886(5) 0.03509(14) Uani 1 1 d . . . . .
S6 S 0.01212(6) 0.60794(5) 0.77420(5) 0.03674(15) Uani 1 1 d . . . . .
S8 S -0.07832(6) 0.87313(5) 0.74810(6) 0.04206(16) Uani 1 1 d . . . . .
S5 S 0.36376(6) -0.16484(5) 0.98980(6) 0.04364(17) Uani 1 1 d . . . . .
S10 S -0.09026(6) 1.08732(6) 0.80639(7) 0.05013(19) Uani 1 1 d . . . . .
Br1A Br 0.07609(8) 0.14563(10) 0.53694(10) 0.0590(4) Uani 0.3519(15) 1 d . . P
A 3
O5 O 0.36176(15) 0.39237(15) 0.62004(14) 0.0386(4) Uani 1 1 d . . . . .
O6 O 0.57279(15) 0.22172(15) 0.62540(14) 0.0411(4) Uani 1 1 d . . . . .
O4 O 0.25693(14) 0.53167(16) 0.42325(14) 0.0420(4) Uani 1 1 d . . . . .
O1 O 0.64645(15) 0.13985(16) 0.45940(15) 0.0438(4) Uani 1 1 d . . . . .
N1 N 0.39959(18) 0.28734(19) 0.46477(18) 0.0418(5) Uani 1 1 d . U . . .
H1BD H 0.346754 0.334516 0.415991 0.050 Uiso 0.519(7) 1 calc R U P B 2
H1BE H 0.471270 0.267583 0.431378 0.050 Uiso 0.519(7) 1 calc R U P B 2
H1BF H 0.412051 0.328593 0.501935 0.050 Uiso 0.519(7) 1 calc R U P B 2
H1AA H 0.407348 0.339177 0.395442 0.050 Uiso 0.481(7) 1 calc R U P B 1
H1AB H 0.474211 0.250720 0.486234 0.050 Uiso 0.481(7) 1 calc R U P B 1
H1AC H 0.363041 0.329177 0.504327 0.050 Uiso 0.481(7) 1 calc R U P B 1
O3 O 0.31903(16) 0.45768(17) 0.25676(16) 0.0509(5) Uani 1 1 d . . . . .
O2 O 0.54614(18) 0.30255(19) 0.26540(16) 0.0577(5) Uani 1 1 d . . . . .
C19 C 0.0707(2) 0.71635(19) 0.89146(19) 0.0289(5) Uani 1 1 d . . . . .
C15 C 0.19897(19) 0.20781(18) 0.88648(18) 0.0278(5) Uani 1 1 d . . . . .
C16 C 0.2686(2) 0.20255(18) 0.96082(18) 0.0285(5) Uani 1 1 d . . . . .
C18 C 0.0064(2) 0.72800(19) 0.8113(2) 0.0315(5) Uani 1 1 d . . . . .
C20 C -0.0406(2) 0.9426(2) 0.8244(2) 0.0351(5) Uani 1 1 d . . . . .
C17 C 0.3122(2) -0.01796(19) 0.96270(19) 0.0309(5) Uani 1 1 d . . . . .
C10 C 0.3048(2) 0.5178(2) 0.5891(2) 0.0459(7) Uani 1 1 d . . . . .
H10A H 0.365755 0.573146 0.548708 0.055 Uiso 1 1 calc R U . . .
H10B H 0.271602 0.533157 0.652977 0.055 Uiso 1 1 calc R U . . .
C8 C 0.1720(2) 0.5633(2) 0.3460(2) 0.0478(7) Uani 1 1 d . . . . .
H8A H 0.121677 0.641808 0.337292 0.057 Uiso 1 1 calc R U . . .
H8B H 0.117562 0.500644 0.369945 0.057 Uiso 1 1 calc R U . . .
C11 C 0.4516(2) 0.3613(2) 0.6940(2) 0.0433(6) Uani 1 1 d . . . . .
H11A H 0.412358 0.371051 0.759103 0.052 Uiso 1 1 calc R U . . .
H11B H 0.514544 0.415984 0.661685 0.052 Uiso 1 1 calc R U . . .
C12 C 0.5098(3) 0.2304(2) 0.7213(2) 0.0461(6) Uani 1 1 d . . . . .
H12A H 0.567644 0.206060 0.775025 0.055 Uiso 1 1 calc R U . . .
H12B H 0.446665 0.175801 0.750665 0.055 Uiso 1 1 calc R U . . .
C9 C 0.2031(2) 0.5411(2) 0.5210(2) 0.0465(7) Uani 1 1 d . . . . .
H9A H 0.146157 0.480775 0.558521 0.056 Uiso 1 1 calc R U . . .
H9B H 0.157322 0.622953 0.506004 0.056 Uiso 1 1 calc R U . . .
C14 C 0.7234(2) 0.1163(3) 0.5408(2) 0.0520(7) Uani 1 1 d . . . . .
H14A H 0.772065 0.183376 0.518399 0.062 Uiso 1 1 calc R U . . .
H14B H 0.779828 0.040409 0.552119 0.062 Uiso 1 1 calc R U . . .
C3 C 0.7146(2) 0.1704(3) 0.3555(2) 0.0481(7) Uani 1 1 d . . . . .
H3A H 0.778937 0.102538 0.356968 0.058 Uiso 1 1 calc R U . . .
H3B H 0.753758 0.243104 0.336780 0.058 Uiso 1 1 calc R U . . .
C13 C 0.6448(3) 0.1048(3) 0.6432(2) 0.0547(8) Uani 1 1 d . . . . .
H13A H 0.591208 0.042140 0.663071 0.066 Uiso 1 1 calc R U . . .
H13B H 0.696515 0.081113 0.701331 0.066 Uiso 1 1 calc R U . . .
C7 C 0.2433(2) 0.5725(3) 0.2416(2) 0.0485(7) Uani 1 1 d . . . . .
H7A H 0.186786 0.592034 0.187795 0.058 Uiso 1 1 calc R U . . .
H7B H 0.294640 0.637969 0.216048 0.058 Uiso 1 1 calc R U . . .
C4 C 0.6305(3) 0.1945(3) 0.2746(3) 0.0560(8) Uani 1 1 d . . . . .
H4A H 0.677399 0.206172 0.205347 0.067 Uiso 1 1 calc R U . . .
H4B H 0.585600 0.124746 0.296402 0.067 Uiso 1 1 calc R U . . .
C6 C 0.4026(3) 0.4668(3) 0.1633(2) 0.0670(10) Uani 1 1 d . . . . .
H6A H 0.459905 0.524003 0.151082 0.080 Uiso 1 1 calc R U . . .
H6B H 0.356715 0.498200 0.100384 0.080 Uiso 1 1 calc R U . . .
C5 C 0.4719(3) 0.3438(4) 0.1789(3) 0.0798(12) Uani 1 1 d . . . . .
H5A H 0.414379 0.285632 0.194537 0.096 Uiso 1 1 calc R U . . .
H5B H 0.523895 0.348518 0.113212 0.096 Uiso 1 1 calc R U . . .
C1A C 0.3436(7) 0.1646(7) 0.5452(6) 0.0554(17) Uani 0.519(7) 1 d . U P B 2
H1AD H 0.354100 0.108970 0.509144 0.067 Uiso 0.519(7) 1 calc R U P B 2
H1AE H 0.390958 0.124309 0.607519 0.067 Uiso 0.519(7) 1 calc R U P B 2
C1 C 0.3295(11) 0.2001(10) 0.4775(14) 0.148(6) Uani 0.481(7) 1 d . U P B 1
H1A H 0.380436 0.149583 0.442587 0.178 Uiso 0.481(7) 1 calc R U P B 1
H1B H 0.323887 0.147900 0.554258 0.178 Uiso 0.481(7) 1 calc R U P B 1
Br1B Br 0.10563(6) 0.22610(8) 0.47382(7) 0.0510(3) Uani 0.4411(14) 1 d . . P B
2
Br1 Br 0.11916(19) 0.2045(2) 0.56872(19) 0.0783(10) Uani 0.2070(15) 1 d . . P B
1
C2 C 0.2212(8) 0.2153(8) 0.4499(8) 0.107(4) Uani 0.481(7) 1 d . U P B 1
H2A H 0.212500 0.151615 0.426919 0.129 Uiso 0.481(7) 1 calc R U P B 1
H2B H 0.203794 0.295542 0.391175 0.129 Uiso 0.481(7) 1 calc R U P B 1
C2A C 0.2128(6) 0.1839(6) 0.5829(5) 0.0524(18) Uani 0.519(7) 1 d . . P B 2
H2AA H 0.199347 0.249517 0.608318 0.063 Uiso 0.519(7) 1 calc R U P B 2
H2AB H 0.191786 0.109010 0.643540 0.063 Uiso 0.519(7) 1 calc R U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S1 2.1669(6) . ?
Ni1 S2 2.1571(6) . ?
Ni1 S7 2.1513(6) . ?
Ni1 S6 2.1650(6) . ?
S1 C15 1.719(2) . ?
S3 C15 1.741(2) . ?
S3 C17 1.725(2) . ?
S9 C19 1.742(2) . ?
S9 C20 1.724(2) . ?
S4 C16 1.736(2) . ?
S4 C17 1.726(2) . ?
S2 C16 1.718(2) . ?
S7 C19 1.707(2) . ?
S6 C18 1.714(2) . ?
S8 C18 1.744(2) . ?
S8 C20 1.731(3) . ?
S5 C17 1.649(2) . ?
S10 C20 1.648(2) . ?
O5 C10 1.428(3) . ?
O5 C11 1.424(3) . ?
O6 C12 1.417(3) . ?
O6 C13 1.421(3) . ?
O4 C8 1.415(3) . ?
O4 C9 1.415(3) . ?
O1 C14 1.417(3) . ?
O1 C3 1.427(3) . ?
N1 H1BD 0.8900 . ?
N1 H1BE 0.8900 . ?
N1 H1BF 0.8900 . ?
N1 H1AA 0.8900 . ?
N1 H1AB 0.8900 . ?
N1 H1AC 0.8900 . ?
N1 C1A 1.590(7) . ?
N1 C1 1.361(9) . ?
O3 C7 1.422(3) . ?
O3 C6 1.426(3) . ?
O2 C4 1.418(3) . ?
O2 C5 1.414(4) . ?
C19 C18 1.352(3) . ?
C15 C16 1.352(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C9 1.492(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C7 1.486(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.494(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C13 1.490(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.467(4) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C5 1.475(4) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C1A H1AD 0.9700 . ?
C1A H1AE 0.9700 . ?
C1A C2A 1.461(9) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.272(13) . ?
Br1B C2A 1.902(6) . ?
Br1 C2 1.791(10) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S2 Ni1 S1 93.34(2) . . ?
S2 Ni1 S6 176.92(3) . . ?
S7 Ni1 S1 176.42(3) . . ?
S7 Ni1 S2 85.43(2) . . ?
S7 Ni1 S6 93.07(2) . . ?
S6 Ni1 S1 88.31(2) . . ?
C15 S1 Ni1 101.70(8) . . ?
C17 S3 C15 97.33(11) . . ?
C20 S9 C19 97.06(11) . . ?
C17 S4 C16 97.24(11) . . ?
C16 S2 Ni1 102.06(8) . . ?
C19 S7 Ni1 102.40(8) . . ?
C18 S6 Ni1 101.78(8) . . ?
C20 S8 C18 97.57(11) . . ?
C11 O5 C10 111.48(19) . . ?
C12 O6 C13 113.5(2) . . ?
C9 O4 C8 114.30(19) . . ?
C14 O1 C3 111.9(2) . . ?
H1BD N1 H1BE 109.5 . . ?
H1BD N1 H1BF 109.5 . . ?
H1BE N1 H1BF 109.5 . . ?
H1AA N1 H1AB 109.5 . . ?
H1AA N1 H1AC 109.5 . . ?
H1AB N1 H1AC 109.5 . . ?
C1A N1 H1BD 109.5 . . ?
C1A N1 H1BE 109.5 . . ?
C1A N1 H1BF 109.5 . . ?
C1 N1 H1AA 109.5 . . ?
C1 N1 H1AB 109.5 . . ?
C1 N1 H1AC 109.5 . . ?
C7 O3 C6 111.4(2) . . ?
C5 O2 C4 113.0(2) . . ?
S7 C19 S9 121.85(14) . . ?
C18 C19 S9 116.85(16) . . ?
C18 C19 S7 121.30(16) . . ?
S1 C15 S3 122.58(14) . . ?
C16 C15 S1 121.52(16) . . ?
C16 C15 S3 115.86(16) . . ?
S2 C16 S4 122.27(14) . . ?
C15 C16 S4 116.34(16) . . ?
C15 C16 S2 121.38(16) . . ?
S6 C18 S8 123.24(14) . . ?
C19 C18 S6 121.43(16) . . ?
C19 C18 S8 115.31(16) . . ?
S9 C20 S8 113.17(12) . . ?
S10 C20 S9 122.75(16) . . ?
S10 C20 S8 124.08(15) . . ?
S3 C17 S4 113.22(11) . . ?
S5 C17 S3 123.92(14) . . ?
S5 C17 S4 122.85(14) . . ?
O5 C10 H10A 109.9 . . ?
O5 C10 H10B 109.9 . . ?
O5 C10 C9 109.0(2) . . ?
H10A C10 H10B 108.3 . . ?
C9 C10 H10A 109.9 . . ?
C9 C10 H10B 109.9 . . ?
O4 C8 H8A 110.0 . . ?
O4 C8 H8B 110.0 . . ?
O4 C8 C7 108.4(2) . . ?
H8A C8 H8B 108.4 . . ?
C7 C8 H8A 110.0 . . ?
C7 C8 H8B 110.0 . . ?
O5 C11 H11A 109.9 . . ?
O5 C11 H11B 109.9 . . ?
O5 C11 C12 109.0(2) . . ?
H11A C11 H11B 108.3 . . ?
C12 C11 H11A 109.9 . . ?
C12 C11 H11B 109.9 . . ?
O6 C12 C11 108.1(2) . . ?
O6 C12 H12A 110.1 . . ?
O6 C12 H12B 110.1 . . ?
C11 C12 H12A 110.1 . . ?
C11 C12 H12B 110.1 . . ?
H12A C12 H12B 108.4 . . ?
O4 C9 C10 108.1(2) . . ?
O4 C9 H9A 110.1 . . ?
O4 C9 H9B 110.1 . . ?
C10 C9 H9A 110.1 . . ?
C10 C9 H9B 110.1 . . ?
H9A C9 H9B 108.4 . . ?
O1 C14 H14A 109.8 . . ?
O1 C14 H14B 109.8 . . ?
O1 C14 C13 109.4(2) . . ?
H14A C14 H14B 108.3 . . ?
C13 C14 H14A 109.8 . . ?
C13 C14 H14B 109.8 . . ?
O1 C3 H3A 109.8 . . ?
O1 C3 H3B 109.8 . . ?
O1 C3 C4 109.5(2) . . ?
H3A C3 H3B 108.2 . . ?
C4 C3 H3A 109.8 . . ?
C4 C3 H3B 109.8 . . ?
O6 C13 C14 107.6(2) . . ?
O6 C13 H13A 110.2 . . ?
O6 C13 H13B 110.2 . . ?
C14 C13 H13A 110.2 . . ?
C14 C13 H13B 110.2 . . ?
H13A C13 H13B 108.5 . . ?
O3 C7 C8 109.1(2) . . ?
O3 C7 H7A 109.9 . . ?
O3 C7 H7B 109.9 . . ?
C8 C7 H7A 109.9 . . ?
C8 C7 H7B 109.9 . . ?
H7A C7 H7B 108.3 . . ?
O2 C4 C3 108.5(2) . . ?
O2 C4 H4A 110.0 . . ?
O2 C4 H4B 110.0 . . ?
C3 C4 H4A 110.0 . . ?
C3 C4 H4B 110.0 . . ?
H4A C4 H4B 108.4 . . ?
O3 C6 H6A 109.7 . . ?
O3 C6 H6B 109.7 . . ?
O3 C6 C5 109.6(3) . . ?
H6A C6 H6B 108.2 . . ?
C5 C6 H6A 109.7 . . ?
C5 C6 H6B 109.7 . . ?
O2 C5 C6 109.6(3) . . ?
O2 C5 H5A 109.8 . . ?
O2 C5 H5B 109.8 . . ?
C6 C5 H5A 109.8 . . ?
C6 C5 H5B 109.8 . . ?
H5A C5 H5B 108.2 . . ?
N1 C1A H1AD 108.6 . . ?
N1 C1A H1AE 108.6 . . ?
H1AD C1A H1AE 107.6 . . ?
C2A C1A N1 114.7(5) . . ?
C2A C1A H1AD 108.6 . . ?
C2A C1A H1AE 108.6 . . ?
N1 C1 H1A 105.1 . . ?
N1 C1 H1B 105.1 . . ?
H1A C1 H1B 105.9 . . ?
C2 C1 N1 128.7(10) . . ?
C2 C1 H1A 105.1 . . ?
C2 C1 H1B 105.1 . . ?
C1 C2 Br1 105.0(11) . . ?
C1 C2 H2A 110.7 . . ?
C1 C2 H2B 110.7 . . ?
Br1 C2 H2A 110.7 . . ?
Br1 C2 H2B 110.7 . . ?
H2A C2 H2B 108.8 . . ?
C1A C2A Br1B 113.0(4) . . ?
C1A C2A H2AA 109.0 . . ?
C1A C2A H2AB 109.0 . . ?
Br1B C2A H2AA 109.0 . . ?
Br1B C2A H2AB 109.0 . . ?
H2AA C2A H2AB 107.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S1 C15 S3 178.51(12) . . . . ?
Ni1 S1 C15 C16 1.1(2) . . . . ?
Ni1 S2 C16 S4 -178.27(12) . . . . ?
Ni1 S2 C16 C15 0.3(2) . . . . ?
Ni1 S7 C19 S9 178.85(12) . . . . ?
Ni1 S7 C19 C18 -1.2(2) . . . . ?
Ni1 S6 C18 S8 178.77(13) . . . . ?
Ni1 S6 C18 C19 0.2(2) . . . . ?
S1 C15 C16 S4 177.67(12) . . . . ?
S1 C15 C16 S2 -0.9(3) . . . . ?
S3 C15 C16 S4 0.1(2) . . . . ?
S3 C15 C16 S2 -178.56(12) . . . . ?
S9 C19 C18 S6 -179.35(12) . . . . ?
S9 C19 C18 S8 2.0(3) . . . . ?
S7 C19 C18 S6 0.7(3) . . . . ?
S7 C19 C18 S8 -177.94(12) . . . . ?
O5 C10 C9 O4 -66.2(3) . . . . ?
O5 C11 C12 O6 63.2(3) . . . . ?
O4 C8 C7 O3 58.0(3) . . . . ?
O1 C14 C13 O6 -65.1(3) . . . . ?
O1 C3 C4 O2 66.0(3) . . . . ?
N1 C1A C2A Br1B 72.2(6) . . . . ?
N1 C1 C2 Br1 -95.2(18) . . . . ?
O3 C6 C5 O2 -63.9(4) . . . . ?
C19 S9 C20 S8 1.28(15) . . . . ?
C19 S9 C20 S10 -178.57(16) . . . . ?
C15 S3 C17 S4 -0.76(15) . . . . ?
C15 S3 C17 S5 179.44(16) . . . . ?
C16 S4 C17 S3 0.79(15) . . . . ?
C16 S4 C17 S5 -179.41(15) . . . . ?
C18 S8 C20 S9 -0.44(15) . . . . ?
C18 S8 C20 S10 179.41(16) . . . . ?
C20 S9 C19 S7 177.93(15) . . . . ?
C20 S9 C19 C18 -2.0(2) . . . . ?
C20 S8 C18 S6 -179.55(16) . . . . ?
C20 S8 C18 C19 -0.9(2) . . . . ?
C17 S3 C15 S1 -177.15(15) . . . . ?
C17 S3 C15 C16 0.4(2) . . . . ?
C17 S4 C16 S2 178.09(15) . . . . ?
C17 S4 C16 C15 -0.5(2) . . . . ?
C10 O5 C11 C12 -178.7(2) . . . . ?
C8 O4 C9 C10 -174.2(2) . . . . ?
C11 O5 C10 C9 -174.3(2) . . . . ?
C12 O6 C13 C14 -169.5(2) . . . . ?
C9 O4 C8 C7 169.4(2) . . . . ?
C14 O1 C3 C4 -179.7(2) . . . . ?
C3 O1 C14 C13 171.1(2) . . . . ?
C13 O6 C12 C11 172.7(2) . . . . ?
C7 O3 C6 C5 -175.3(3) . . . . ?
C4 O2 C5 C6 -170.5(3) . . . . ?
C6 O3 C7 C8 -171.5(2) . . . . ?
C5 O2 C4 C3 171.8(3) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.263
_oxdiff_exptl_absorpt_empirical_full_min 0.460
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_153k
_database_code_depnum_ccdc_archive 'CCDC 2053301'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-18 downloaded from the CCDC.
;
_audit_creation_date             2020-11-10
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C2 H7 Br1 N, C12 H24 O6'
_chemical_formula_sum            'C20 H31 Br N Ni O6 S10'
_chemical_formula_weight         840.68
_chemical_melting_point          ?
_chemical_oxdiff_formula         BrCHNONiS
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.0165(3)
_cell_length_b                   12.0569(4)
_cell_length_c                   13.7786(4)
_cell_angle_alpha                64.116(3)
_cell_angle_beta                 79.239(3)
_cell_angle_gamma                78.965(2)
_cell_volume                     1605.03(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    19221
_cell_measurement_temperature    153
_cell_measurement_theta_max      30.6450
_cell_measurement_theta_min      1.9190
_shelx_estimated_absorpt_T_max   0.842
_shelx_estimated_absorpt_T_min   0.430
_exptl_absorpt_coefficient_mu    2.536
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48119
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             858
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.829
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            39974
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.829
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.032
_diffrn_reflns_theta_min         1.892
_diffrn_ambient_temperature      153
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.829
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -55.00  18.00   0.50    0.82    --    5.18 -32.00 -74.71  146
  2  ω    -64.00  18.00   0.50    0.82    --    5.18 -37.00-120.00  164
  3  ω    -67.00  18.00   0.50    0.82    --    5.18 -31.00  -9.85  170
  4  ω    -64.00  19.00   0.50    0.82    --    5.18 -28.00  51.52  166
  5  ω    -69.00  19.00   0.50    0.82    --    5.18 -28.00 120.27  176
  6  ω    -30.00  19.00   0.50    0.82    --    5.18 -28.00 162.44   98
  7  ω    -17.00  22.00   0.50    0.82    --   -4.95 -99.00  90.00   78
  8  ω    -79.00 -15.00   0.50    0.82    --   -4.95 -19.00   0.00  128
  9  ω    -18.00  26.00   0.50    0.82    --   -4.95 -99.00-120.00   88
 10  ω    -13.00  29.00   0.50    0.82    --   -4.95 -99.00 -60.00   84
 11  ω    -18.00  29.00   0.50    0.82    --   -4.95 -99.00 150.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0304360000
_diffrn_orient_matrix_UB_12      0.0048748000
_diffrn_orient_matrix_UB_13      0.0387711000
_diffrn_orient_matrix_UB_21      -0.0299918000
_diffrn_orient_matrix_UB_22      -0.0495363000
_diffrn_orient_matrix_UB_23      0.0419940000
_diffrn_orient_matrix_UB_31      0.0503669000
_diffrn_orient_matrix_UB_32      -0.0431889000
_diffrn_orient_matrix_UB_33      -0.0072488000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6249
_reflns_number_total             8484
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT n/a (Sheldrick, 2015)'
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         8484
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0337
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0293P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0706
_refine_ls_wR_factor_ref         0.0762
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C2 \\sim C1 \\sim N1: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
C1A \\sim N1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
3. Others
 1*[Sof(Br1)]+1*[Sof(Br1B)]+1*[Sof(Br1A)]=1 with esd of 0.0001
 Sof(H1BD)=Sof(H1BE)=Sof(H1BF)=Sof(C1A)=Sof(H1AD)=Sof(H1AE)=Sof(C2A)=Sof(H2AA)=
 Sof(H2AB)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=
 Sof(H2B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C8(H8A,H8B), C11(H11A,H11B), C12(H12A,H12B), C9(H9A,H9B),
 C14(H14A,H14B), C3(H3A,H3B), C13(H13A,H13B), C7(H7A,H7B), C4(H4A,H4B), C6(H6A,
 H6B), C5(H5A,H5B), C1A(H1AD,H1AE), C1(H1A,H1B), C2(H2A,H2B), C2A(H2AA,H2AB)
4.b Idealised Me refined as rotating group:
 N1(H1BD,H1BE,H1BF), N1(H1AA,H1AB,H1AC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.13808(2) 0.46469(2) 0.88579(2) 0.02045(7) Uani 1 1 d . . . . .
S1 S 0.10452(4) 0.33978(4) 0.82122(4) 0.02213(11) Uani 1 1 d . . . . .
S3 S 0.21006(5) 0.07152(4) 0.87144(4) 0.02250(11) Uani 1 1 d . . . . .
S9 S 0.05871(5) 0.84598(4) 0.92100(4) 0.02396(12) Uani 1 1 d . . . . .
S4 S 0.35760(5) 0.05973(5) 1.02891(4) 0.02322(12) Uani 1 1 d . . . . .
S2 S 0.26773(5) 0.32742(5) 0.99170(5) 0.02522(12) Uani 1 1 d . . . . .
S7 S 0.16571(5) 0.58254(5) 0.95838(5) 0.02531(12) Uani 1 1 d . . . . .
S6 S 0.01375(5) 0.60743(5) 0.77711(5) 0.02695(12) Uani 1 1 d . . . . .
S8 S -0.07477(5) 0.87419(5) 0.74822(5) 0.02984(13) Uani 1 1 d . . . . .
S5 S 0.36413(5) -0.16645(5) 0.99169(5) 0.02966(13) Uani 1 1 d . . . . .
S10 S -0.08432(5) 1.09022(5) 0.80254(5) 0.03369(14) Uani 1 1 d . . . . .
Br1A Br 0.0740(3) 0.1471(4) 0.5319(3) 0.0532(13) Uani 0.1052(14) 1 d . . P A 3
O5 O 0.36500(13) 0.39252(13) 0.62132(12) 0.0281(3) Uani 1 1 d . . . . .
O6 O 0.57665(13) 0.22193(13) 0.62640(12) 0.0279(3) Uani 1 1 d . . . . .
O4 O 0.25689(12) 0.52991(14) 0.42678(13) 0.0307(4) Uani 1 1 d . . . . .
O1 O 0.64584(13) 0.13725(14) 0.46246(12) 0.0284(3) Uani 1 1 d . . . . .
N1 N 0.39617(15) 0.28182(16) 0.47219(16) 0.0286(4) Uani 1 1 d . U . . .
H1BD H 0.350952 0.321740 0.416784 0.034 Uiso 0.821(5) 1 calc R U P B 2
H1BE H 0.474534 0.263811 0.447375 0.034 Uiso 0.821(5) 1 calc R U P B 2
H1BF H 0.394162 0.329847 0.506632 0.034 Uiso 0.821(5) 1 calc R U P B 2
H1AA H 0.397665 0.345045 0.406843 0.034 Uiso 0.179(5) 1 calc R U P B 1
H1AB H 0.473062 0.256819 0.491075 0.034 Uiso 0.179(5) 1 calc R U P B 1
H1AC H 0.347691 0.306084 0.520537 0.034 Uiso 0.179(5) 1 calc R U P B 1
O3 O 0.31496(13) 0.45146(14) 0.26325(13) 0.0350(4) Uani 1 1 d . . . . .
O2 O 0.54373(14) 0.29719(15) 0.26911(13) 0.0377(4) Uani 1 1 d . . . . .
C19 C 0.07382(18) 0.71693(18) 0.89184(17) 0.0225(4) Uani 1 1 d . . . . .
C15 C 0.20023(17) 0.20770(17) 0.88907(17) 0.0204(4) Uani 1 1 d . . . . .
C16 C 0.26964(17) 0.20141(17) 0.96313(16) 0.0200(4) Uani 1 1 d . . . . .
C18 C 0.00857(17) 0.72840(18) 0.81231(17) 0.0227(4) Uani 1 1 d . . . . .
C20 C -0.03589(18) 0.94395(18) 0.82302(18) 0.0247(4) Uani 1 1 d . . . . .
C17 C 0.31286(18) -0.01962(18) 0.96573(17) 0.0215(4) Uani 1 1 d . . . . .
C10 C 0.3073(2) 0.5182(2) 0.59000(19) 0.0317(5) Uani 1 1 d . . . . .
H10A H 0.368300 0.574804 0.547276 0.038 Uiso 1 1 calc R U . . .
H10B H 0.274595 0.533266 0.654165 0.038 Uiso 1 1 calc R U . . .
C8 C 0.16890(19) 0.5591(2) 0.3526(2) 0.0343(5) Uani 1 1 d . . . . .
H8A H 0.118479 0.637608 0.343275 0.041 Uiso 1 1 calc R U . . .
H8B H 0.114244 0.494952 0.380129 0.041 Uiso 1 1 calc R U . . .
C11 C 0.4556(2) 0.3632(2) 0.69344(19) 0.0311(5) Uani 1 1 d . . . . .
H11A H 0.416102 0.373608 0.758548 0.037 Uiso 1 1 calc R U . . .
H11B H 0.518829 0.419006 0.658703 0.037 Uiso 1 1 calc R U . . .
C12 C 0.5142(2) 0.2319(2) 0.72281(18) 0.0315(5) Uani 1 1 d . . . . .
H12A H 0.573022 0.209581 0.774694 0.038 Uiso 1 1 calc R U . . .
H12B H 0.450945 0.175994 0.755572 0.038 Uiso 1 1 calc R U . . .
C9 C 0.2044(2) 0.5401(2) 0.5248(2) 0.0343(5) Uani 1 1 d . . . . .
H9A H 0.146756 0.479196 0.565120 0.041 Uiso 1 1 calc R U . . .
H9B H 0.159055 0.622202 0.509341 0.041 Uiso 1 1 calc R U . . .
C14 C 0.7256(2) 0.1136(2) 0.5420(2) 0.0364(6) Uani 1 1 d . . . . .
H14A H 0.776735 0.180325 0.516455 0.044 Uiso 1 1 calc R U . . .
H14B H 0.780304 0.036601 0.553860 0.044 Uiso 1 1 calc R U . . .
C3 C 0.7140(2) 0.1665(2) 0.35745(19) 0.0327(5) Uani 1 1 d . . . . .
H3A H 0.778049 0.098333 0.359297 0.039 Uiso 1 1 calc R U . . .
H3B H 0.754081 0.240124 0.335632 0.039 Uiso 1 1 calc R U . . .
C13 C 0.6481(2) 0.1044(2) 0.6457(2) 0.0349(5) Uani 1 1 d . . . . .
H13A H 0.593419 0.040805 0.669390 0.042 Uiso 1 1 calc R U . . .
H13B H 0.700980 0.082365 0.701899 0.042 Uiso 1 1 calc R U . . .
C7 C 0.2397(2) 0.5672(2) 0.2470(2) 0.0342(5) Uani 1 1 d . . . . .
H7A H 0.182357 0.585682 0.194810 0.041 Uiso 1 1 calc R U . . .
H7B H 0.292001 0.633360 0.218476 0.041 Uiso 1 1 calc R U . . .
C4 C 0.6274(2) 0.1888(2) 0.2781(2) 0.0366(6) Uani 1 1 d . . . . .
H4A H 0.673842 0.200155 0.207996 0.044 Uiso 1 1 calc R U . . .
H4B H 0.581738 0.118177 0.302912 0.044 Uiso 1 1 calc R U . . .
C6 C 0.3978(2) 0.4595(3) 0.1683(2) 0.0473(7) Uani 1 1 d . . . . .
H6A H 0.456529 0.517264 0.152951 0.057 Uiso 1 1 calc R U . . .
H6B H 0.351091 0.490062 0.106589 0.057 Uiso 1 1 calc R U . . .
C5 C 0.4663(3) 0.3341(3) 0.1857(2) 0.0532(8) Uani 1 1 d . . . . .
H5A H 0.407655 0.274742 0.206602 0.064 Uiso 1 1 calc R U . . .
H5B H 0.516608 0.337101 0.119043 0.064 Uiso 1 1 calc R U . . .
C1A C 0.3429(3) 0.1622(3) 0.5505(3) 0.0301(7) Uani 0.821(5) 1 d . U P B 2
H1AD H 0.355538 0.105979 0.515237 0.036 Uiso 0.821(5) 1 calc R U P B 2
H1AE H 0.388477 0.122802 0.613430 0.036 Uiso 0.821(5) 1 calc R U P B 2
C1 C 0.350(2) 0.184(2) 0.469(3) 0.110(9) Uani 0.179(5) 1 d . U P B 1
H1A H 0.356053 0.113888 0.539053 0.132 Uiso 0.179(5) 1 calc R U P B 1
H1B H 0.402601 0.160569 0.415074 0.132 Uiso 0.179(5) 1 calc R U P B 1
Br1B Br 0.10572(3) 0.22345(4) 0.47314(3) 0.03612(14) Uani 0.8003(14) 1 d . . P
B 2
Br1 Br 0.1161(3) 0.2043(3) 0.5709(3) 0.0588(14) Uani 0.0945(12) 1 d . . P B 1
C2 C 0.2239(14) 0.2070(17) 0.4459(16) 0.060(5) Uani 0.179(5) 1 d . U P B 1
H2A H 0.207920 0.143616 0.426075 0.072 Uiso 0.179(5) 1 calc R U P B 1
H2B H 0.209812 0.287205 0.385410 0.072 Uiso 0.179(5) 1 calc R U P B 1
C2A C 0.2081(3) 0.1816(3) 0.5875(2) 0.0307(8) Uani 0.821(5) 1 d . . P B 2
H2AA H 0.192944 0.248065 0.611648 0.037 Uiso 0.821(5) 1 calc R U P B 2
H2AB H 0.184649 0.106557 0.648859 0.037 Uiso 0.821(5) 1 calc R U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S1 2.1684(5) . ?
Ni1 S2 2.1618(6) . ?
Ni1 S7 2.1523(6) . ?
Ni1 S6 2.1665(6) . ?
S1 C15 1.7167(19) . ?
S3 C15 1.7427(19) . ?
S3 C17 1.733(2) . ?
S9 C19 1.7412(19) . ?
S9 C20 1.722(2) . ?
S4 C16 1.7381(19) . ?
S4 C17 1.727(2) . ?
S2 C16 1.7235(19) . ?
S7 C19 1.707(2) . ?
S6 C18 1.715(2) . ?
S8 C18 1.7442(19) . ?
S8 C20 1.736(2) . ?
S5 C17 1.6495(19) . ?
S10 C20 1.6541(19) . ?
O5 C10 1.431(2) . ?
O5 C11 1.427(3) . ?
O6 C12 1.421(3) . ?
O6 C13 1.422(2) . ?
O4 C8 1.426(3) . ?
O4 C9 1.414(3) . ?
O1 C14 1.430(3) . ?
O1 C3 1.425(3) . ?
N1 H1BD 0.8900 . ?
N1 H1BE 0.8900 . ?
N1 H1BF 0.8900 . ?
N1 H1AA 0.8900 . ?
N1 H1AB 0.8900 . ?
N1 H1AC 0.8900 . ?
N1 C1A 1.522(3) . ?
N1 C1 1.39(2) . ?
O3 C7 1.427(2) . ?
O3 C6 1.425(3) . ?
O2 C4 1.419(3) . ?
O2 C5 1.421(3) . ?
C19 C18 1.364(3) . ?
C15 C16 1.354(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C9 1.490(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C7 1.489(3) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.495(3) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C13 1.492(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.487(3) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C5 1.492(4) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C1A H1AD 0.9700 . ?
C1A H1AE 0.9700 . ?
C1A C2A 1.486(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.43(3) . ?
Br1B C2A 1.940(3) . ?
Br1 C2 1.892(19) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S2 Ni1 S1 93.46(2) . . ?
S2 Ni1 S6 177.68(2) . . ?
S7 Ni1 S1 176.79(3) . . ?
S7 Ni1 S2 85.48(2) . . ?
S7 Ni1 S6 93.19(2) . . ?
S6 Ni1 S1 87.97(2) . . ?
C15 S1 Ni1 101.62(7) . . ?
C17 S3 C15 97.47(9) . . ?
C20 S9 C19 97.18(10) . . ?
C17 S4 C16 97.30(9) . . ?
C16 S2 Ni1 101.85(7) . . ?
C19 S7 Ni1 102.48(7) . . ?
C18 S6 Ni1 101.87(7) . . ?
C20 S8 C18 97.41(10) . . ?
C11 O5 C10 111.24(16) . . ?
C12 O6 C13 113.36(17) . . ?
C9 O4 C8 113.99(16) . . ?
C3 O1 C14 111.37(16) . . ?
H1BD N1 H1BE 109.5 . . ?
H1BD N1 H1BF 109.5 . . ?
H1BE N1 H1BF 109.5 . . ?
H1AA N1 H1AB 109.5 . . ?
H1AA N1 H1AC 109.5 . . ?
H1AB N1 H1AC 109.5 . . ?
C1A N1 H1BD 109.5 . . ?
C1A N1 H1BE 109.5 . . ?
C1A N1 H1BF 109.5 . . ?
C1 N1 H1AA 109.5 . . ?
C1 N1 H1AB 109.5 . . ?
C1 N1 H1AC 109.5 . . ?
C6 O3 C7 111.37(18) . . ?
C4 O2 C5 112.06(18) . . ?
S7 C19 S9 122.17(12) . . ?
C18 C19 S9 116.61(15) . . ?
C18 C19 S7 121.22(15) . . ?
S1 C15 S3 122.49(12) . . ?
C16 C15 S1 121.85(14) . . ?
C16 C15 S3 115.61(14) . . ?
S2 C16 S4 122.17(12) . . ?
C15 C16 S4 116.61(14) . . ?
C15 C16 S2 121.21(14) . . ?
S6 C18 S8 123.45(12) . . ?
C19 C18 S6 121.23(15) . . ?
C19 C18 S8 115.30(15) . . ?
S9 C20 S8 113.42(11) . . ?
S10 C20 S9 123.01(13) . . ?
S10 C20 S8 123.56(13) . . ?
S4 C17 S3 113.01(10) . . ?
S5 C17 S3 123.64(12) . . ?
S5 C17 S4 123.34(12) . . ?
O5 C10 H10A 109.8 . . ?
O5 C10 H10B 109.8 . . ?
O5 C10 C9 109.20(18) . . ?
H10A C10 H10B 108.3 . . ?
C9 C10 H10A 109.8 . . ?
C9 C10 H10B 109.8 . . ?
O4 C8 H8A 110.2 . . ?
O4 C8 H8B 110.2 . . ?
O4 C8 C7 107.77(17) . . ?
H8A C8 H8B 108.5 . . ?
C7 C8 H8A 110.2 . . ?
C7 C8 H8B 110.2 . . ?
O5 C11 H11A 109.8 . . ?
O5 C11 H11B 109.8 . . ?
O5 C11 C12 109.33(18) . . ?
H11A C11 H11B 108.3 . . ?
C12 C11 H11A 109.8 . . ?
C12 C11 H11B 109.8 . . ?
O6 C12 C11 108.17(18) . . ?
O6 C12 H12A 110.1 . . ?
O6 C12 H12B 110.1 . . ?
C11 C12 H12A 110.1 . . ?
C11 C12 H12B 110.1 . . ?
H12A C12 H12B 108.4 . . ?
O4 C9 C10 108.29(17) . . ?
O4 C9 H9A 110.0 . . ?
O4 C9 H9B 110.0 . . ?
C10 C9 H9A 110.0 . . ?
C10 C9 H9B 110.0 . . ?
H9A C9 H9B 108.4 . . ?
O1 C14 H14A 109.8 . . ?
O1 C14 H14B 109.8 . . ?
O1 C14 C13 109.22(18) . . ?
H14A C14 H14B 108.3 . . ?
C13 C14 H14A 109.8 . . ?
C13 C14 H14B 109.8 . . ?
O1 C3 H3A 109.8 . . ?
O1 C3 H3B 109.8 . . ?
O1 C3 C4 109.32(18) . . ?
H3A C3 H3B 108.3 . . ?
C4 C3 H3A 109.8 . . ?
C4 C3 H3B 109.8 . . ?
O6 C13 C14 107.86(19) . . ?
O6 C13 H13A 110.1 . . ?
O6 C13 H13B 110.1 . . ?
C14 C13 H13A 110.1 . . ?
C14 C13 H13B 110.1 . . ?
H13A C13 H13B 108.4 . . ?
O3 C7 C8 109.07(19) . . ?
O3 C7 H7A 109.9 . . ?
O3 C7 H7B 109.9 . . ?
C8 C7 H7A 109.9 . . ?
C8 C7 H7B 109.9 . . ?
H7A C7 H7B 108.3 . . ?
O2 C4 C3 108.02(18) . . ?
O2 C4 H4A 110.1 . . ?
O2 C4 H4B 110.1 . . ?
C3 C4 H4A 110.1 . . ?
C3 C4 H4B 110.1 . . ?
H4A C4 H4B 108.4 . . ?
O3 C6 H6A 109.8 . . ?
O3 C6 H6B 109.8 . . ?
O3 C6 C5 109.5(2) . . ?
H6A C6 H6B 108.2 . . ?
C5 C6 H6A 109.8 . . ?
C5 C6 H6B 109.8 . . ?
O2 C5 C6 108.6(2) . . ?
O2 C5 H5A 110.0 . . ?
O2 C5 H5B 110.0 . . ?
C6 C5 H5A 110.0 . . ?
C6 C5 H5B 110.0 . . ?
H5A C5 H5B 108.3 . . ?
N1 C1A H1AD 108.9 . . ?
N1 C1A H1AE 108.9 . . ?
H1AD C1A H1AE 107.7 . . ?
C2A C1A N1 113.5(2) . . ?
C2A C1A H1AD 108.9 . . ?
C2A C1A H1AE 108.9 . . ?
N1 C1 H1A 108.1 . . ?
N1 C1 H1B 108.1 . . ?
N1 C1 C2 117(2) . . ?
H1A C1 H1B 107.3 . . ?
C2 C1 H1A 108.1 . . ?
C2 C1 H1B 108.1 . . ?
C1 C2 Br1 108.6(18) . . ?
C1 C2 H2A 110.0 . . ?
C1 C2 H2B 110.0 . . ?
Br1 C2 H2A 110.0 . . ?
Br1 C2 H2B 110.0 . . ?
H2A C2 H2B 108.3 . . ?
C1A C2A Br1B 111.9(2) . . ?
C1A C2A H2AA 109.2 . . ?
C1A C2A H2AB 109.2 . . ?
Br1B C2A H2AA 109.2 . . ?
Br1B C2A H2AB 109.2 . . ?
H2AA C2A H2AB 107.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S1 C15 S3 178.70(11) . . . . ?
Ni1 S1 C15 C16 1.27(18) . . . . ?
Ni1 S2 C16 S4 -178.42(10) . . . . ?
Ni1 S2 C16 C15 0.36(18) . . . . ?
Ni1 S7 C19 S9 178.85(11) . . . . ?
Ni1 S7 C19 C18 -1.40(19) . . . . ?
Ni1 S6 C18 S8 177.88(11) . . . . ?
Ni1 S6 C18 C19 -0.18(19) . . . . ?
S1 C15 C16 S4 177.67(11) . . . . ?
S1 C15 C16 S2 -1.2(3) . . . . ?
S3 C15 C16 S4 0.1(2) . . . . ?
S3 C15 C16 S2 -178.77(11) . . . . ?
S9 C19 C18 S6 -179.10(11) . . . . ?
S9 C19 C18 S8 2.7(2) . . . . ?
S7 C19 C18 S6 1.1(3) . . . . ?
S7 C19 C18 S8 -177.08(11) . . . . ?
O5 C10 C9 O4 -65.5(2) . . . . ?
O5 C11 C12 O6 62.6(2) . . . . ?
O4 C8 C7 O3 58.6(2) . . . . ?
O1 C14 C13 O6 -63.9(2) . . . . ?
O1 C3 C4 O2 65.7(2) . . . . ?
N1 C1A C2A Br1B 72.0(3) . . . . ?
N1 C1 C2 Br1 -75(3) . . . . ?
O3 C6 C5 O2 -65.4(3) . . . . ?
C19 S9 C20 S8 1.86(13) . . . . ?
C19 S9 C20 S10 -178.02(14) . . . . ?
C15 S3 C17 S4 -0.69(13) . . . . ?
C15 S3 C17 S5 179.96(13) . . . . ?
C16 S4 C17 S3 0.72(13) . . . . ?
C16 S4 C17 S5 -179.93(13) . . . . ?
C18 S8 C20 S9 -0.72(13) . . . . ?
C18 S8 C20 S10 179.16(14) . . . . ?
C20 S9 C19 S7 176.98(13) . . . . ?
C20 S9 C19 C18 -2.78(18) . . . . ?
C20 S8 C18 S6 -179.33(14) . . . . ?
C20 S8 C18 C19 -1.17(18) . . . . ?
C17 S3 C15 S1 -177.20(13) . . . . ?
C17 S3 C15 C16 0.38(17) . . . . ?
C17 S4 C16 S2 178.35(13) . . . . ?
C17 S4 C16 C15 -0.49(18) . . . . ?
C10 O5 C11 C12 -179.33(17) . . . . ?
C8 O4 C9 C10 -175.09(18) . . . . ?
C11 O5 C10 C9 -173.88(17) . . . . ?
C12 O6 C13 C14 -170.12(18) . . . . ?
C9 O4 C8 C7 169.74(19) . . . . ?
C14 O1 C3 C4 179.32(18) . . . . ?
C3 O1 C14 C13 170.67(18) . . . . ?
C13 O6 C12 C11 173.31(18) . . . . ?
C7 O3 C6 C5 -175.0(2) . . . . ?
C4 O2 C5 C6 -170.1(2) . . . . ?
C6 O3 C7 C8 -171.7(2) . . . . ?
C5 O2 C4 C3 173.3(2) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.216
_oxdiff_exptl_absorpt_empirical_full_min 0.497
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_113k
_database_code_depnum_ccdc_archive 'CCDC 2053299'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-18 downloaded from the CCDC.
;
_audit_creation_date             2020-11-10
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C2 H7 Br1 N, C12 H24 O6'
_chemical_formula_sum            'C20 H29 Br N Ni O6 S10'
_chemical_formula_weight         838.66
_chemical_melting_point          ?
_chemical_oxdiff_formula         BrCHNONiS
_chemical_oxdiff_usercomment     223K
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.9810(3)
_cell_length_b                   12.0448(3)
_cell_length_c                   13.7409(4)
_cell_angle_alpha                115.825(3)
_cell_angle_beta                 91.535(2)
_cell_angle_gamma                100.927(2)
_cell_volume                     1593.91(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    20361
_cell_measurement_temperature    113
_cell_measurement_theta_max      30.9380
_cell_measurement_theta_min      1.9240
_shelx_estimated_absorpt_T_max   0.784
_shelx_estimated_absorpt_T_min   0.629
_exptl_absorpt_coefficient_mu    2.554
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58143
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             854
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_unetI/netI     0.0483
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.823
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            38281
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.823
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.043
_diffrn_reflns_theta_min         1.896
_diffrn_ambient_temperature      113
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.823
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -44.00  17.00   0.50    0.68    --    5.18 -22.00  55.21  122
  2  ω    -63.00  19.00   0.50    0.68    --    5.18 -28.00 121.78  164
  3  ω    -64.00  19.00   0.50    0.68    --    5.18 -20.00  -2.46  166
  4  ω    -70.00  18.00   0.50    0.68    --    5.18 -30.00 -65.58  176
  5  ω    -26.00  18.00   0.50    0.68    --    5.18 -19.00-150.00   88
  6  ω    -58.00  19.00   0.50    0.68    --    5.18 -28.00-175.10  154
  7  ω    -62.00 -34.00   0.50    0.68    --    5.18 -19.00-150.00   56
  8  ω    -15.00  27.00   0.50    0.68    --   -4.95 -99.00 120.00   84
  9  ω    -18.00  28.00   0.50    0.68    --   -4.95 -99.00  30.00   92
 10  ω    -13.00  24.00   0.50    0.68    --   -4.95 -99.00 -60.00   74
 11  ω    -18.00  26.00   0.50    0.68    --   -4.95 -99.00-120.00   88
 12  ω    -14.00  29.00   0.50    0.68    --   -4.95 -99.00-180.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0310094000
_diffrn_orient_matrix_UB_12      -0.0436313000
_diffrn_orient_matrix_UB_13      -0.0380035000
_diffrn_orient_matrix_UB_21      -0.0300922000
_diffrn_orient_matrix_UB_22      0.0064974000
_diffrn_orient_matrix_UB_23      -0.0429436000
_diffrn_orient_matrix_UB_31      0.0502791000
_diffrn_orient_matrix_UB_32      0.0505919000
_diffrn_orient_matrix_UB_33      0.0071668000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6461
_reflns_number_total             8378
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         8378
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0315
_refine_ls_restrained_S_all      1.015
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0321P)²+0.0488P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0726
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
N1 \\sim C1A \\sim C2A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.01 within 2A
3. Others
 1*[Sof(Br1B)]+1*[Sof(Br1A)]+1*[Sof(Br1)]=1 with esd of 0.0001
 Sof(H1BD)=Sof(H1BE)=Sof(H1BF)=Sof(C2A)=Sof(H2A1)=Sof(H2A2)=Sof(C1A)=Sof(H1AD)=
 Sof(H1AE)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C1)=Sof(H1A)=
 Sof(H1B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C3(H3A,H3B), C12(H12A,H12B), C8(H8A,H8B), C9(H9A,H9B),
 C33(H33A,H33B), C32(H32A,H32B), C10(H10A,H10B), C7(H7A,H7B), C4(H4A,H4B),
 C2(H2A,H2B), C6(H6A,H6B), C5(H5A,H5B), C1(H1A,H1B), C2A(H2A1,H2A2), C1A(H1AD,
 H1AE)
4.b Idealised Me refined as rotating group:
 N1(H1AA,H1AB,H1AC), N1(H1BD,H1BE,H1BF)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.86093(2) 0.85079(2) 0.88634(2) 0.01526(7) Uani 1 1 d . . . . .
Br1B Br 0.10538(2) 0.80453(2) 0.52733(3) 0.02716(11) Uani 0.9269(14) 1 d . . P
A 1
S1 S 0.89458(5) 0.66151(5) 0.82181(4) 0.01683(11) Uani 1 1 d . . . . .
S2 S 0.73170(5) 0.81942(5) 0.99250(4) 0.01913(11) Uani 1 1 d . . . . .
S3 S 0.78939(5) 0.44329(4) 0.87218(4) 0.01687(11) Uani 1 1 d . . . . .
S4 S 0.64198(5) 0.58851(4) 1.02980(4) 0.01688(11) Uani 1 1 d . . . . .
S7 S 0.83315(5) 1.04105(5) 0.95847(4) 0.01888(11) Uani 1 1 d . . . . .
S5 S 0.63550(5) 0.32460(5) 0.99190(5) 0.02171(12) Uani 1 1 d . . . . .
S9 S 0.94047(5) 1.26717(5) 0.92117(4) 0.01777(11) Uani 1 1 d . . . . .
S8 S 1.07415(5) 1.12281(5) 0.74857(5) 0.02215(12) Uani 1 1 d . . . . .
S6 S 0.98598(5) 0.88524(5) 0.77826(4) 0.02035(12) Uani 1 1 d . . . . .
S10 S 1.08308(5) 1.39300(5) 0.80198(5) 0.02402(13) Uani 1 1 d . . . . .
O6 O 0.57794(13) 0.65139(13) 0.37300(12) 0.0207(3) Uani 1 1 d . . . . .
O5 O 0.36598(13) 0.48505(13) 0.37810(12) 0.0211(3) Uani 1 1 d . . . . .
O1 O 0.64547(13) 0.89991(13) 0.53632(12) 0.0214(3) Uani 1 1 d . . . . .
O4 O 0.25677(13) 0.54192(14) 0.57159(12) 0.0237(3) Uani 1 1 d . . . . .
O2 O 0.54356(14) 0.93376(14) 0.73017(12) 0.0262(3) Uani 1 1 d . . . . .
O3 O 0.31348(13) 0.78444(14) 0.73434(13) 0.0255(3) Uani 1 1 d . . . . .
N1 N 0.39537(15) 0.74463(16) 0.52498(15) 0.0198(4) Uani 1 1 d . U . . .
H1AA H 0.391196 0.659943 0.489468 0.024 Uiso 0.946(4) 1 calc R U P B 1
H1AB H 0.350429 0.761596 0.582490 0.024 Uiso 0.946(4) 1 calc R U P B 1
H1AC H 0.476504 0.786711 0.549482 0.024 Uiso 0.946(4) 1 calc R U P B 1
H1BD H 0.330697 0.677747 0.485757 0.024 Uiso 0.054(4) 1 calc R U P B 2
H1BE H 0.411811 0.748901 0.591942 0.024 Uiso 0.054(4) 1 calc R U P B 2
H1BF H 0.464370 0.734484 0.489635 0.024 Uiso 0.054(4) 1 calc R U P B 2
C13 C 0.79912(18) 0.59703(17) 0.88978(16) 0.0151(4) Uani 1 1 d . . . . .
C15 C 0.68680(17) 0.44602(18) 0.96641(16) 0.0157(4) Uani 1 1 d . . . . .
C14 C 0.72955(17) 0.66506(18) 0.96392(16) 0.0159(4) Uani 1 1 d . . . . .
C17 C 0.92599(18) 1.10921(18) 0.89206(17) 0.0165(4) Uani 1 1 d . . . . .
C18 C 1.03491(18) 1.26714(19) 0.82272(18) 0.0190(4) Uani 1 1 d . . . . .
C11 C 0.4567(2) 0.4418(2) 0.30602(18) 0.0228(5) Uani 1 1 d . . . . .
H11A H 0.416049 0.364685 0.239443 0.027 Uiso 1 1 calc R U . . .
H11B H 0.521673 0.420550 0.342012 0.027 Uiso 1 1 calc R U . . .
C16 C 0.99143(18) 1.04131(19) 0.81351(17) 0.0185(4) Uani 1 1 d . . . . .
C3 C 0.7142(2) 0.9772(2) 0.64213(18) 0.0244(5) Uani 1 1 d . . . . .
H3A H 0.779018 1.045262 0.640065 0.029 Uiso 1 1 calc R U . . .
H3B H 0.756319 0.925300 0.665313 0.029 Uiso 1 1 calc R U . . .
C12 C 0.5157(2) 0.5443(2) 0.27613(17) 0.0220(5) Uani 1 1 d . . . . .
H12A H 0.576180 0.514275 0.223726 0.026 Uiso 1 1 calc R U . . .
H12B H 0.450755 0.567239 0.241658 0.026 Uiso 1 1 calc R U . . .
C8 C 0.16776(19) 0.5867(2) 0.64490(19) 0.0259(5) Uani 1 1 d . . . . .
H8A H 0.116233 0.516050 0.654459 0.031 Uiso 1 1 calc R U . . .
H8B H 0.111710 0.623480 0.615773 0.031 Uiso 1 1 calc R U . . .
C9 C 0.2045(2) 0.4323(2) 0.47332(19) 0.0261(5) Uani 1 1 d . . . . .
H9A H 0.144883 0.451915 0.430999 0.031 Uiso 1 1 calc R U . . .
H9B H 0.158949 0.364412 0.489670 0.031 Uiso 1 1 calc R U . . .
C33 C 0.7258(2) 0.8458(2) 0.45710(19) 0.0255(5) Uani 1 1 d . . . . .
H33A H 0.779825 0.805222 0.483748 0.031 Uiso 1 1 calc R U . . .
H33B H 0.780081 0.912915 0.444741 0.031 Uiso 1 1 calc R U . . .
C32 C 0.6482(2) 0.7496(2) 0.35283(19) 0.0249(5) Uani 1 1 d . . . . .
H32A H 0.591328 0.788951 0.327457 0.030 Uiso 1 1 calc R U . . .
H32B H 0.702650 0.714983 0.295824 0.030 Uiso 1 1 calc R U . . .
C10 C 0.3087(2) 0.3902(2) 0.40942(19) 0.0244(5) Uani 1 1 d . . . . .
H10A H 0.371284 0.376960 0.454111 0.029 Uiso 1 1 calc R U . . .
H10B H 0.275986 0.309099 0.343709 0.029 Uiso 1 1 calc R U . . .
C7 C 0.2387(2) 0.6850(2) 0.75133(19) 0.0273(5) Uani 1 1 d . . . . .
H7A H 0.179814 0.719178 0.804192 0.033 Uiso 1 1 calc R U . . .
H7B H 0.292719 0.647276 0.781228 0.033 Uiso 1 1 calc R U . . .
C4 C 0.6267(2) 1.0333(2) 0.72079(19) 0.0263(5) Uani 1 1 d . . . . .
H4A H 0.674012 1.094044 0.792712 0.032 Uiso 1 1 calc R U . . .
H4B H 0.579187 1.079189 0.694566 0.032 Uiso 1 1 calc R U . . .
C2 C 0.2061(2) 0.7292(2) 0.41166(19) 0.0228(5) Uani 0.946(4) 1 d . . P A 1
H2A H 0.190526 0.636978 0.388321 0.027 Uiso 0.946(4) 1 calc R U P B 1
H2B H 0.180956 0.741832 0.348148 0.027 Uiso 0.946(4) 1 calc R U P B 1
C6 C 0.3967(2) 0.8718(2) 0.83012(19) 0.0333(6) Uani 1 1 d . . . . .
H6A H 0.456914 0.828744 0.846495 0.040 Uiso 1 1 calc R U . . .
H6B H 0.348794 0.903545 0.892884 0.040 Uiso 1 1 calc R U . . .
C5 C 0.4656(2) 0.9800(2) 0.8128(2) 0.0374(6) Uani 1 1 d . . . . .
H5A H 0.405525 1.018975 0.790510 0.045 Uiso 1 1 calc R U . . .
H5B H 0.516846 1.045295 0.881286 0.045 Uiso 1 1 calc R U . . .
C1 C 0.3428(2) 0.7867(2) 0.44873(19) 0.0214(5) Uani 0.946(4) 1 d . . P A 1
H1A H 0.388862 0.763320 0.384264 0.026 Uiso 0.946(4) 1 calc R U P B 1
H1B H 0.355683 0.880011 0.485445 0.026 Uiso 0.946(4) 1 calc R U P B 1
Br1A Br 0.0726(10) 0.8249(12) 0.4704(13) 0.067(5) Uani 0.0346(15) 1 d . . P C 3
C2A C 0.218(3) 0.848(4) 0.555(3) 0.023(7) Uani 0.054(4) 1 d . U P B 2
H2A1 H 0.190154 0.928558 0.577746 0.028 Uiso 0.054(4) 1 calc R U P B 2
H2A2 H 0.207449 0.822074 0.613570 0.028 Uiso 0.054(4) 1 calc R U P B 2
Br1 Br 0.1172(9) 0.7252(10) 0.4290(10) 0.069(4) Uani 0.0384(12) 1 d . . P B 2
C1A C 0.359(4) 0.871(4) 0.538(4) 0.028(6) Uani 0.054(4) 1 d . U P B 2
H1AD H 0.371395 0.883245 0.472225 0.034 Uiso 0.054(4) 1 calc R U P B 2
H1AE H 0.409594 0.945030 0.602176 0.034 Uiso 0.054(4) 1 calc R U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S1 2.1671(6) . ?
Ni1 S2 2.1616(5) . ?
Ni1 S7 2.1516(6) . ?
Ni1 S6 2.1664(6) . ?
Br1B C2 1.947(3) . ?
S1 C13 1.7175(19) . ?
S2 C14 1.720(2) . ?
S3 C13 1.7415(19) . ?
S3 C15 1.733(2) . ?
S4 C15 1.728(2) . ?
S4 C14 1.7412(19) . ?
S7 C17 1.712(2) . ?
S5 C15 1.6502(19) . ?
S9 C17 1.739(2) . ?
S9 C18 1.726(2) . ?
S8 C18 1.735(2) . ?
S8 C16 1.747(2) . ?
S6 C16 1.713(2) . ?
S10 C18 1.655(2) . ?
O6 C12 1.423(2) . ?
O6 C32 1.423(2) . ?
O5 C11 1.430(3) . ?
O5 C10 1.434(2) . ?
O1 C3 1.430(3) . ?
O1 C33 1.428(3) . ?
O4 C8 1.428(3) . ?
O4 C9 1.419(3) . ?
O2 C4 1.419(2) . ?
O2 C5 1.419(3) . ?
O3 C7 1.430(2) . ?
O3 C6 1.428(3) . ?
N1 H1AA 0.9100 . ?
N1 H1AB 0.9100 . ?
N1 H1AC 0.9100 . ?
N1 H1BD 0.9100 . ?
N1 H1BE 0.9100 . ?
N1 H1BF 0.9100 . ?
N1 C1 1.493(3) . ?
N1 C1A 1.58(4) . ?
C13 C14 1.358(3) . ?
C17 C16 1.358(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.505(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.488(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C7 1.493(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.491(3) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C32 1.495(3) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C1 1.500(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C5 1.495(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2A H2A1 0.9900 . ?
C2A H2A2 0.9900 . ?
C2A Br1 1.86(4) . ?
C2A C1A 1.57(5) . ?
C1A H1AD 0.9900 . ?
C1A H1AE 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S2 Ni1 S1 93.53(2) . . ?
S2 Ni1 S6 178.02(2) . . ?
S7 Ni1 S1 176.94(2) . . ?
S7 Ni1 S2 85.51(2) . . ?
S7 Ni1 S6 93.17(2) . . ?
S6 Ni1 S1 87.86(2) . . ?
C13 S1 Ni1 101.63(7) . . ?
C14 S2 Ni1 101.86(7) . . ?
C15 S3 C13 97.54(10) . . ?
C15 S4 C14 97.38(10) . . ?
C17 S7 Ni1 102.42(7) . . ?
C18 S9 C17 96.98(10) . . ?
C18 S8 C16 97.42(10) . . ?
C16 S6 Ni1 101.85(7) . . ?
C32 O6 C12 112.97(16) . . ?
C11 O5 C10 110.82(16) . . ?
C33 O1 C3 111.37(16) . . ?
C9 O4 C8 113.86(16) . . ?
C5 O2 C4 111.98(17) . . ?
C6 O3 C7 110.93(17) . . ?
H1AA N1 H1AB 109.5 . . ?
H1AA N1 H1AC 109.5 . . ?
H1AB N1 H1AC 109.5 . . ?
H1BD N1 H1BE 109.5 . . ?
H1BD N1 H1BF 109.5 . . ?
H1BE N1 H1BF 109.5 . . ?
C1 N1 H1AA 109.5 . . ?
C1 N1 H1AB 109.5 . . ?
C1 N1 H1AC 109.5 . . ?
C1A N1 H1BD 109.5 . . ?
C1A N1 H1BE 109.5 . . ?
C1A N1 H1BF 109.5 . . ?
S1 C13 S3 122.52(12) . . ?
C14 C13 S1 121.69(15) . . ?
C14 C13 S3 115.75(14) . . ?
S4 C15 S3 113.02(10) . . ?
S5 C15 S3 123.57(12) . . ?
S5 C15 S4 123.40(12) . . ?
S2 C14 S4 122.39(12) . . ?
C13 C14 S2 121.29(14) . . ?
C13 C14 S4 116.31(15) . . ?
S7 C17 S9 121.89(13) . . ?
C16 C17 S7 121.07(15) . . ?
C16 C17 S9 117.04(15) . . ?
S9 C18 S8 113.35(11) . . ?
S10 C18 S9 122.99(13) . . ?
S10 C18 S8 123.66(13) . . ?
O5 C11 H11A 109.8 . . ?
O5 C11 H11B 109.8 . . ?
O5 C11 C12 109.22(17) . . ?
H11A C11 H11B 108.3 . . ?
C12 C11 H11A 109.8 . . ?
C12 C11 H11B 109.8 . . ?
S6 C16 S8 123.35(13) . . ?
C17 C16 S8 115.11(15) . . ?
C17 C16 S6 121.48(15) . . ?
O1 C3 H3A 109.9 . . ?
O1 C3 H3B 109.9 . . ?
O1 C3 C4 109.12(17) . . ?
H3A C3 H3B 108.3 . . ?
C4 C3 H3A 109.9 . . ?
C4 C3 H3B 109.9 . . ?
O6 C12 C11 108.22(17) . . ?
O6 C12 H12A 110.1 . . ?
O6 C12 H12B 110.1 . . ?
C11 C12 H12A 110.1 . . ?
C11 C12 H12B 110.1 . . ?
H12A C12 H12B 108.4 . . ?
O4 C8 H8A 110.2 . . ?
O4 C8 H8B 110.2 . . ?
O4 C8 C7 107.60(17) . . ?
H8A C8 H8B 108.5 . . ?
C7 C8 H8A 110.2 . . ?
C7 C8 H8B 110.2 . . ?
O4 C9 H9A 110.1 . . ?
O4 C9 H9B 110.1 . . ?
O4 C9 C10 107.99(17) . . ?
H9A C9 H9B 108.4 . . ?
C10 C9 H9A 110.1 . . ?
C10 C9 H9B 110.1 . . ?
O1 C33 H33A 109.8 . . ?
O1 C33 H33B 109.8 . . ?
O1 C33 C32 109.29(17) . . ?
H33A C33 H33B 108.3 . . ?
C32 C33 H33A 109.8 . . ?
C32 C33 H33B 109.8 . . ?
O6 C32 C33 107.75(17) . . ?
O6 C32 H32A 110.2 . . ?
O6 C32 H32B 110.2 . . ?
C33 C32 H32A 110.2 . . ?
C33 C32 H32B 110.2 . . ?
H32A C32 H32B 108.5 . . ?
O5 C10 C9 109.17(18) . . ?
O5 C10 H10A 109.8 . . ?
O5 C10 H10B 109.8 . . ?
C9 C10 H10A 109.8 . . ?
C9 C10 H10B 109.8 . . ?
H10A C10 H10B 108.3 . . ?
O3 C7 C8 108.75(18) . . ?
O3 C7 H7A 109.9 . . ?
O3 C7 H7B 109.9 . . ?
C8 C7 H7A 109.9 . . ?
C8 C7 H7B 109.9 . . ?
H7A C7 H7B 108.3 . . ?
O2 C4 C3 108.23(18) . . ?
O2 C4 H4A 110.1 . . ?
O2 C4 H4B 110.1 . . ?
C3 C4 H4A 110.1 . . ?
C3 C4 H4B 110.1 . . ?
H4A C4 H4B 108.4 . . ?
Br1B C2 H2A 109.4 . . ?
Br1B C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
C1 C2 Br1B 111.39(16) . . ?
C1 C2 H2A 109.4 . . ?
C1 C2 H2B 109.4 . . ?
O3 C6 H6A 109.8 . . ?
O3 C6 H6B 109.8 . . ?
O3 C6 C5 109.5(2) . . ?
H6A C6 H6B 108.2 . . ?
C5 C6 H6A 109.8 . . ?
C5 C6 H6B 109.8 . . ?
O2 C5 C6 108.6(2) . . ?
O2 C5 H5A 110.0 . . ?
O2 C5 H5B 110.0 . . ?
C6 C5 H5A 110.0 . . ?
C6 C5 H5B 110.0 . . ?
H5A C5 H5B 108.4 . . ?
N1 C1 C2 112.69(17) . . ?
N1 C1 H1A 109.1 . . ?
N1 C1 H1B 109.1 . . ?
C2 C1 H1A 109.1 . . ?
C2 C1 H1B 109.1 . . ?
H1A C1 H1B 107.8 . . ?
H2A1 C2A H2A2 107.8 . . ?
Br1 C2A H2A1 109.1 . . ?
Br1 C2A H2A2 109.1 . . ?
C1A C2A H2A1 109.1 . . ?
C1A C2A H2A2 109.1 . . ?
C1A C2A Br1 112(3) . . ?
N1 C1A C2A 103(3) . . ?
N1 C1A H1AD 111.2 . . ?
N1 C1A H1AE 111.2 . . ?
C2A C1A H1AD 111.2 . . ?
C2A C1A H1AE 111.2 . . ?
H1AD C1A H1AE 109.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S1 C13 S3 -178.75(10) . . . . ?
Ni1 S1 C13 C14 -1.14(18) . . . . ?
Ni1 S2 C14 S4 178.35(10) . . . . ?
Ni1 S2 C14 C13 -0.10(18) . . . . ?
Ni1 S7 C17 S9 -179.02(10) . . . . ?
Ni1 S7 C17 C16 1.27(18) . . . . ?
Ni1 S6 C16 S8 -177.13(11) . . . . ?
Ni1 S6 C16 C17 -0.09(19) . . . . ?
Br1B C2 C1 N1 73.4(2) . . . . ?
S1 C13 C14 S2 0.9(2) . . . . ?
S1 C13 C14 S4 -177.65(10) . . . . ?
S3 C13 C14 S2 178.65(10) . . . . ?
S3 C13 C14 S4 0.1(2) . . . . ?
S7 C17 C16 S8 176.42(11) . . . . ?
S7 C17 C16 S6 -0.8(3) . . . . ?
S9 C17 C16 S8 -3.3(2) . . . . ?
S9 C17 C16 S6 179.44(11) . . . . ?
O5 C11 C12 O6 62.1(2) . . . . ?
O1 C3 C4 O2 65.6(2) . . . . ?
O1 C33 C32 O6 -63.2(2) . . . . ?
O4 C8 C7 O3 58.9(2) . . . . ?
O4 C9 C10 O5 -65.0(2) . . . . ?
O3 C6 C5 O2 -65.5(3) . . . . ?
C13 S3 C15 S4 0.64(12) . . . . ?
C13 S3 C15 S5 179.83(13) . . . . ?
C15 S3 C13 S1 177.28(13) . . . . ?
C15 S3 C13 C14 -0.46(17) . . . . ?
C15 S4 C14 S2 -178.22(12) . . . . ?
C15 S4 C14 C13 0.30(17) . . . . ?
C14 S4 C15 S3 -0.59(12) . . . . ?
C14 S4 C15 S5 -179.78(13) . . . . ?
C17 S9 C18 S8 -2.05(13) . . . . ?
C17 S9 C18 S10 178.10(13) . . . . ?
C18 S9 C17 S7 -176.45(13) . . . . ?
C18 S9 C17 C16 3.27(18) . . . . ?
C18 S8 C16 S6 178.77(13) . . . . ?
C18 S8 C16 C17 1.56(18) . . . . ?
C11 O5 C10 C9 -173.24(17) . . . . ?
C16 S8 C18 S9 0.65(13) . . . . ?
C16 S8 C18 S10 -179.50(14) . . . . ?
C3 O1 C33 C32 170.57(17) . . . . ?
C12 O6 C32 C33 -170.41(17) . . . . ?
C8 O4 C9 C10 -175.30(17) . . . . ?
C9 O4 C8 C7 169.27(17) . . . . ?
C33 O1 C3 C4 178.73(17) . . . . ?
C32 O6 C12 C11 173.84(17) . . . . ?
C10 O5 C11 C12 -179.33(16) . . . . ?
C7 O3 C6 C5 -175.2(2) . . . . ?
C4 O2 C5 C6 -170.7(2) . . . . ?
C6 O3 C7 C8 -171.55(19) . . . . ?
C5 O2 C4 C3 173.44(19) . . . . ?
Br1 C2A C1A N1 -70(3) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.997
_oxdiff_exptl_absorpt_empirical_full_min 0.588
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_253k
_database_code_depnum_ccdc_archive 'CCDC 2053306'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-18 downloaded from the CCDC.
;
_audit_creation_date             2020-11-10
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C2 H7 Br1 N, C12 H24 O6'
_chemical_formula_sum            'C20 H31 Br N Ni O6 S10'
_chemical_formula_weight         840.68
_chemical_melting_point          ?
_chemical_oxdiff_formula         BrCHNONiS
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.0864(3)
_cell_length_b                   12.0734(3)
_cell_length_c                   13.7103(4)
_cell_angle_alpha                65.253(3)
_cell_angle_beta                 80.773(3)
_cell_angle_gamma                78.660(2)
_cell_volume                     1627.77(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    14525
_cell_measurement_temperature    253
_cell_measurement_theta_max      31.0070
_cell_measurement_theta_min      1.9100
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.501
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67852
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             858
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0640
_diffrn_reflns_av_unetI/netI     0.0568
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.828
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            42066
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.828
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.080
_diffrn_reflns_theta_min         1.877
_diffrn_ambient_temperature      253
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.828
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -60.00  19.00   0.50    1.11    --    5.18 -28.00   5.69  158
  2  ω    -64.00  18.00   0.50    1.11    --    5.18 -32.00 130.25  164
  3  ω    -69.00  19.00   0.50    1.11    --    5.18 -28.00  51.55  176
  4  ω    -67.00  18.00   0.50    1.11    --    5.18 -37.00 -60.00  170
  5  ω    -45.00  18.00   0.50    1.11    --    5.18 -19.00-120.00  126
  6  ω    -49.00  18.00   0.50    1.11    --    5.18 -37.00-180.00  134
  7  ω    -78.00 -45.00   0.50    1.11    --   -4.95 -37.00 -90.00   66
  8  ω    -33.00   1.00   0.50    1.11    --   -4.95 -37.00 -90.00   68
  9  ω    -18.00  29.00   0.50    1.11    --   -4.95 -99.00-180.00   94
 10  ω    -12.00  39.00   0.50    1.11    --    5.18 -99.00-120.00  102
 11  ω    -18.00  29.00   0.50    1.11    --   -4.95 -99.00   0.00   94
 12  ω    -18.00  27.00   0.50    1.11    --   -4.95 -99.00 120.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0292408000
_diffrn_orient_matrix_UB_12      0.0032563000
_diffrn_orient_matrix_UB_13      0.0409154000
_diffrn_orient_matrix_UB_21      -0.0297340000
_diffrn_orient_matrix_UB_22      -0.0491044000
_diffrn_orient_matrix_UB_23      0.0393289000
_diffrn_orient_matrix_UB_31      0.0505157000
_diffrn_orient_matrix_UB_32      -0.0430365000
_diffrn_orient_matrix_UB_33      -0.0070328000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5823
_reflns_number_total             8660
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT n/a (Sheldrick, 2015)'
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         8660
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0377
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0404P)²+0.0374P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.0967
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C9 \\sim C16 \\sim N1: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C2 \\sim C1 \\sim N1: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
C1A \\sim N1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
3. Others
 1*[Sof(Br1)]+1*[Sof(Br1B)]+1*[Sof(Br1A)]=1 with esd of 0.0001
 Sof(H1BD)=Sof(H1BE)=Sof(H1BF)=Sof(C1A)=Sof(H1AD)=Sof(H1AE)=Sof(C2A)=Sof(H2AA)=
 Sof(H2AB)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=
 Sof(H2B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C8(H8A,H8B), C11(H11A,H11B), C12(H12A,H12B), C9(H9A,H9B),
 C14(H14A,H14B), C3(H3A,H3B), C13(H13A,H13B), C7(H7A,H7B), C4(H4A,H4B), C6(H6A,
 H6B), C5(H5A,H5B), C1A(H1AD,H1AE), C1(H1A,H1B), C2(H2A,H2B), C2A(H2AA,H2AB)
4.b Idealised Me refined as rotating group:
 N1(H1BD,H1BE,H1BF), N1(H1AA,H1AB,H1AC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.13446(2) 0.46449(2) 0.88355(2) 0.03279(9) Uani 1 1 d . . . . .
S1 S 0.10128(5) 0.33965(5) 0.81758(5) 0.03633(13) Uani 1 1 d . . . . .
S3 S 0.20835(5) 0.07220(5) 0.86726(5) 0.03809(14) Uani 1 1 d . . . . .
S9 S 0.05460(5) 0.84405(5) 0.92231(5) 0.03905(14) Uani 1 1 d . . . . .
S4 S 0.35718(5) 0.06234(5) 1.02536(5) 0.03893(14) Uani 1 1 d . . . . .
S2 S 0.26544(5) 0.32830(5) 0.98938(5) 0.04087(15) Uani 1 1 d . . . . .
S7 S 0.16120(5) 0.58136(5) 0.95872(5) 0.04134(15) Uani 1 1 d . . . . .
S6 S 0.01166(6) 0.60801(5) 0.77282(5) 0.04337(15) Uani 1 1 d . . . . .
S8 S -0.07929(6) 0.87222(5) 0.74782(6) 0.04914(17) Uani 1 1 d . . . . .
S5 S 0.36374(6) -0.16377(5) 0.98886(6) 0.05076(17) Uani 1 1 d . . . . .
S10 S -0.09313(6) 1.08521(6) 0.80803(7) 0.0576(2) Uani 1 1 d . . . . .
Br1A Br 0.07691(6) 0.14536(8) 0.53849(8) 0.0695(3) Uani 0.4719(16) 1 d . . P A
3
O5 O 0.36064(14) 0.39289(15) 0.61935(14) 0.0468(4) Uani 1 1 d . . . . .
O6 O 0.57026(15) 0.22142(15) 0.62549(14) 0.0498(4) Uani 1 1 d . . . . .
O4 O 0.25692(14) 0.53313(16) 0.42194(15) 0.0511(4) Uani 1 1 d . . . . .
O1 O 0.64456(15) 0.14103(17) 0.45835(15) 0.0530(4) Uani 1 1 d . . . . .
N1 N 0.39999(17) 0.29008(19) 0.46206(17) 0.0471(5) Uani 1 1 d . U . . .
H1BD H 0.343528 0.356880 0.439807 0.057 Uiso 0.455(8) 1 calc R U P B 2
H1BE H 0.439911 0.276910 0.405306 0.057 Uiso 0.455(8) 1 calc R U P B 2
H1BF H 0.453485 0.301333 0.497873 0.057 Uiso 0.455(8) 1 calc R U P B 2
H1AA H 0.389731 0.354036 0.399174 0.057 Uiso 0.545(8) 1 calc R U P B 1
H1AB H 0.479525 0.258276 0.465513 0.057 Uiso 0.545(8) 1 calc R U P B 1
H1AC H 0.374805 0.314950 0.515570 0.057 Uiso 0.545(8) 1 calc R U P B 1
O3 O 0.31998(16) 0.46191(18) 0.25434(16) 0.0598(5) Uani 1 1 d . . . . .
O2 O 0.54558(18) 0.3053(2) 0.26415(16) 0.0696(6) Uani 1 1 d . . . . .
C19 C 0.07024(18) 0.71601(18) 0.89119(19) 0.0336(5) Uani 1 1 d . . . . .
C15 C 0.19821(18) 0.20817(18) 0.88531(18) 0.0320(5) Uani 1 1 d . . . . .
C16 C 0.26799(18) 0.20256(18) 0.95990(18) 0.0323(5) Uani 1 1 d . . . . .
C18 C 0.00622(19) 0.72768(19) 0.81072(19) 0.0361(5) Uani 1 1 d . . . . .
C20 C -0.0423(2) 0.9414(2) 0.8251(2) 0.0413(5) Uani 1 1 d . . . . .
C17 C 0.3124(2) -0.01704(19) 0.96177(19) 0.0375(5) Uani 1 1 d . . . . .
C10 C 0.3036(2) 0.5176(2) 0.5894(2) 0.0530(7) Uani 1 1 d . . . . .
H10A H 0.364379 0.572430 0.550626 0.064 Uiso 1 1 calc R U . . .
H10B H 0.270123 0.532217 0.653517 0.064 Uiso 1 1 calc R U . . .
C8 C 0.1734(2) 0.5673(3) 0.3435(2) 0.0574(7) Uani 1 1 d . . . . .
H8A H 0.124402 0.646262 0.334901 0.069 Uiso 1 1 calc R U . . .
H8B H 0.117839 0.506446 0.365820 0.069 Uiso 1 1 calc R U . . .
C11 C 0.4498(2) 0.3607(3) 0.6940(2) 0.0513(6) Uani 1 1 d . . . . .
H11A H 0.410554 0.370800 0.758860 0.062 Uiso 1 1 calc R U . . .
H11B H 0.512761 0.414407 0.662778 0.062 Uiso 1 1 calc R U . . .
C12 C 0.5071(2) 0.2304(3) 0.7211(2) 0.0543(7) Uani 1 1 d . . . . .
H12A H 0.564540 0.205638 0.775479 0.065 Uiso 1 1 calc R U . . .
H12B H 0.443968 0.176790 0.749396 0.065 Uiso 1 1 calc R U . . .
C9 C 0.2029(2) 0.5427(3) 0.5200(2) 0.0559(7) Uani 1 1 d . . . . .
H9A H 0.145563 0.483562 0.556190 0.067 Uiso 1 1 calc R U . . .
H9B H 0.157903 0.624729 0.505221 0.067 Uiso 1 1 calc R U . . .
C14 C 0.7202(2) 0.1164(3) 0.5411(3) 0.0627(8) Uani 1 1 d . . . . .
H14A H 0.768619 0.182845 0.520323 0.075 Uiso 1 1 calc R U . . .
H14B H 0.776644 0.040609 0.552397 0.075 Uiso 1 1 calc R U . . .
C3 C 0.7125(2) 0.1715(3) 0.3556(2) 0.0592(7) Uani 1 1 d . . . . .
H3A H 0.776354 0.103345 0.356970 0.071 Uiso 1 1 calc R U . . .
H3B H 0.752052 0.243055 0.338557 0.071 Uiso 1 1 calc R U . . .
C13 C 0.6413(3) 0.1048(3) 0.6426(2) 0.0649(8) Uani 1 1 d . . . . .
H13A H 0.587550 0.043324 0.660582 0.078 Uiso 1 1 calc R U . . .
H13B H 0.692352 0.079820 0.701593 0.078 Uiso 1 1 calc R U . . .
C7 C 0.2442(2) 0.5756(3) 0.2402(2) 0.0553(7) Uani 1 1 d . . . . .
H7A H 0.187784 0.595342 0.186030 0.066 Uiso 1 1 calc R U . . .
H7B H 0.295047 0.640708 0.215353 0.066 Uiso 1 1 calc R U . . .
C4 C 0.6301(3) 0.1978(3) 0.2730(3) 0.0687(8) Uani 1 1 d . . . . .
H4A H 0.677765 0.210158 0.204345 0.082 Uiso 1 1 calc R U . . .
H4B H 0.585673 0.128755 0.292476 0.082 Uiso 1 1 calc R U . . .
C6 C 0.4025(3) 0.4703(3) 0.1617(2) 0.0767(10) Uani 1 1 d . . . . .
H6A H 0.459332 0.527245 0.149910 0.092 Uiso 1 1 calc R U . . .
H6B H 0.356314 0.501567 0.098826 0.092 Uiso 1 1 calc R U . . .
C5 C 0.4718(3) 0.3486(4) 0.1765(3) 0.0959(13) Uani 1 1 d . . . . .
H5A H 0.414749 0.291186 0.190250 0.115 Uiso 1 1 calc R U . . .
H5B H 0.524037 0.353885 0.111247 0.115 Uiso 1 1 calc R U . . .
C1A C 0.3342(11) 0.1745(12) 0.5390(9) 0.084(3) Uani 0.455(8) 1 d . U P B 2
H1AD H 0.340713 0.121621 0.500617 0.100 Uiso 0.455(8) 1 calc R U P B 2
H1AE H 0.382336 0.129181 0.600644 0.100 Uiso 0.455(8) 1 calc R U P B 2
C1 C 0.3310(11) 0.2008(10) 0.4713(12) 0.127(4) Uani 0.545(8) 1 d . U P B 1
H1A H 0.375246 0.161559 0.424465 0.152 Uiso 0.545(8) 1 calc R U P B 1
H1B H 0.336176 0.138968 0.544461 0.152 Uiso 0.545(8) 1 calc R U P B 1
Br1B Br 0.10523(9) 0.22782(12) 0.47429(11) 0.0617(5) Uani 0.3133(15) 1 d . . P
B 2
Br1 Br 0.1207(2) 0.2053(2) 0.5686(2) 0.0957(11) Uani 0.2149(16) 1 d . . P B 1
C2 C 0.2149(7) 0.2223(8) 0.4527(8) 0.136(5) Uani 0.545(8) 1 d . U P B 1
H2A H 0.199589 0.165480 0.424338 0.163 Uiso 0.545(8) 1 calc R U P B 1
H2B H 0.196177 0.305431 0.399069 0.163 Uiso 0.545(8) 1 calc R U P B 1
C2A C 0.2168(8) 0.1893(8) 0.5771(8) 0.078(3) Uani 0.455(8) 1 d . . P B 2
H2AA H 0.203809 0.254717 0.602798 0.093 Uiso 0.455(8) 1 calc R U P B 2
H2AB H 0.199872 0.114014 0.638147 0.093 Uiso 0.455(8) 1 calc R U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S1 2.1658(6) . ?
Ni1 S2 2.1580(6) . ?
Ni1 S7 2.1497(6) . ?
Ni1 S6 2.1664(6) . ?
S1 C15 1.718(2) . ?
S3 C15 1.740(2) . ?
S3 C17 1.730(2) . ?
S9 C19 1.739(2) . ?
S9 C20 1.721(2) . ?
S4 C16 1.733(2) . ?
S4 C17 1.718(2) . ?
S2 C16 1.721(2) . ?
S7 C19 1.706(2) . ?
S6 C18 1.716(2) . ?
S8 C18 1.743(2) . ?
S8 C20 1.734(3) . ?
S5 C17 1.649(2) . ?
S10 C20 1.644(2) . ?
O5 C10 1.423(3) . ?
O5 C11 1.419(3) . ?
O6 C12 1.420(3) . ?
O6 C13 1.416(3) . ?
O4 C8 1.408(3) . ?
O4 C9 1.422(3) . ?
O1 C14 1.416(3) . ?
O1 C3 1.422(3) . ?
N1 H1BD 0.8900 . ?
N1 H1BE 0.8900 . ?
N1 H1BF 0.8900 . ?
N1 H1AA 0.8900 . ?
N1 H1AB 0.8900 . ?
N1 H1AC 0.8900 . ?
N1 C1A 1.586(11) . ?
N1 C1 1.393(10) . ?
O3 C7 1.415(3) . ?
O3 C6 1.420(3) . ?
O2 C4 1.415(3) . ?
O2 C5 1.417(4) . ?
C19 C18 1.350(3) . ?
C15 C16 1.350(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C9 1.488(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C7 1.480(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.486(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C13 1.488(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.461(4) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C5 1.465(5) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C1A H1AD 0.9700 . ?
C1A H1AE 0.9700 . ?
C1A C2A 1.329(13) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.307(12) . ?
Br1B C2A 1.876(9) . ?
Br1 C2 1.714(10) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S1 Ni1 S6 88.42(2) . . ?
S2 Ni1 S1 93.30(2) . . ?
S2 Ni1 S6 176.57(3) . . ?
S7 Ni1 S1 176.27(3) . . ?
S7 Ni1 S2 85.43(2) . . ?
S7 Ni1 S6 93.03(2) . . ?
C15 S1 Ni1 101.76(8) . . ?
C17 S3 C15 97.25(11) . . ?
C20 S9 C19 97.29(11) . . ?
C17 S4 C16 97.26(10) . . ?
C16 S2 Ni1 102.07(8) . . ?
C19 S7 Ni1 102.59(8) . . ?
C18 S6 Ni1 101.63(8) . . ?
C20 S8 C18 97.51(11) . . ?
C11 O5 C10 111.65(19) . . ?
C13 O6 C12 113.8(2) . . ?
C8 O4 C9 114.45(19) . . ?
C14 O1 C3 112.3(2) . . ?
H1BD N1 H1BE 109.5 . . ?
H1BD N1 H1BF 109.5 . . ?
H1BE N1 H1BF 109.5 . . ?
H1AA N1 H1AB 109.5 . . ?
H1AA N1 H1AC 109.5 . . ?
H1AB N1 H1AC 109.5 . . ?
C1A N1 H1BD 109.5 . . ?
C1A N1 H1BE 109.5 . . ?
C1A N1 H1BF 109.5 . . ?
C1 N1 H1AA 109.5 . . ?
C1 N1 H1AB 109.5 . . ?
C1 N1 H1AC 109.5 . . ?
C7 O3 C6 111.8(2) . . ?
C4 O2 C5 113.6(2) . . ?
S7 C19 S9 122.14(14) . . ?
C18 C19 S9 116.76(16) . . ?
C18 C19 S7 121.10(16) . . ?
S1 C15 S3 122.71(13) . . ?
C16 C15 S1 121.67(16) . . ?
C16 C15 S3 115.57(16) . . ?
S2 C16 S4 122.14(13) . . ?
C15 C16 S4 116.66(16) . . ?
C15 C16 S2 121.20(16) . . ?
S6 C18 S8 122.96(14) . . ?
C19 C18 S6 121.64(16) . . ?
C19 C18 S8 115.40(16) . . ?
S9 C20 S8 113.03(12) . . ?
S10 C20 S9 122.95(15) . . ?
S10 C20 S8 124.02(15) . . ?
S4 C17 S3 113.26(12) . . ?
S5 C17 S3 123.69(14) . . ?
S5 C17 S4 123.05(14) . . ?
O5 C10 H10A 109.8 . . ?
O5 C10 H10B 109.8 . . ?
O5 C10 C9 109.4(2) . . ?
H10A C10 H10B 108.2 . . ?
C9 C10 H10A 109.8 . . ?
C9 C10 H10B 109.8 . . ?
O4 C8 H8A 109.9 . . ?
O4 C8 H8B 109.9 . . ?
O4 C8 C7 108.7(2) . . ?
H8A C8 H8B 108.3 . . ?
C7 C8 H8A 109.9 . . ?
C7 C8 H8B 109.9 . . ?
O5 C11 H11A 109.8 . . ?
O5 C11 H11B 109.8 . . ?
O5 C11 C12 109.2(2) . . ?
H11A C11 H11B 108.3 . . ?
C12 C11 H11A 109.8 . . ?
C12 C11 H11B 109.8 . . ?
O6 C12 C11 108.0(2) . . ?
O6 C12 H12A 110.1 . . ?
O6 C12 H12B 110.1 . . ?
C11 C12 H12A 110.1 . . ?
C11 C12 H12B 110.1 . . ?
H12A C12 H12B 108.4 . . ?
O4 C9 C10 108.23(19) . . ?
O4 C9 H9A 110.1 . . ?
O4 C9 H9B 110.1 . . ?
C10 C9 H9A 110.1 . . ?
C10 C9 H9B 110.1 . . ?
H9A C9 H9B 108.4 . . ?
O1 C14 H14A 109.8 . . ?
O1 C14 H14B 109.8 . . ?
O1 C14 C13 109.5(2) . . ?
H14A C14 H14B 108.2 . . ?
C13 C14 H14A 109.8 . . ?
C13 C14 H14B 109.8 . . ?
O1 C3 H3A 109.6 . . ?
O1 C3 H3B 109.6 . . ?
O1 C3 C4 110.1(2) . . ?
H3A C3 H3B 108.2 . . ?
C4 C3 H3A 109.6 . . ?
C4 C3 H3B 109.6 . . ?
O6 C13 C14 107.6(2) . . ?
O6 C13 H13A 110.2 . . ?
O6 C13 H13B 110.2 . . ?
C14 C13 H13A 110.2 . . ?
C14 C13 H13B 110.2 . . ?
H13A C13 H13B 108.5 . . ?
O3 C7 C8 109.7(2) . . ?
O3 C7 H7A 109.7 . . ?
O3 C7 H7B 109.7 . . ?
C8 C7 H7A 109.7 . . ?
C8 C7 H7B 109.7 . . ?
H7A C7 H7B 108.2 . . ?
O2 C4 C3 108.9(2) . . ?
O2 C4 H4A 109.9 . . ?
O2 C4 H4B 109.9 . . ?
C3 C4 H4A 109.9 . . ?
C3 C4 H4B 109.9 . . ?
H4A C4 H4B 108.3 . . ?
O3 C6 H6A 109.7 . . ?
O3 C6 H6B 109.7 . . ?
O3 C6 C5 110.0(3) . . ?
H6A C6 H6B 108.2 . . ?
C5 C6 H6A 109.7 . . ?
C5 C6 H6B 109.7 . . ?
O2 C5 C6 110.2(3) . . ?
O2 C5 H5A 109.6 . . ?
O2 C5 H5B 109.6 . . ?
C6 C5 H5A 109.6 . . ?
C6 C5 H5B 109.6 . . ?
H5A C5 H5B 108.1 . . ?
N1 C1A H1AD 107.2 . . ?
N1 C1A H1AE 107.2 . . ?
H1AD C1A H1AE 106.8 . . ?
C2A C1A N1 120.7(10) . . ?
C2A C1A H1AD 107.2 . . ?
C2A C1A H1AE 107.2 . . ?
N1 C1 H1A 106.1 . . ?
N1 C1 H1B 106.1 . . ?
H1A C1 H1B 106.3 . . ?
C2 C1 N1 124.9(10) . . ?
C2 C1 H1A 106.1 . . ?
C2 C1 H1B 106.1 . . ?
C1 C2 Br1 110.7(9) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
Br1 C2 H2A 109.5 . . ?
Br1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
C1A C2A Br1B 113.2(7) . . ?
C1A C2A H2AA 108.9 . . ?
C1A C2A H2AB 108.9 . . ?
Br1B C2A H2AA 108.9 . . ?
Br1B C2A H2AB 108.9 . . ?
H2AA C2A H2AB 107.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S1 C15 S3 178.37(11) . . . . ?
Ni1 S1 C15 C16 1.25(19) . . . . ?
Ni1 S2 C16 S4 -178.43(11) . . . . ?
Ni1 S2 C16 C15 0.4(2) . . . . ?
Ni1 S7 C19 S9 178.58(11) . . . . ?
Ni1 S7 C19 C18 -1.1(2) . . . . ?
Ni1 S6 C18 S8 179.36(12) . . . . ?
Ni1 S6 C18 C19 0.3(2) . . . . ?
S1 C15 C16 S4 177.70(11) . . . . ?
S1 C15 C16 S2 -1.2(3) . . . . ?
S3 C15 C16 S4 0.4(2) . . . . ?
S3 C15 C16 S2 -178.49(11) . . . . ?
S9 C19 C18 S6 -179.17(12) . . . . ?
S9 C19 C18 S8 1.7(2) . . . . ?
S7 C19 C18 S6 0.6(3) . . . . ?
S7 C19 C18 S8 -178.52(12) . . . . ?
O5 C10 C9 O4 -65.6(3) . . . . ?
O5 C11 C12 O6 63.3(3) . . . . ?
O4 C8 C7 O3 56.8(3) . . . . ?
O1 C14 C13 O6 -65.6(3) . . . . ?
O1 C3 C4 O2 65.4(3) . . . . ?
N1 C1A C2A Br1B 75.9(9) . . . . ?
N1 C1 C2 Br1 -91.4(13) . . . . ?
O3 C6 C5 O2 -62.9(4) . . . . ?
C19 S9 C20 S8 0.89(15) . . . . ?
C19 S9 C20 S10 -178.84(15) . . . . ?
C15 S3 C17 S4 -0.61(14) . . . . ?
C15 S3 C17 S5 179.27(15) . . . . ?
C16 S4 C17 S3 0.78(14) . . . . ?
C16 S4 C17 S5 -179.11(15) . . . . ?
C18 S8 C20 S9 -0.15(15) . . . . ?
C18 S8 C20 S10 179.57(16) . . . . ?
C20 S9 C19 S7 178.65(14) . . . . ?
C20 S9 C19 C18 -1.6(2) . . . . ?
C20 S8 C18 S6 179.98(15) . . . . ?
C20 S8 C18 C19 -1.0(2) . . . . ?
C17 S3 C15 S1 -177.14(14) . . . . ?
C17 S3 C15 C16 0.14(19) . . . . ?
C17 S4 C16 S2 178.15(14) . . . . ?
C17 S4 C16 C15 -0.72(19) . . . . ?
C10 O5 C11 C12 -179.3(2) . . . . ?
C8 O4 C9 C10 -173.7(2) . . . . ?
C11 O5 C10 C9 -174.5(2) . . . . ?
C12 O6 C13 C14 -169.2(2) . . . . ?
C9 O4 C8 C7 169.5(2) . . . . ?
C14 O1 C3 C4 -179.2(2) . . . . ?
C3 O1 C14 C13 171.1(2) . . . . ?
C13 O6 C12 C11 173.0(2) . . . . ?
C7 O3 C6 C5 -175.4(3) . . . . ?
C4 O2 C5 C6 -170.4(3) . . . . ?
C6 O3 C7 C8 -171.7(2) . . . . ?
C5 O2 C4 C3 172.1(3) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.358
_oxdiff_exptl_absorpt_empirical_full_min 0.458
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_273k
_database_code_depnum_ccdc_archive 'CCDC 2053307'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-18 downloaded from the CCDC.
;
_audit_creation_date             2020-11-10
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C2 H7 Br1 N, C12 H23 O6'
_chemical_formula_sum            'C20 H30 Br N Ni O6 S10'
_chemical_formula_weight         839.67
_chemical_melting_point          ?
_chemical_oxdiff_formula         BrCHNONiS
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.1022(4)
_cell_length_b                   12.0838(4)
_cell_length_c                   13.7055(5)
_cell_angle_alpha                65.348(3)
_cell_angle_beta                 80.897(3)
_cell_angle_gamma                78.557(3)
_cell_volume                     1632.00(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    14001
_cell_measurement_temperature    273
_cell_measurement_theta_max      31.0180
_cell_measurement_theta_min      2.3640
_shelx_estimated_absorpt_T_max   0.845
_shelx_estimated_absorpt_T_min   0.435
_exptl_absorpt_coefficient_mu    2.494
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0635
_diffrn_reflns_av_unetI/netI     0.0604
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.832
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            41574
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.832
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.078
_diffrn_reflns_theta_min         1.875
_diffrn_ambient_temperature      273
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.832
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -67.00  18.00   0.50    1.30    --    5.18 -37.00-150.00  170
  2  ω    -69.00  18.00   0.50    1.30    --    5.18 -32.00-113.50  174
  3  ω    -54.00  18.00   0.50    1.30    --    5.18 -27.00 -69.74  144
  4  ω    -54.00  19.00   0.50    1.30    --    5.18 -28.00  -4.20  146
  5  ω    -48.00  19.00   0.50    1.30    --    5.18 -28.00  54.08  134
  6  ω    -64.00  19.00   0.50    1.30    --    5.18 -28.00 115.55  166
  7  ω    -25.00  19.00   0.50    1.30    --    5.18 -33.00 154.09   88
  8  ω    -17.00  24.00   0.50    1.30    --   -4.95 -99.00  60.00   82
  9  ω    -16.00  25.00   0.50    1.30    --   -4.95 -99.00 120.00   82
 10  ω     -3.00  28.00   0.50    1.30    --   -4.95 -99.00 -60.00   62
 11  ω    -18.00  28.00   0.50    1.30    --   -4.95 -99.00-120.00   92
 12  ω    -14.00  27.00   0.50    1.30    --   -4.95 -99.00-180.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0290863000
_diffrn_orient_matrix_UB_12      0.0033972000
_diffrn_orient_matrix_UB_13      0.0409693000
_diffrn_orient_matrix_UB_21      -0.0287359000
_diffrn_orient_matrix_UB_22      -0.0496874000
_diffrn_orient_matrix_UB_23      0.0391269000
_diffrn_orient_matrix_UB_31      0.0510688000
_diffrn_orient_matrix_UB_32      -0.0422329000
_diffrn_orient_matrix_UB_33      -0.0075198000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5547
_reflns_number_total             8724
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT n/a (Sheldrick, 2015)'
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         8724
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0413
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0400P)²+0.2941P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.1026
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C1A \\sim N1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
C1 \\sim C2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
3. Others
 1*[Sof(Br1)]+1*[Sof(Br1A)]+1*[Sof(Br1B)]=1 with esd of 0.0001
 Sof(H1BD)=Sof(H1BE)=Sof(H1BF)=Sof(C1A)=Sof(H1AD)=Sof(H1AE)=Sof(C2A)=Sof(H2AA)=
 Sof(H2AB)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=
 Sof(H2B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C9(H9A,H9B), C14(H14A,H14B),
 C3(H3A,H3B), C13(H13A,H13B), C7(H7A,H7B), C4(H4A,H4B), C6(H6A,H6B), C5(H5A,
 H5B), C1A(H1AD,H1AE), C1(H1A,H1B), C2(H2A,H2B), C2A(H2AA,H2AB)
4.b Aromatic/amide H refined with riding coordinates:
 C8(H8)
4.c Idealised Me refined as rotating group:
 N1(H1BD,H1BE,H1BF), N1(H1AA,H1AB,H1AC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.13417(3) 0.46436(3) 0.88335(3) 0.03559(10) Uani 1 1 d . . . . .
S1 S 0.10090(6) 0.33960(5) 0.81736(6) 0.03952(15) Uani 1 1 d . . . . .
S3 S 0.20795(6) 0.07232(5) 0.86709(6) 0.04128(16) Uani 1 1 d . . . . .
S9 S 0.05450(6) 0.84380(6) 0.92197(6) 0.04234(16) Uani 1 1 d . . . . .
S4 S 0.35705(6) 0.06259(6) 1.02512(6) 0.04195(16) Uani 1 1 d . . . . .
S2 S 0.26526(6) 0.32839(6) 0.98917(6) 0.04416(17) Uani 1 1 d . . . . .
S7 S 0.16077(6) 0.58137(6) 0.95859(6) 0.04491(17) Uani 1 1 d . . . . .
S6 S 0.01156(6) 0.60777(6) 0.77257(6) 0.04673(18) Uani 1 1 d . . . . .
S8 S -0.07946(7) 0.87191(6) 0.74757(7) 0.0528(2) Uani 1 1 d . . . . .
S5 S 0.36367(7) -0.16335(6) 0.98860(7) 0.0549(2) Uani 1 1 d . . . . .
S10 S -0.09402(7) 1.08450(6) 0.80824(8) 0.0620(2) Uani 1 1 d . . . . .
Br1B Br 0.07718(7) 0.14530(9) 0.53908(9) 0.0748(4) Uani 0.5075(18) 1 d . . P A
3
O1 O 0.36001(17) 0.39287(18) 0.61927(16) 0.0511(5) Uani 1 1 d . . . . .
O2 O 0.56944(17) 0.22126(17) 0.62509(16) 0.0539(5) Uani 1 1 d . . . . .
O6 O 0.25674(17) 0.53355(19) 0.42177(17) 0.0570(5) Uani 1 1 d . . . . .
O3 O 0.64377(18) 0.14137(19) 0.45773(18) 0.0586(5) Uani 1 1 d . . . . .
N1 N 0.39995(19) 0.2914(2) 0.4608(2) 0.0508(6) Uani 1 1 d . U . . .
H1BD H 0.439996 0.275625 0.405387 0.061 Uiso 0.452(10) 1 calc R U P B 2
H1BE H 0.453650 0.301121 0.497424 0.061 Uiso 0.452(10) 1 calc R U P B 2
H1BF H 0.345969 0.359952 0.436650 0.061 Uiso 0.452(10) 1 calc R U P B 2
H1AA H 0.479932 0.261473 0.460388 0.061 Uiso 0.548(10) 1 calc R U P B 1
H1AB H 0.377747 0.313614 0.516169 0.061 Uiso 0.548(10) 1 calc R U P B 1
H1AC H 0.385604 0.356617 0.399577 0.061 Uiso 0.548(10) 1 calc R U P B 1
O5 O 0.32043(19) 0.4636(2) 0.25371(18) 0.0661(6) Uani 1 1 d . . . . .
O4 O 0.5454(2) 0.3059(2) 0.26362(19) 0.0758(7) Uani 1 1 d . . . . .
C19 C 0.0699(2) 0.7159(2) 0.8907(2) 0.0375(6) Uani 1 1 d . . . . .
C15 C 0.1979(2) 0.2082(2) 0.8852(2) 0.0345(5) Uani 1 1 d . . . . .
C16 C 0.2674(2) 0.2028(2) 0.9599(2) 0.0352(5) Uani 1 1 d . . . . .
C18 C 0.0058(2) 0.7274(2) 0.8103(2) 0.0389(6) Uani 1 1 d . . . . .
C20 C -0.0423(2) 0.9405(2) 0.8254(2) 0.0440(6) Uani 1 1 d . . . . .
C17 C 0.3120(2) -0.0168(2) 0.9615(2) 0.0398(6) Uani 1 1 d . . . . .
C10 C 0.3036(3) 0.5183(3) 0.5891(3) 0.0581(8) Uani 1 1 d . . . . .
H10A H 0.364403 0.572592 0.549926 0.070 Uiso 1 1 calc R U . . .
H10B H 0.270649 0.533558 0.652929 0.070 Uiso 1 1 calc R U . . .
C8 C 0.1738(3) 0.5682(3) 0.3427(3) 0.0632(9) Uani 1 1 d . . . . .
H8 H 0.088319 0.583431 0.353530 0.076 Uiso 1 1 calc R U . . .
C11 C 0.4495(3) 0.3604(3) 0.6943(3) 0.0563(8) Uani 1 1 d . . . . .
H11A H 0.410408 0.369983 0.759379 0.068 Uiso 1 1 calc R U . . .
H11B H 0.512218 0.414035 0.663472 0.068 Uiso 1 1 calc R U . . .
C12 C 0.5067(3) 0.2303(3) 0.7203(2) 0.0601(8) Uani 1 1 d . . . . .
H12A H 0.564077 0.204766 0.774817 0.072 Uiso 1 1 calc R U . . .
H12B H 0.443507 0.177051 0.748027 0.072 Uiso 1 1 calc R U . . .
C9 C 0.2028(3) 0.5428(3) 0.5201(3) 0.0623(9) Uani 1 1 d . . . . .
H9A H 0.146238 0.483295 0.556285 0.075 Uiso 1 1 calc R U . . .
H9B H 0.157214 0.624514 0.505594 0.075 Uiso 1 1 calc R U . . .
C14 C 0.7190(3) 0.1163(3) 0.5412(3) 0.0692(10) Uani 1 1 d . . . . .
H14A H 0.767768 0.182080 0.520692 0.083 Uiso 1 1 calc R U . . .
H14B H 0.774964 0.040115 0.552819 0.083 Uiso 1 1 calc R U . . .
C3 C 0.7116(3) 0.1722(3) 0.3550(3) 0.0665(9) Uani 1 1 d . . . . .
H3A H 0.775360 0.104048 0.356177 0.080 Uiso 1 1 calc R U . . .
H3B H 0.751133 0.243379 0.338613 0.080 Uiso 1 1 calc R U . . .
C13 C 0.6402(3) 0.1056(3) 0.6421(3) 0.0718(10) Uani 1 1 d . . . . .
H13A H 0.586606 0.044191 0.660092 0.086 Uiso 1 1 calc R U . . .
H13B H 0.691162 0.080732 0.701184 0.086 Uiso 1 1 calc R U . . .
C7 C 0.2438(3) 0.5762(3) 0.2405(3) 0.0635(9) Uani 1 1 d . . . . .
H7A H 0.187334 0.595767 0.186412 0.076 Uiso 1 1 calc R U . . .
H7B H 0.293935 0.641688 0.215737 0.076 Uiso 1 1 calc R U . . .
C4 C 0.6302(3) 0.1991(4) 0.2727(3) 0.0760(10) Uani 1 1 d . . . . .
H4A H 0.678059 0.211627 0.204296 0.091 Uiso 1 1 calc R U . . .
H4B H 0.586171 0.130165 0.291573 0.091 Uiso 1 1 calc R U . . .
C6 C 0.4019(3) 0.4714(4) 0.1614(3) 0.0830(12) Uani 1 1 d . . . . .
H6A H 0.458151 0.528943 0.148881 0.100 Uiso 1 1 calc R U . . .
H6B H 0.355254 0.501810 0.098819 0.100 Uiso 1 1 calc R U . . .
C5 C 0.4724(4) 0.3499(5) 0.1763(3) 0.1019(15) Uani 1 1 d . . . . .
H5A H 0.415979 0.292402 0.189210 0.122 Uiso 1 1 calc R U . . .
H5B H 0.524923 0.355544 0.111189 0.122 Uiso 1 1 calc R U . . .
C1A C 0.3313(15) 0.1834(16) 0.5353(12) 0.098(4) Uani 0.452(10) 1 d . U P B 2
H1AD H 0.338197 0.130524 0.496823 0.117 Uiso 0.452(10) 1 calc R U P B 2
H1AE H 0.379756 0.137666 0.596653 0.117 Uiso 0.452(10) 1 calc R U P B 2
C1 C 0.3306(14) 0.1996(13) 0.4711(15) 0.128(4) Uani 0.548(10) 1 d . U P B 1
H1A H 0.374238 0.160051 0.424234 0.153 Uiso 0.548(10) 1 calc R U P B 1
H1B H 0.335942 0.138099 0.544254 0.153 Uiso 0.548(10) 1 calc R U P B 1
Br1A Br 0.10521(12) 0.22844(16) 0.47415(15) 0.0667(7) Uani 0.2730(17) 1 d . . P
B 2
Br1 Br 0.1211(3) 0.2054(3) 0.5678(3) 0.1066(14) Uani 0.2195(19) 1 d . . P B 1
C2 C 0.2149(8) 0.2230(9) 0.4525(9) 0.135(5) Uani 0.548(10) 1 d . U P B 1
H2A H 0.198659 0.167755 0.422747 0.162 Uiso 0.548(10) 1 calc R U P B 1
H2B H 0.196912 0.306655 0.399705 0.162 Uiso 0.548(10) 1 calc R U P B 1
C2A C 0.2166(10) 0.1920(11) 0.5752(10) 0.099(4) Uani 0.452(10) 1 d . . P B 2
H2AA H 0.200803 0.255692 0.603052 0.119 Uiso 0.452(10) 1 calc R U P B 2
H2AB H 0.203561 0.114707 0.634865 0.119 Uiso 0.452(10) 1 calc R U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S1 2.1659(7) . ?
Ni1 S2 2.1569(7) . ?
Ni1 S7 2.1513(7) . ?
Ni1 S6 2.1644(7) . ?
S1 C15 1.718(2) . ?
S3 C15 1.741(2) . ?
S3 C17 1.728(3) . ?
S9 C19 1.739(2) . ?
S9 C20 1.713(3) . ?
S4 C16 1.735(2) . ?
S4 C17 1.720(3) . ?
S2 C16 1.719(2) . ?
S7 C19 1.706(2) . ?
S6 C18 1.714(3) . ?
S8 C18 1.742(2) . ?
S8 C20 1.734(3) . ?
S5 C17 1.649(2) . ?
S10 C20 1.649(2) . ?
O1 C10 1.429(3) . ?
O1 C11 1.425(3) . ?
O2 C12 1.414(4) . ?
O2 C13 1.406(4) . ?
O6 C8 1.408(4) . ?
O6 C9 1.425(4) . ?
O3 C14 1.418(4) . ?
O3 C3 1.423(4) . ?
N1 H1BD 0.8900 . ?
N1 H1BE 0.8900 . ?
N1 H1BF 0.8900 . ?
N1 H1AA 0.8900 . ?
N1 H1AB 0.8900 . ?
N1 H1AC 0.8900 . ?
N1 C1A 1.537(16) . ?
N1 C1 1.421(12) . ?
O5 C7 1.411(4) . ?
O5 C6 1.415(4) . ?
O4 C4 1.410(4) . ?
O4 C5 1.406(4) . ?
C19 C18 1.350(4) . ?
C15 C16 1.349(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C9 1.485(5) . ?
C8 H8 0.9300 . ?
C8 C7 1.466(5) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.487(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C13 1.485(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.447(5) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C5 1.469(5) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C1A H1AD 0.9700 . ?
C1A H1AE 0.9700 . ?
C1A C2A 1.306(18) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.302(16) . ?
Br1A C2A 1.859(12) . ?
Br1 C2 1.707(12) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S2 Ni1 S1 93.34(3) . . ?
S2 Ni1 S6 176.47(3) . . ?
S7 Ni1 S1 176.25(3) . . ?
S7 Ni1 S2 85.45(3) . . ?
S7 Ni1 S6 92.96(3) . . ?
S6 Ni1 S1 88.43(3) . . ?
C15 S1 Ni1 101.68(9) . . ?
C17 S3 C15 97.22(12) . . ?
C20 S9 C19 97.17(13) . . ?
C17 S4 C16 97.25(12) . . ?
C16 S2 Ni1 101.98(9) . . ?
C19 S7 Ni1 102.54(9) . . ?
C18 S6 Ni1 101.78(9) . . ?
C20 S8 C18 97.42(12) . . ?
C11 O1 C10 111.4(2) . . ?
C13 O2 C12 113.7(2) . . ?
C8 O6 C9 114.8(2) . . ?
C14 O3 C3 112.5(2) . . ?
H1BD N1 H1BE 109.5 . . ?
H1BD N1 H1BF 109.5 . . ?
H1BE N1 H1BF 109.5 . . ?
H1AA N1 H1AB 109.5 . . ?
H1AA N1 H1AC 109.5 . . ?
H1AB N1 H1AC 109.5 . . ?
C1A N1 H1BD 109.5 . . ?
C1A N1 H1BE 109.5 . . ?
C1A N1 H1BF 109.5 . . ?
C1 N1 H1AA 109.5 . . ?
C1 N1 H1AB 109.5 . . ?
C1 N1 H1AC 109.5 . . ?
C7 O5 C6 112.5(3) . . ?
C5 O4 C4 114.2(3) . . ?
S7 C19 S9 121.94(16) . . ?
C18 C19 S9 116.92(18) . . ?
C18 C19 S7 121.14(18) . . ?
S1 C15 S3 122.59(15) . . ?
C16 C15 S1 121.62(17) . . ?
C16 C15 S3 115.73(17) . . ?
S2 C16 S4 122.11(15) . . ?
C15 C16 S4 116.52(18) . . ?
C15 C16 S2 121.37(18) . . ?
S6 C18 S8 123.24(16) . . ?
C19 C18 S6 121.57(18) . . ?
C19 C18 S8 115.18(18) . . ?
S9 C20 S8 113.28(14) . . ?
S10 C20 S9 123.10(17) . . ?
S10 C20 S8 123.62(17) . . ?
S4 C17 S3 113.27(13) . . ?
S5 C17 S3 123.80(16) . . ?
S5 C17 S4 122.92(16) . . ?
O1 C10 H10A 109.9 . . ?
O1 C10 H10B 109.9 . . ?
O1 C10 C9 108.8(2) . . ?
H10A C10 H10B 108.3 . . ?
C9 C10 H10A 109.9 . . ?
C9 C10 H10B 109.9 . . ?
O6 C8 H8 125.5 . . ?
O6 C8 C7 109.0(2) . . ?
C7 C8 H8 125.5 . . ?
O1 C11 H11A 109.9 . . ?
O1 C11 H11B 109.9 . . ?
O1 C11 C12 108.7(2) . . ?
H11A C11 H11B 108.3 . . ?
C12 C11 H11A 109.9 . . ?
C12 C11 H11B 109.9 . . ?
O2 C12 C11 108.5(2) . . ?
O2 C12 H12A 110.0 . . ?
O2 C12 H12B 110.0 . . ?
C11 C12 H12A 110.0 . . ?
C11 C12 H12B 110.0 . . ?
H12A C12 H12B 108.4 . . ?
O6 C9 C10 108.1(2) . . ?
O6 C9 H9A 110.1 . . ?
O6 C9 H9B 110.1 . . ?
C10 C9 H9A 110.1 . . ?
C10 C9 H9B 110.1 . . ?
H9A C9 H9B 108.4 . . ?
O3 C14 H14A 109.7 . . ?
O3 C14 H14B 109.7 . . ?
O3 C14 C13 109.7(3) . . ?
H14A C14 H14B 108.2 . . ?
C13 C14 H14A 109.7 . . ?
C13 C14 H14B 109.7 . . ?
O3 C3 H3A 109.6 . . ?
O3 C3 H3B 109.6 . . ?
O3 C3 C4 110.2(3) . . ?
H3A C3 H3B 108.1 . . ?
C4 C3 H3A 109.6 . . ?
C4 C3 H3B 109.6 . . ?
O2 C13 C14 107.9(3) . . ?
O2 C13 H13A 110.1 . . ?
O2 C13 H13B 110.1 . . ?
C14 C13 H13A 110.1 . . ?
C14 C13 H13B 110.1 . . ?
H13A C13 H13B 108.4 . . ?
O5 C7 C8 110.3(3) . . ?
O5 C7 H7A 109.6 . . ?
O5 C7 H7B 109.6 . . ?
C8 C7 H7A 109.6 . . ?
C8 C7 H7B 109.6 . . ?
H7A C7 H7B 108.1 . . ?
O4 C4 C3 109.5(3) . . ?
O4 C4 H4A 109.8 . . ?
O4 C4 H4B 109.8 . . ?
C3 C4 H4A 109.8 . . ?
C3 C4 H4B 109.8 . . ?
H4A C4 H4B 108.2 . . ?
O5 C6 H6A 109.6 . . ?
O5 C6 H6B 109.6 . . ?
O5 C6 C5 110.2(3) . . ?
H6A C6 H6B 108.1 . . ?
C5 C6 H6A 109.6 . . ?
C5 C6 H6B 109.6 . . ?
O4 C5 C6 110.9(3) . . ?
O4 C5 H5A 109.5 . . ?
O4 C5 H5B 109.5 . . ?
C6 C5 H5A 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 108.0 . . ?
N1 C1A H1AD 105.8 . . ?
N1 C1A H1AE 105.8 . . ?
H1AD C1A H1AE 106.2 . . ?
C2A C1A N1 126.1(14) . . ?
C2A C1A H1AD 105.8 . . ?
C2A C1A H1AE 105.8 . . ?
N1 C1 H1A 106.5 . . ?
N1 C1 H1B 106.5 . . ?
H1A C1 H1B 106.5 . . ?
C2 C1 N1 123.3(12) . . ?
C2 C1 H1A 106.5 . . ?
C2 C1 H1B 106.5 . . ?
C1 C2 Br1 111.1(10) . . ?
C1 C2 H2A 109.4 . . ?
C1 C2 H2B 109.4 . . ?
Br1 C2 H2A 109.4 . . ?
Br1 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
C1A C2A Br1A 112.8(9) . . ?
C1A C2A H2AA 109.0 . . ?
C1A C2A H2AB 109.0 . . ?
Br1A C2A H2AA 109.0 . . ?
Br1A C2A H2AB 109.0 . . ?
H2AA C2A H2AB 107.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S1 C15 S3 178.38(13) . . . . ?
Ni1 S1 C15 C16 1.4(2) . . . . ?
Ni1 S2 C16 S4 -178.64(13) . . . . ?
Ni1 S2 C16 C15 0.6(2) . . . . ?
Ni1 S7 C19 S9 178.58(13) . . . . ?
Ni1 S7 C19 C18 -0.9(2) . . . . ?
Ni1 S6 C18 S8 179.34(14) . . . . ?
Ni1 S6 C18 C19 0.5(2) . . . . ?
S1 C15 C16 S4 177.88(13) . . . . ?
S1 C15 C16 S2 -1.4(3) . . . . ?
S3 C15 C16 S4 0.7(3) . . . . ?
S3 C15 C16 S2 -178.65(13) . . . . ?
S9 C19 C18 S6 -179.25(14) . . . . ?
S9 C19 C18 S8 1.8(3) . . . . ?
S7 C19 C18 S6 0.3(3) . . . . ?
S7 C19 C18 S8 -178.62(14) . . . . ?
O1 C10 C9 O6 -66.3(3) . . . . ?
O1 C11 C12 O2 63.3(3) . . . . ?
O6 C8 C7 O5 56.3(4) . . . . ?
O3 C14 C13 O2 -65.2(4) . . . . ?
O3 C3 C4 O4 65.3(4) . . . . ?
N1 C1A C2A Br1A 75.5(12) . . . . ?
N1 C1 C2 Br1 -92.5(15) . . . . ?
O5 C6 C5 O4 -61.9(5) . . . . ?
C19 S9 C20 S8 0.66(17) . . . . ?
C19 S9 C20 S10 -179.02(18) . . . . ?
C15 S3 C17 S4 -0.64(17) . . . . ?
C15 S3 C17 S5 179.34(17) . . . . ?
C16 S4 C17 S3 0.93(16) . . . . ?
C16 S4 C17 S5 -179.06(17) . . . . ?
C18 S8 C20 S9 0.12(17) . . . . ?
C18 S8 C20 S10 179.80(18) . . . . ?
C20 S9 C19 S7 178.93(16) . . . . ?
C20 S9 C19 C18 -1.5(2) . . . . ?
C20 S8 C18 S6 179.94(17) . . . . ?
C20 S8 C18 C19 -1.2(2) . . . . ?
C17 S3 C15 S1 -177.19(16) . . . . ?
C17 S3 C15 C16 0.0(2) . . . . ?
C17 S4 C16 S2 178.34(16) . . . . ?
C17 S4 C16 C15 -1.0(2) . . . . ?
C10 O1 C11 C12 -178.6(2) . . . . ?
C8 O6 C9 C10 -173.1(3) . . . . ?
C11 O1 C10 C9 -174.2(2) . . . . ?
C12 O2 C13 C14 -169.2(3) . . . . ?
C9 O6 C8 C7 169.7(3) . . . . ?
C14 O3 C3 C4 -178.9(3) . . . . ?
C3 O3 C14 C13 170.6(3) . . . . ?
C13 O2 C12 C11 172.5(3) . . . . ?
C7 O5 C6 C5 -175.6(3) . . . . ?
C4 O4 C5 C6 -170.5(3) . . . . ?
C6 O5 C7 C8 -172.2(3) . . . . ?
C5 O4 C4 C3 172.0(3) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.343
_oxdiff_exptl_absorpt_empirical_full_min 0.397
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_293k
_database_code_depnum_ccdc_archive 'CCDC 2053308'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-18 downloaded from the CCDC.
;
_audit_creation_date             2020-11-10
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C2 H7 Br N, C12 H24 O6'
_chemical_formula_sum            'C20 H31 Br N Ni O6 S10'
_chemical_formula_weight         840.68
_chemical_melting_point          ?
_chemical_oxdiff_formula         BrCHNONiS
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.1201(5)
_cell_length_b                   12.1021(5)
_cell_length_c                   13.7058(7)
_cell_angle_alpha                65.393(5)
_cell_angle_beta                 80.958(4)
_cell_angle_gamma                78.454(4)
_cell_volume                     1637.40(15)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    13385
_cell_measurement_temperature    293
_cell_measurement_theta_max      31.0650
_cell_measurement_theta_min      1.9200
_shelx_estimated_absorpt_T_max   0.845
_shelx_estimated_absorpt_T_min   0.436
_exptl_absorpt_coefficient_mu    2.486
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38563
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             858
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0744
_diffrn_reflns_av_unetI/netI     0.0685
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.833
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            42141
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.833
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.053
_diffrn_reflns_theta_min         1.872
_diffrn_ambient_temperature      293
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.833
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -70.00  18.00   0.50    1.37    --    5.18 -30.00  37.72  176
  2  ω    -65.00  18.00   0.50    1.37    --    5.18 -32.00 103.60  166
  3  ω    -46.00  19.00   0.50    1.37    --    5.18 -28.00  -1.37  130
  4  ω    -67.00 -41.00   0.50    1.37    --    5.18 -28.00 -58.05   52
  5  ω    -58.00  19.00   0.50    1.37    --    5.18 -33.00 -79.47  154
  6  ω    -63.00  18.00   0.50    1.37    --    5.18 -29.00-140.18  162
  7  ω    -27.00  19.00   0.50    1.37    --    5.18 -28.00 -58.05   92
  8  ω    -69.00  18.00   0.50    1.37    --    5.18 -27.00 154.51  174
  9  ω    -13.00  29.00   0.50    1.37    --   -4.95 -99.00  30.00   84
 10  ω    -15.00  29.00   0.50    1.37    --   -4.95 -99.00 120.00   88
 11  ω    -18.00  23.00   0.50    1.37    --   -4.95 -99.00 -30.00   82
 12  ω    -14.00  25.00   0.50    1.37    --   -4.95 -99.00-150.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0301763000
_diffrn_orient_matrix_UB_12      0.0046716000
_diffrn_orient_matrix_UB_13      0.0397376000
_diffrn_orient_matrix_UB_21      -0.0278926000
_diffrn_orient_matrix_UB_22      -0.0492860000
_diffrn_orient_matrix_UB_23      0.0403277000
_diffrn_orient_matrix_UB_31      0.0507844000
_diffrn_orient_matrix_UB_32      -0.0424306000
_diffrn_orient_matrix_UB_33      -0.0075504000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5418
_reflns_number_total             8744
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT n/a (Sheldrick, 2015)'
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         8744
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0431
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0369P)²+0.2204P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.1082
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C1A \\sim N1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
C1 \\sim C2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
3. Others
 1*[Sof(Br1)]+1*[Sof(Br1B)]+1*[Sof(Br1A)]=1 with esd of 0.0001
 Sof(H1BD)=Sof(H1BE)=Sof(H1BF)=Sof(C1A)=Sof(H1AD)=Sof(H1AE)=Sof(C2A)=Sof(H2AA)=
 Sof(H2AB)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=
 Sof(H2B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C8(H8A,H8B), C11(H11A,H11B), C12(H12A,H12B), C9(H9A,H9B),
 C14(H14A,H14B), C3(H3A,H3B), C13(H13A,H13B), C7(H7A,H7B), C4(H4A,H4B), C6(H6A,
 H6B), C5(H5A,H5B), C1A(H1AD,H1AE), C1(H1A,H1B), C2(H2A,H2B), C2A(H2AA,H2AB)
4.b Idealised Me refined as rotating group:
 N1(H1BD,H1BE,H1BF), N1(H1AA,H1AB,H1AC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.13389(3) 0.46427(3) 0.88322(3) 0.03805(10) Uani 1 1 d . . . . .
S1 S 0.10055(6) 0.33946(6) 0.81744(6) 0.04218(16) Uani 1 1 d . . . . .
S3 S 0.20780(6) 0.07248(6) 0.86682(6) 0.04444(17) Uani 1 1 d . . . . .
S9 S 0.05431(6) 0.84335(6) 0.92193(6) 0.04521(17) Uani 1 1 d . . . . .
S4 S 0.35681(6) 0.06277(6) 1.02492(6) 0.04473(17) Uani 1 1 d . . . . .
S2 S 0.26495(6) 0.32824(6) 0.98890(6) 0.04681(18) Uani 1 1 d . . . . .
S7 S 0.16061(7) 0.58119(6) 0.95835(6) 0.04821(18) Uani 1 1 d . . . . .
S6 S 0.01163(7) 0.60787(6) 0.77217(6) 0.04985(19) Uani 1 1 d . . . . .
S8 S -0.07955(7) 0.87154(6) 0.74739(7) 0.0565(2) Uani 1 1 d . . . . .
S5 S 0.36367(8) -0.16290(6) 0.98862(7) 0.0589(2) Uani 1 1 d . . . . .
S10 S -0.09480(8) 1.08369(7) 0.80836(8) 0.0658(2) Uani 1 1 d . . . . .
Br1A Br 0.07731(7) 0.14507(9) 0.53935(10) 0.0801(4) Uani 0.531(2) 1 d . . P A 3
O5 O 0.35984(17) 0.39331(19) 0.61877(17) 0.0554(5) Uani 1 1 d . . . . .
O6 O 0.56854(18) 0.22064(19) 0.62512(16) 0.0592(5) Uani 1 1 d . . . . .
O4 O 0.25660(18) 0.5340(2) 0.42144(18) 0.0625(6) Uani 1 1 d . . . . .
O1 O 0.64315(18) 0.1417(2) 0.45767(18) 0.0637(6) Uani 1 1 d . . . . .
N1 N 0.3994(2) 0.2917(2) 0.4607(2) 0.0541(6) Uani 1 1 d . U . . .
H1BD H 0.447752 0.270777 0.410995 0.065 Uiso 0.455(11) 1 calc R U P B 2
H1BE H 0.445546 0.304382 0.501526 0.065 Uiso 0.455(11) 1 calc R U P B 2
H1BF H 0.348110 0.360220 0.428689 0.065 Uiso 0.455(11) 1 calc R U P B 2
H1AA H 0.479223 0.261292 0.462034 0.065 Uiso 0.545(11) 1 calc R U P B 1
H1AB H 0.375083 0.312485 0.516671 0.065 Uiso 0.545(11) 1 calc R U P B 1
H1AC H 0.386836 0.357847 0.399870 0.065 Uiso 0.545(11) 1 calc R U P B 1
O3 O 0.3213(2) 0.4646(2) 0.25369(19) 0.0723(7) Uani 1 1 d . . . . .
O2 O 0.5437(2) 0.3063(3) 0.26358(19) 0.0833(8) Uani 1 1 d . . . . .
C19 C 0.0701(2) 0.7161(2) 0.8904(2) 0.0391(6) Uani 1 1 d . . . . .
C15 C 0.1976(2) 0.2080(2) 0.8851(2) 0.0380(6) Uani 1 1 d . . . . .
C16 C 0.2675(2) 0.2031(2) 0.9594(2) 0.0366(6) Uani 1 1 d . . . . .
C18 C 0.0056(2) 0.7275(2) 0.8096(2) 0.0417(6) Uani 1 1 d . . . . .
C20 C -0.0430(2) 0.9404(2) 0.8247(2) 0.0475(7) Uani 1 1 d . . . . .
C17 C 0.3121(2) -0.0168(2) 0.9615(2) 0.0422(6) Uani 1 1 d . . . . .
C10 C 0.3030(3) 0.5181(3) 0.5889(3) 0.0617(8) Uani 1 1 d . . . . .
H10A H 0.363591 0.572361 0.550272 0.074 Uiso 1 1 calc R U . . .
H10B H 0.269820 0.532930 0.652849 0.074 Uiso 1 1 calc R U . . .
C8 C 0.1751(3) 0.5701(3) 0.3421(3) 0.0679(9) Uani 1 1 d . . . . .
H8A H 0.127603 0.649611 0.333514 0.081 Uiso 1 1 calc R U . . .
H8B H 0.118374 0.511124 0.363593 0.081 Uiso 1 1 calc R U . . .
C11 C 0.4484(3) 0.3601(3) 0.6944(3) 0.0625(8) Uani 1 1 d . . . . .
H11A H 0.408964 0.369438 0.759453 0.075 Uiso 1 1 calc R U . . .
H11B H 0.511253 0.413266 0.664387 0.075 Uiso 1 1 calc R U . . .
C12 C 0.5056(3) 0.2299(3) 0.7203(3) 0.0640(9) Uani 1 1 d . . . . .
H12A H 0.562858 0.204252 0.775047 0.077 Uiso 1 1 calc R U . . .
H12B H 0.442489 0.176989 0.747904 0.077 Uiso 1 1 calc R U . . .
C9 C 0.2030(3) 0.5434(3) 0.5196(3) 0.0675(9) Uani 1 1 d . . . . .
H9A H 0.146053 0.484539 0.555554 0.081 Uiso 1 1 calc R U . . .
H9B H 0.157882 0.625242 0.505173 0.081 Uiso 1 1 calc R U . . .
C14 C 0.7182(3) 0.1164(3) 0.5410(3) 0.0744(10) Uani 1 1 d . . . . .
H14A H 0.766543 0.182195 0.520982 0.089 Uiso 1 1 calc R U . . .
H14B H 0.774476 0.040487 0.552319 0.089 Uiso 1 1 calc R U . . .
C3 C 0.7104(3) 0.1720(3) 0.3552(3) 0.0720(10) Uani 1 1 d . . . . .
H3A H 0.773754 0.103594 0.356386 0.086 Uiso 1 1 calc R U . . .
H3B H 0.750350 0.242690 0.338871 0.086 Uiso 1 1 calc R U . . .
C13 C 0.6394(3) 0.1051(3) 0.6412(3) 0.0758(10) Uani 1 1 d . . . . .
H13A H 0.585859 0.044183 0.658225 0.091 Uiso 1 1 calc R U . . .
H13B H 0.689959 0.079390 0.700707 0.091 Uiso 1 1 calc R U . . .
C7 C 0.2442(3) 0.5775(3) 0.2398(3) 0.0661(9) Uani 1 1 d . . . . .
H7A H 0.187322 0.596095 0.186226 0.079 Uiso 1 1 calc R U . . .
H7B H 0.293884 0.643085 0.214173 0.079 Uiso 1 1 calc R U . . .
C4 C 0.6292(4) 0.1995(4) 0.2728(3) 0.0841(12) Uani 1 1 d . . . . .
H4A H 0.677068 0.212300 0.204429 0.101 Uiso 1 1 calc R U . . .
H4B H 0.585524 0.130711 0.291163 0.101 Uiso 1 1 calc R U . . .
C6 C 0.4021(4) 0.4712(4) 0.1609(3) 0.0881(13) Uani 1 1 d . . . . .
H6A H 0.458354 0.528639 0.147567 0.106 Uiso 1 1 calc R U . . .
H6B H 0.354735 0.501146 0.098811 0.106 Uiso 1 1 calc R U . . .
C5 C 0.4720(4) 0.3509(5) 0.1754(3) 0.1153(18) Uani 1 1 d . . . . .
H5A H 0.415770 0.293860 0.187249 0.138 Uiso 1 1 calc R U . . .
H5B H 0.525139 0.356853 0.110684 0.138 Uiso 1 1 calc R U . . .
C1A C 0.3258(15) 0.1890(16) 0.5307(14) 0.101(4) Uani 0.455(11) 1 d . U P B 2
H1AD H 0.330098 0.139709 0.489313 0.121 Uiso 0.455(11) 1 calc R U P B 2
H1AE H 0.374309 0.138581 0.591361 0.121 Uiso 0.455(11) 1 calc R U P B 2
C1 C 0.3299(15) 0.2001(13) 0.4667(15) 0.129(5) Uani 0.545(11) 1 d . U P B 1
H1A H 0.370587 0.167365 0.414251 0.155 Uiso 0.545(11) 1 calc R U P B 1
H1B H 0.339360 0.133532 0.537038 0.155 Uiso 0.545(11) 1 calc R U P B 1
Br1B Br 0.10514(14) 0.2286(2) 0.47475(18) 0.0743(8) Uani 0.2509(18) 1 d . . P B
2
Br1 Br 0.1205(3) 0.2049(3) 0.5681(3) 0.1155(15) Uani 0.218(2) 1 d . . P B 1
C2 C 0.2130(8) 0.2247(9) 0.4526(9) 0.137(6) Uani 0.545(11) 1 d . U P B 1
H2A H 0.194341 0.172217 0.421243 0.164 Uiso 0.545(11) 1 calc R U P B 1
H2B H 0.194563 0.309227 0.401802 0.164 Uiso 0.545(11) 1 calc R U P B 1
C2A C 0.2150(12) 0.1958(13) 0.5713(12) 0.113(5) Uani 0.455(11) 1 d . . P B 2
H2AA H 0.198871 0.259876 0.598745 0.136 Uiso 0.455(11) 1 calc R U P B 2
H2AB H 0.203861 0.118600 0.631493 0.136 Uiso 0.455(11) 1 calc R U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S1 2.1668(7) . ?
Ni1 S2 2.1563(7) . ?
Ni1 S7 2.1514(8) . ?
Ni1 S6 2.1649(7) . ?
S1 C15 1.719(2) . ?
S3 C15 1.740(2) . ?
S3 C17 1.732(3) . ?
S9 C19 1.736(2) . ?
S9 C20 1.723(3) . ?
S4 C16 1.736(2) . ?
S4 C17 1.719(3) . ?
S2 C16 1.717(2) . ?
S7 C19 1.708(2) . ?
S6 C18 1.712(3) . ?
S8 C18 1.737(2) . ?
S8 C20 1.728(3) . ?
S5 C17 1.645(2) . ?
S10 C20 1.645(3) . ?
O5 C10 1.425(4) . ?
O5 C11 1.422(4) . ?
O6 C12 1.418(4) . ?
O6 C13 1.407(4) . ?
O4 C8 1.396(4) . ?
O4 C9 1.424(4) . ?
O1 C14 1.415(4) . ?
O1 C3 1.420(4) . ?
N1 H1BD 0.8900 . ?
N1 H1BE 0.8900 . ?
N1 H1BF 0.8900 . ?
N1 H1AA 0.8900 . ?
N1 H1AB 0.8900 . ?
N1 H1AC 0.8900 . ?
N1 C1A 1.517(16) . ?
N1 C1 1.443(13) . ?
O3 C7 1.415(4) . ?
O3 C6 1.420(4) . ?
O2 C4 1.414(4) . ?
O2 C5 1.406(4) . ?
C19 C18 1.357(4) . ?
C15 C16 1.350(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C9 1.478(5) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C7 1.467(5) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.488(5) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C13 1.479(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.445(5) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C5 1.455(6) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C1A H1AD 0.9700 . ?
C1A H1AE 0.9700 . ?
C1A C2A 1.272(19) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.300(17) . ?
Br1B C2A 1.810(13) . ?
Br1 C2 1.700(13) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S2 Ni1 S1 93.21(3) . . ?
S2 Ni1 S6 176.34(3) . . ?
S7 Ni1 S1 176.21(3) . . ?
S7 Ni1 S2 85.54(3) . . ?
S7 Ni1 S6 92.91(3) . . ?
S6 Ni1 S1 88.54(3) . . ?
C15 S1 Ni1 101.84(9) . . ?
C17 S3 C15 97.19(12) . . ?
C20 S9 C19 97.05(13) . . ?
C17 S4 C16 97.45(12) . . ?
C16 S2 Ni1 102.07(9) . . ?
C19 S7 Ni1 102.71(9) . . ?
C18 S6 Ni1 101.97(9) . . ?
C20 S8 C18 97.84(13) . . ?
C11 O5 C10 111.8(2) . . ?
C13 O6 C12 114.2(2) . . ?
C8 O4 C9 115.1(2) . . ?
C14 O1 C3 112.6(3) . . ?
H1BD N1 H1BE 109.5 . . ?
H1BD N1 H1BF 109.5 . . ?
H1BE N1 H1BF 109.5 . . ?
H1AA N1 H1AB 109.5 . . ?
H1AA N1 H1AC 109.5 . . ?
H1AB N1 H1AC 109.5 . . ?
C1A N1 H1BD 109.5 . . ?
C1A N1 H1BE 109.5 . . ?
C1A N1 H1BF 109.5 . . ?
C1 N1 H1AA 109.5 . . ?
C1 N1 H1AB 109.5 . . ?
C1 N1 H1AC 109.5 . . ?
C7 O3 C6 112.6(3) . . ?
C5 O2 C4 114.3(3) . . ?
S7 C19 S9 122.08(16) . . ?
C18 C19 S9 117.01(18) . . ?
C18 C19 S7 120.91(19) . . ?
S1 C15 S3 122.68(16) . . ?
C16 C15 S1 121.31(19) . . ?
C16 C15 S3 115.96(18) . . ?
S2 C16 S4 122.15(15) . . ?
C15 C16 S4 116.27(18) . . ?
C15 C16 S2 121.56(18) . . ?
S6 C18 S8 123.54(16) . . ?
C19 C18 S6 121.49(18) . . ?
C19 C18 S8 114.96(19) . . ?
S9 C20 S8 113.10(14) . . ?
S10 C20 S9 122.75(18) . . ?
S10 C20 S8 124.15(17) . . ?
S4 C17 S3 113.12(14) . . ?
S5 C17 S3 123.83(17) . . ?
S5 C17 S4 123.06(16) . . ?
O5 C10 H10A 109.8 . . ?
O5 C10 H10B 109.8 . . ?
O5 C10 C9 109.3(3) . . ?
H10A C10 H10B 108.3 . . ?
C9 C10 H10A 109.8 . . ?
C9 C10 H10B 109.8 . . ?
O4 C8 H8A 109.7 . . ?
O4 C8 H8B 109.7 . . ?
O4 C8 C7 109.7(2) . . ?
H8A C8 H8B 108.2 . . ?
C7 C8 H8A 109.7 . . ?
C7 C8 H8B 109.7 . . ?
O5 C11 H11A 109.9 . . ?
O5 C11 H11B 109.9 . . ?
O5 C11 C12 108.9(3) . . ?
H11A C11 H11B 108.3 . . ?
C12 C11 H11A 109.9 . . ?
C12 C11 H11B 109.9 . . ?
O6 C12 C11 108.6(3) . . ?
O6 C12 H12A 110.0 . . ?
O6 C12 H12B 110.0 . . ?
C11 C12 H12A 110.0 . . ?
C11 C12 H12B 110.0 . . ?
H12A C12 H12B 108.4 . . ?
O4 C9 C10 108.3(2) . . ?
O4 C9 H9A 110.0 . . ?
O4 C9 H9B 110.0 . . ?
C10 C9 H9A 110.0 . . ?
C10 C9 H9B 110.0 . . ?
H9A C9 H9B 108.4 . . ?
O1 C14 H14A 109.8 . . ?
O1 C14 H14B 109.8 . . ?
O1 C14 C13 109.3(3) . . ?
H14A C14 H14B 108.3 . . ?
C13 C14 H14A 109.8 . . ?
C13 C14 H14B 109.8 . . ?
O1 C3 H3A 109.6 . . ?
O1 C3 H3B 109.6 . . ?
O1 C3 C4 110.4(3) . . ?
H3A C3 H3B 108.1 . . ?
C4 C3 H3A 109.6 . . ?
C4 C3 H3B 109.6 . . ?
O6 C13 C14 108.1(3) . . ?
O6 C13 H13A 110.1 . . ?
O6 C13 H13B 110.1 . . ?
C14 C13 H13A 110.1 . . ?
C14 C13 H13B 110.1 . . ?
H13A C13 H13B 108.4 . . ?
O3 C7 C8 110.1(3) . . ?
O3 C7 H7A 109.6 . . ?
O3 C7 H7B 109.6 . . ?
C8 C7 H7A 109.6 . . ?
C8 C7 H7B 109.6 . . ?
H7A C7 H7B 108.2 . . ?
O2 C4 C3 109.9(3) . . ?
O2 C4 H4A 109.7 . . ?
O2 C4 H4B 109.7 . . ?
C3 C4 H4A 109.7 . . ?
C3 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
O3 C6 H6A 109.5 . . ?
O3 C6 H6B 109.5 . . ?
O3 C6 C5 110.7(4) . . ?
H6A C6 H6B 108.1 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
O2 C5 C6 110.8(3) . . ?
O2 C5 H5A 109.5 . . ?
O2 C5 H5B 109.5 . . ?
C6 C5 H5A 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
N1 C1A H1AD 105.0 . . ?
N1 C1A H1AE 105.0 . . ?
H1AD C1A H1AE 105.8 . . ?
C2A C1A N1 129.2(15) . . ?
C2A C1A H1AD 105.0 . . ?
C2A C1A H1AE 105.0 . . ?
N1 C1 H1A 106.7 . . ?
N1 C1 H1B 106.7 . . ?
H1A C1 H1B 106.6 . . ?
C2 C1 N1 122.4(13) . . ?
C2 C1 H1A 106.7 . . ?
C2 C1 H1B 106.7 . . ?
C1 C2 Br1 113.6(10) . . ?
C1 C2 H2A 108.8 . . ?
C1 C2 H2B 108.8 . . ?
Br1 C2 H2A 108.8 . . ?
Br1 C2 H2B 108.8 . . ?
H2A C2 H2B 107.7 . . ?
C1A C2A Br1B 112.5(10) . . ?
C1A C2A H2AA 109.1 . . ?
C1A C2A H2AB 109.1 . . ?
Br1B C2A H2AA 109.1 . . ?
Br1B C2A H2AB 109.1 . . ?
H2AA C2A H2AB 107.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S1 C15 S3 178.52(13) . . . . ?
Ni1 S1 C15 C16 1.1(2) . . . . ?
Ni1 S2 C16 S4 -178.35(13) . . . . ?
Ni1 S2 C16 C15 0.2(2) . . . . ?
Ni1 S7 C19 S9 178.26(14) . . . . ?
Ni1 S7 C19 C18 -0.8(2) . . . . ?
Ni1 S6 C18 S8 179.56(15) . . . . ?
Ni1 S6 C18 C19 0.7(3) . . . . ?
S1 C15 C16 S4 177.66(13) . . . . ?
S1 C15 C16 S2 -0.9(3) . . . . ?
S3 C15 C16 S4 0.1(3) . . . . ?
S3 C15 C16 S2 -178.49(14) . . . . ?
S9 C19 C18 S6 -179.08(15) . . . . ?
S9 C19 C18 S8 2.0(3) . . . . ?
S7 C19 C18 S6 0.0(3) . . . . ?
S7 C19 C18 S8 -178.86(14) . . . . ?
O5 C10 C9 O4 -65.8(3) . . . . ?
O5 C11 C12 O6 62.9(3) . . . . ?
O4 C8 C7 O3 54.7(4) . . . . ?
O1 C14 C13 O6 -65.6(4) . . . . ?
O1 C3 C4 O2 64.8(4) . . . . ?
N1 C1A C2A Br1B 79.5(15) . . . . ?
N1 C1 C2 Br1 -89.5(15) . . . . ?
O3 C6 C5 O2 -60.5(5) . . . . ?
C19 S9 C20 S8 0.83(18) . . . . ?
C19 S9 C20 S10 -179.15(18) . . . . ?
C15 S3 C17 S4 -0.71(17) . . . . ?
C15 S3 C17 S5 179.25(18) . . . . ?
C16 S4 C17 S3 0.76(17) . . . . ?
C16 S4 C17 S5 -179.20(18) . . . . ?
C18 S8 C20 S9 0.03(18) . . . . ?
C18 S8 C20 S10 -179.99(19) . . . . ?
C20 S9 C19 S7 179.15(17) . . . . ?
C20 S9 C19 C18 -1.7(2) . . . . ?
C20 S8 C18 S6 179.90(18) . . . . ?
C20 S8 C18 C19 -1.2(2) . . . . ?
C17 S3 C15 S1 -177.14(16) . . . . ?
C17 S3 C15 C16 0.4(2) . . . . ?
C17 S4 C16 S2 178.06(17) . . . . ?
C17 S4 C16 C15 -0.5(2) . . . . ?
C10 O5 C11 C12 -178.9(2) . . . . ?
C8 O4 C9 C10 -172.6(3) . . . . ?
C11 O5 C10 C9 -174.0(2) . . . . ?
C12 O6 C13 C14 -168.8(3) . . . . ?
C9 O4 C8 C7 169.9(3) . . . . ?
C14 O1 C3 C4 -178.8(3) . . . . ?
C3 O1 C14 C13 171.2(3) . . . . ?
C13 O6 C12 C11 172.6(3) . . . . ?
C7 O3 C6 C5 -175.1(3) . . . . ?
C4 O2 C5 C6 -170.3(4) . . . . ?
C6 O3 C7 C8 -172.4(3) . . . . ?
C5 O2 C4 C3 171.4(4) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.173
_oxdiff_exptl_absorpt_empirical_full_min 0.366
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_133k
_database_code_depnum_ccdc_archive 'CCDC 2053300'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-18 downloaded from the CCDC.
;
_audit_creation_date             2020-11-10
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C2 H7 Br1 N, C12 H24 O6'
_chemical_formula_sum            'C20 H31 Br N Ni O6 S10'
_chemical_formula_weight         840.68
_chemical_melting_point          ?
_chemical_oxdiff_formula         BrC20H31NO6NiS10
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.0117(3)
_cell_length_b                   12.0652(3)
_cell_length_c                   13.7791(4)
_cell_angle_alpha                115.895(3)
_cell_angle_beta                 91.351(2)
_cell_angle_gamma                101.004(2)
_cell_volume                     1604.68(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    19815
_cell_measurement_temperature    133
_cell_measurement_theta_max      31.2050
_cell_measurement_theta_min      1.9130
_shelx_estimated_absorpt_T_max   0.786
_shelx_estimated_absorpt_T_min   0.631
_exptl_absorpt_coefficient_mu    2.537
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54335
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             858
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.830
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            38326
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.830
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.917
_diffrn_reflns_theta_min         1.892
_diffrn_ambient_temperature      133
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.830
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -69.00  19.00   0.50    0.77    --    5.18 -28.00  51.29  176
  2  ω    -63.00  19.00   0.50    0.77    --    5.18 -28.00 120.90  164
  3  ω    -56.00  18.00   0.50    0.77    --    5.18 -19.00 -30.00  148
  4  ω    -22.00  19.00   0.50    0.77    --    5.18 -20.00 -76.51   82
  5  ω    -62.00  19.00   0.50    0.77    --    5.18 -33.00-104.04  162
  6  ω    -70.00 -44.00   0.50    0.77    --    5.18 -20.00 -76.51   52
  7  ω    -66.00  18.00   0.50    0.77    --    5.18 -34.00-163.07  168
  8  ω    -18.00  29.00   0.50    0.77    --   -4.95 -99.00 150.00   94
  9  ω    -18.00  23.00   0.50    0.77    --   -4.95 -99.00  90.00   82
 10  ω     -8.00  23.00   0.50    0.77    --   -4.95 -99.00   0.00   62
 11  ω    -12.00  24.00   0.50    0.77    --   -4.95 -99.00 -60.00   72
 12  ω    -18.00  26.00   0.50    0.77    --   -4.95 -99.00-120.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0307990000
_diffrn_orient_matrix_UB_12      -0.0434757000
_diffrn_orient_matrix_UB_13      -0.0382843000
_diffrn_orient_matrix_UB_21      -0.0299683000
_diffrn_orient_matrix_UB_22      0.0069898000
_diffrn_orient_matrix_UB_23      -0.0424709000
_diffrn_orient_matrix_UB_31      0.0502334000
_diffrn_orient_matrix_UB_32      0.0505636000
_diffrn_orient_matrix_UB_33      0.0073224000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6316
_reflns_number_total             8423
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT n/a (Sheldrick, 2015)'
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         8423
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0325
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0305P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0728
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
N1 \\sim C1A \\sim C2A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.01 within 2A
3. Others
 1*[Sof(Br1B)]+1*[Sof(Br1A)]+1*[Sof(Br1)]=1 with esd of 0.0001
 Sof(H1BD)=Sof(H1BE)=Sof(H1BF)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C1A)=Sof(H1AD)=
 Sof(H1AE)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C1)=Sof(H1A)=
 Sof(H1B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C3(H3A,H3B), C12(H12A,H12B), C8(H8A,H8B), C9(H9A,H9B),
 C33(H33A,H33B), C32(H32A,H32B), C10(H10A,H10B), C7(H7A,H7B), C4(H4A,H4B),
 C2(H2A,H2B), C6(H6A,H6B), C5(H5A,H5B), C1(H1A,H1B), C2A(H2AA,H2AB), C1A(H1AD,
 H1AE)
4.b Idealised Me refined as rotating group:
 N1(H1AA,H1AB,H1AC), N1(H1BD,H1BE,H1BF)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.13868(2) 0.14926(2) 0.11385(2) 0.01765(7) Uani 1 1 d . . . . .
Br1B Br 0.10558(3) 0.80400(3) 0.52710(3) 0.03151(12) Uani 0.8800(14) 1 d . . P
A 1
S1 S 0.10508(4) 0.33857(4) 0.17832(4) 0.01928(11) Uani 1 1 d . . . . .
S2 S 0.26800(5) 0.18064(4) 0.00779(4) 0.02184(12) Uani 1 1 d . . . . .
S3 S 0.21040(4) 0.55669(4) 0.12797(4) 0.01965(11) Uani 1 1 d . . . . .
S4 S 0.35780(5) 0.41132(4) -0.02956(4) 0.01974(11) Uani 1 1 d . . . . .
S7 S 0.16642(5) -0.04101(4) 0.04162(4) 0.02184(12) Uani 1 1 d . . . . .
S5 S 0.36436(5) 0.67494(5) 0.00804(5) 0.02532(13) Uani 1 1 d . . . . .
S9 S 0.05929(5) -0.26696(4) 0.07906(4) 0.02058(11) Uani 1 1 d . . . . .
S8 S -0.07434(5) -0.12249(5) 0.25160(5) 0.02582(13) Uani 1 1 d . . . . .
S6 S 0.01404(5) 0.11500(5) 0.22226(5) 0.02361(12) Uani 1 1 d . . . . .
S10 S -0.08346(5) -0.39279(5) 0.19792(5) 0.02853(13) Uani 1 1 d . . . . .
O6 O 0.57741(13) 0.65159(13) 0.37348(12) 0.0239(3) Uani 1 1 d . . . . .
O5 O 0.36564(12) 0.48520(13) 0.37803(12) 0.0241(3) Uani 1 1 d . . . . .
O1 O 0.64552(13) 0.90014(13) 0.53693(12) 0.0249(3) Uani 1 1 d . . . . .
O4 O 0.25669(12) 0.54223(14) 0.57225(13) 0.0275(3) Uani 1 1 d . . . . .
O2 O 0.54344(14) 0.93381(14) 0.73024(13) 0.0322(4) Uani 1 1 d . . . . .
O3 O 0.31397(13) 0.78455(14) 0.73497(13) 0.0296(4) Uani 1 1 d . . . . .
N1 N 0.39563(15) 0.74521(16) 0.52590(15) 0.0241(4) Uani 1 1 d . U . . .
H1AA H 0.391844 0.660662 0.490882 0.029 Uiso 0.911(4) 1 calc R U P B 1
H1AB H 0.350751 0.762410 0.583350 0.029 Uiso 0.911(4) 1 calc R U P B 1
H1AC H 0.476429 0.787648 0.550131 0.029 Uiso 0.911(4) 1 calc R U P B 1
H1BD H 0.348485 0.673953 0.470590 0.029 Uiso 0.089(4) 1 calc R U P B 2
H1BE H 0.384320 0.742616 0.590142 0.029 Uiso 0.089(4) 1 calc R U P B 2
H1BF H 0.477445 0.750093 0.515657 0.029 Uiso 0.089(4) 1 calc R U P B 2
C13 C 0.20076(17) 0.40291(17) 0.11069(17) 0.0174(4) Uani 1 1 d . . . . .
C15 C 0.31290(17) 0.55358(17) 0.03372(16) 0.0180(4) Uani 1 1 d . . . . .
C14 C 0.26983(17) 0.33498(17) 0.03605(17) 0.0188(4) Uani 1 1 d . . . . .
C17 C 0.07380(17) -0.10885(17) 0.10812(17) 0.0182(4) Uani 1 1 d . . . . .
C18 C -0.03511(18) -0.26701(18) 0.17744(18) 0.0214(4) Uani 1 1 d . . . . .
C11 C 0.4564(2) 0.44256(19) 0.30615(19) 0.0262(5) Uani 1 1 d . . . . .
H11A H 0.416162 0.365566 0.239604 0.031 Uiso 1 1 calc R U . . .
H11B H 0.521122 0.421271 0.341925 0.031 Uiso 1 1 calc R U . . .
C16 C 0.00918(18) -0.04090(18) 0.18742(18) 0.0206(4) Uani 1 1 d . . . . .
C3 C 0.7135(2) 0.9764(2) 0.6420(2) 0.0293(5) Uani 1 1 d . . . . .
H3A H 0.778735 1.044026 0.639949 0.035 Uiso 1 1 calc R U . . .
H3B H 0.754738 0.924048 0.664803 0.035 Uiso 1 1 calc R U . . .
C12 C 0.5150(2) 0.5445(2) 0.27687(18) 0.0272(5) Uani 1 1 d . . . . .
H12A H 0.575233 0.514555 0.224306 0.033 Uiso 1 1 calc R U . . .
H12B H 0.450293 0.567623 0.242828 0.033 Uiso 1 1 calc R U . . .
C8 C 0.16856(19) 0.5870(2) 0.6459(2) 0.0293(5) Uani 1 1 d . . . . .
H8A H 0.117199 0.516474 0.655478 0.035 Uiso 1 1 calc R U . . .
H8B H 0.112591 0.623918 0.617250 0.035 Uiso 1 1 calc R U . . .
C9 C 0.2044(2) 0.4334(2) 0.4741(2) 0.0297(5) Uani 1 1 d . . . . .
H9A H 0.145518 0.453603 0.432221 0.036 Uiso 1 1 calc R U . . .
H9B H 0.158441 0.365502 0.490117 0.036 Uiso 1 1 calc R U . . .
C33 C 0.72536(19) 0.8451(2) 0.4575(2) 0.0297(5) Uani 1 1 d . . . . .
H33A H 0.778375 0.803843 0.483894 0.036 Uiso 1 1 calc R U . . .
H33B H 0.780475 0.911890 0.445440 0.036 Uiso 1 1 calc R U . . .
C32 C 0.6483(2) 0.7498(2) 0.35327(19) 0.0292(5) Uani 1 1 d . . . . .
H32A H 0.592062 0.789483 0.328176 0.035 Uiso 1 1 calc R U . . .
H32B H 0.702674 0.714991 0.296370 0.035 Uiso 1 1 calc R U . . .
C10 C 0.3085(2) 0.39071(19) 0.40988(19) 0.0283(5) Uani 1 1 d . . . . .
H10A H 0.370959 0.377696 0.454404 0.034 Uiso 1 1 calc R U . . .
H10B H 0.275737 0.309462 0.344563 0.034 Uiso 1 1 calc R U . . .
C7 C 0.2395(2) 0.6853(2) 0.7521(2) 0.0307(5) Uani 1 1 d . . . . .
H7A H 0.180881 0.719390 0.805104 0.037 Uiso 1 1 calc R U . . .
H7B H 0.293434 0.647508 0.781614 0.037 Uiso 1 1 calc R U . . .
C4 C 0.6269(2) 1.0333(2) 0.7209(2) 0.0319(5) Uani 1 1 d . . . . .
H4A H 0.674340 1.093729 0.792534 0.038 Uiso 1 1 calc R U . . .
H4B H 0.579858 1.079534 0.695079 0.038 Uiso 1 1 calc R U . . .
C2 C 0.2066(2) 0.7302(2) 0.4121(2) 0.0268(6) Uani 0.911(4) 1 d . . P A 1
H2A H 0.190465 0.637898 0.387728 0.032 Uiso 0.911(4) 1 calc R U P B 1
H2B H 0.182258 0.744136 0.349389 0.032 Uiso 0.911(4) 1 calc R U P B 1
C6 C 0.3970(2) 0.8717(2) 0.8309(2) 0.0395(6) Uani 1 1 d . . . . .
H6A H 0.457288 0.828674 0.846738 0.047 Uiso 1 1 calc R U . . .
H6B H 0.349231 0.902962 0.893697 0.047 Uiso 1 1 calc R U . . .
C5 C 0.4654(2) 0.9804(2) 0.8137(2) 0.0450(7) Uani 1 1 d . . . . .
H5A H 0.405257 1.019202 0.791792 0.054 Uiso 1 1 calc R U . . .
H5B H 0.516599 1.045641 0.881868 0.054 Uiso 1 1 calc R U . . .
C1 C 0.3426(2) 0.7863(2) 0.4490(2) 0.0256(6) Uani 0.911(4) 1 d . . P A 1
H1A H 0.388485 0.762103 0.384495 0.031 Uiso 0.911(4) 1 calc R U P B 1
H1B H 0.356090 0.879572 0.485031 0.031 Uiso 0.911(4) 1 calc R U P B 1
Br1A Br 0.0732(5) 0.8234(5) 0.4706(6) 0.058(2) Uani 0.0615(14) 1 d . . P C 3
C2A C 0.220(2) 0.847(3) 0.553(2) 0.034(6) Uani 0.089(4) 1 d . U P B 2
H2AA H 0.201406 0.931022 0.573460 0.041 Uiso 0.089(4) 1 calc R U P B 2
H2AB H 0.207098 0.826283 0.614713 0.041 Uiso 0.089(4) 1 calc R U P B 2
Br1 Br 0.1164(5) 0.7245(5) 0.4284(5) 0.056(2) Uani 0.0584(11) 1 d . . P B 2
C1A C 0.360(3) 0.850(3) 0.528(3) 0.044(5) Uani 0.089(4) 1 d . U P B 2
H1AD H 0.367938 0.850867 0.456684 0.053 Uiso 0.089(4) 1 calc R U P B 2
H1AE H 0.415412 0.928157 0.584258 0.053 Uiso 0.089(4) 1 calc R U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S1 2.1700(5) . ?
Ni1 S2 2.1640(5) . ?
Ni1 S7 2.1541(5) . ?
Ni1 S6 2.1692(6) . ?
Br1B C2 1.941(3) . ?
S1 C13 1.7166(19) . ?
S2 C14 1.7238(19) . ?
S3 C13 1.7459(18) . ?
S3 C15 1.733(2) . ?
S4 C15 1.729(2) . ?
S4 C14 1.7414(19) . ?
S7 C17 1.7118(19) . ?
S5 C15 1.6539(19) . ?
S9 C17 1.7431(18) . ?
S9 C18 1.728(2) . ?
S8 C18 1.739(2) . ?
S8 C16 1.7464(19) . ?
S6 C16 1.716(2) . ?
S10 C18 1.6551(19) . ?
O6 C12 1.424(3) . ?
O6 C32 1.427(2) . ?
O5 C11 1.430(3) . ?
O5 C10 1.437(2) . ?
O1 C3 1.423(3) . ?
O1 C33 1.430(3) . ?
O4 C8 1.425(3) . ?
O4 C9 1.417(3) . ?
O2 C4 1.422(2) . ?
O2 C5 1.429(3) . ?
O3 C7 1.430(2) . ?
O3 C6 1.432(3) . ?
N1 H1AA 0.9100 . ?
N1 H1AB 0.9100 . ?
N1 H1AC 0.9100 . ?
N1 H1BD 0.9100 . ?
N1 H1BE 0.9100 . ?
N1 H1BF 0.9100 . ?
N1 C1 1.500(3) . ?
N1 C1A 1.39(3) . ?
C13 C14 1.359(3) . ?
C17 C16 1.360(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.495(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.487(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C7 1.495(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.495(3) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C32 1.494(3) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C1 1.496(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C5 1.500(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2A H2AA 0.9900 . ?
C2A H2AB 0.9900 . ?
C2A Br1 1.87(3) . ?
C2A C1A 1.58(4) . ?
C1A H1AD 0.9900 . ?
C1A H1AE 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S2 Ni1 S1 93.49(2) . . ?
S2 Ni1 S6 177.87(2) . . ?
S7 Ni1 S1 176.89(3) . . ?
S7 Ni1 S2 85.50(2) . . ?
S7 Ni1 S6 93.18(2) . . ?
S6 Ni1 S1 87.91(2) . . ?
C13 S1 Ni1 101.60(7) . . ?
C14 S2 Ni1 101.89(7) . . ?
C15 S3 C13 97.51(9) . . ?
C15 S4 C14 97.25(9) . . ?
C17 S7 Ni1 102.35(7) . . ?
C18 S9 C17 97.06(10) . . ?
C18 S8 C16 97.44(10) . . ?
C16 S6 Ni1 101.84(7) . . ?
C32 O6 C12 113.07(16) . . ?
C11 O5 C10 111.16(16) . . ?
C33 O1 C3 111.55(16) . . ?
C9 O4 C8 114.07(16) . . ?
C4 O2 C5 112.03(17) . . ?
C6 O3 C7 110.58(18) . . ?
H1AA N1 H1AB 109.5 . . ?
H1AA N1 H1AC 109.5 . . ?
H1AB N1 H1AC 109.5 . . ?
H1BD N1 H1BE 109.5 . . ?
H1BD N1 H1BF 109.5 . . ?
H1BE N1 H1BF 109.5 . . ?
C1 N1 H1AA 109.5 . . ?
C1 N1 H1AB 109.5 . . ?
C1 N1 H1AC 109.5 . . ?
C1A N1 H1BD 109.5 . . ?
C1A N1 H1BE 109.5 . . ?
C1A N1 H1BF 109.5 . . ?
S1 C13 S3 122.54(12) . . ?
C14 C13 S1 121.91(14) . . ?
C14 C13 S3 115.48(14) . . ?
S4 C15 S3 113.16(10) . . ?
S5 C15 S3 123.55(12) . . ?
S5 C15 S4 123.29(12) . . ?
S2 C14 S4 122.32(12) . . ?
C13 C14 S2 121.08(15) . . ?
C13 C14 S4 116.60(14) . . ?
S7 C17 S9 121.86(12) . . ?
C16 C17 S7 121.28(14) . . ?
C16 C17 S9 116.85(14) . . ?
S9 C18 S8 113.26(11) . . ?
S10 C18 S9 123.02(13) . . ?
S10 C18 S8 123.72(13) . . ?
O5 C11 H11A 109.8 . . ?
O5 C11 H11B 109.8 . . ?
O5 C11 C12 109.30(17) . . ?
H11A C11 H11B 108.3 . . ?
C12 C11 H11A 109.8 . . ?
C12 C11 H11B 109.8 . . ?
S6 C16 S8 123.34(13) . . ?
C17 C16 S8 115.32(15) . . ?
C17 C16 S6 121.32(15) . . ?
O1 C3 H3A 109.8 . . ?
O1 C3 H3B 109.8 . . ?
O1 C3 C4 109.44(18) . . ?
H3A C3 H3B 108.2 . . ?
C4 C3 H3A 109.8 . . ?
C4 C3 H3B 109.8 . . ?
O6 C12 C11 108.43(18) . . ?
O6 C12 H12A 110.0 . . ?
O6 C12 H12B 110.0 . . ?
C11 C12 H12A 110.0 . . ?
C11 C12 H12B 110.0 . . ?
H12A C12 H12B 108.4 . . ?
O4 C8 H8A 110.1 . . ?
O4 C8 H8B 110.1 . . ?
O4 C8 C7 107.79(17) . . ?
H8A C8 H8B 108.5 . . ?
C7 C8 H8A 110.1 . . ?
C7 C8 H8B 110.1 . . ?
O4 C9 H9A 110.1 . . ?
O4 C9 H9B 110.1 . . ?
O4 C9 C10 108.08(17) . . ?
H9A C9 H9B 108.4 . . ?
C10 C9 H9A 110.1 . . ?
C10 C9 H9B 110.1 . . ?
O1 C33 H33A 109.8 . . ?
O1 C33 H33B 109.8 . . ?
O1 C33 C32 109.59(17) . . ?
H33A C33 H33B 108.2 . . ?
C32 C33 H33A 109.8 . . ?
C32 C33 H33B 109.8 . . ?
O6 C32 C33 107.40(18) . . ?
O6 C32 H32A 110.2 . . ?
O6 C32 H32B 110.2 . . ?
C33 C32 H32A 110.2 . . ?
C33 C32 H32B 110.2 . . ?
H32A C32 H32B 108.5 . . ?
O5 C10 C9 109.09(17) . . ?
O5 C10 H10A 109.9 . . ?
O5 C10 H10B 109.9 . . ?
C9 C10 H10A 109.9 . . ?
C9 C10 H10B 109.9 . . ?
H10A C10 H10B 108.3 . . ?
O3 C7 C8 108.65(19) . . ?
O3 C7 H7A 110.0 . . ?
O3 C7 H7B 110.0 . . ?
C8 C7 H7A 110.0 . . ?
C8 C7 H7B 110.0 . . ?
H7A C7 H7B 108.3 . . ?
O2 C4 C3 107.92(18) . . ?
O2 C4 H4A 110.1 . . ?
O2 C4 H4B 110.1 . . ?
C3 C4 H4A 110.1 . . ?
C3 C4 H4B 110.1 . . ?
H4A C4 H4B 108.4 . . ?
Br1B C2 H2A 109.3 . . ?
Br1B C2 H2B 109.3 . . ?
H2A C2 H2B 107.9 . . ?
C1 C2 Br1B 111.82(18) . . ?
C1 C2 H2A 109.3 . . ?
C1 C2 H2B 109.3 . . ?
O3 C6 H6A 109.8 . . ?
O3 C6 H6B 109.8 . . ?
O3 C6 C5 109.2(2) . . ?
H6A C6 H6B 108.3 . . ?
C5 C6 H6A 109.8 . . ?
C5 C6 H6B 109.8 . . ?
O2 C5 C6 108.3(2) . . ?
O2 C5 H5A 110.0 . . ?
O2 C5 H5B 110.0 . . ?
C6 C5 H5A 110.0 . . ?
C6 C5 H5B 110.0 . . ?
H5A C5 H5B 108.4 . . ?
N1 C1 C2 113.54(18) . . ?
N1 C1 H1A 108.9 . . ?
N1 C1 H1B 108.9 . . ?
C2 C1 H1A 108.9 . . ?
C2 C1 H1B 108.9 . . ?
H1A C1 H1B 107.7 . . ?
H2AA C2A H2AB 108.4 . . ?
Br1 C2A H2AA 110.1 . . ?
Br1 C2A H2AB 110.1 . . ?
C1A C2A H2AA 110.1 . . ?
C1A C2A H2AB 110.1 . . ?
C1A C2A Br1 108(2) . . ?
N1 C1A C2A 110(2) . . ?
N1 C1A H1AD 109.7 . . ?
N1 C1A H1AE 109.7 . . ?
C2A C1A H1AD 109.7 . . ?
C2A C1A H1AE 109.7 . . ?
H1AD C1A H1AE 108.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S1 C13 S3 178.54(10) . . . . ?
Ni1 S1 C13 C14 1.71(18) . . . . ?
Ni1 S2 C14 S4 -178.60(11) . . . . ?
Ni1 S2 C14 C13 0.69(18) . . . . ?
Ni1 S7 C17 S9 179.05(11) . . . . ?
Ni1 S7 C17 C16 -1.83(19) . . . . ?
Ni1 S6 C16 S8 177.88(11) . . . . ?
Ni1 S6 C16 C17 -0.60(19) . . . . ?
Br1B C2 C1 N1 72.3(2) . . . . ?
S1 C13 C14 S2 -1.7(3) . . . . ?
S1 C13 C14 S4 177.61(11) . . . . ?
S3 C13 C14 S2 -178.77(11) . . . . ?
S3 C13 C14 S4 0.6(2) . . . . ?
S7 C17 C16 S8 -176.86(11) . . . . ?
S7 C17 C16 S6 1.7(3) . . . . ?
S9 C17 C16 S8 2.3(2) . . . . ?
S9 C17 C16 S6 -179.09(11) . . . . ?
O5 C11 C12 O6 62.4(2) . . . . ?
O1 C3 C4 O2 65.8(2) . . . . ?
O1 C33 C32 O6 -63.4(2) . . . . ?
O4 C8 C7 O3 58.9(2) . . . . ?
O4 C9 C10 O5 -65.6(2) . . . . ?
O3 C6 C5 O2 -65.5(3) . . . . ?
C13 S3 C15 S4 -0.59(13) . . . . ?
C13 S3 C15 S5 -179.72(13) . . . . ?
C15 S3 C13 S1 -177.00(13) . . . . ?
C15 S3 C13 C14 0.02(17) . . . . ?
C15 S4 C14 S2 178.47(13) . . . . ?
C15 S4 C14 C13 -0.85(18) . . . . ?
C14 S4 C15 S3 0.82(13) . . . . ?
C14 S4 C15 S5 179.97(13) . . . . ?
C17 S9 C18 S8 2.04(13) . . . . ?
C17 S9 C18 S10 -178.26(14) . . . . ?
C18 S9 C17 S7 176.50(13) . . . . ?
C18 S9 C17 C16 -2.66(18) . . . . ?
C18 S8 C16 S6 -179.29(14) . . . . ?
C18 S8 C16 C17 -0.72(18) . . . . ?
C11 O5 C10 C9 -173.47(17) . . . . ?
C16 S8 C18 S9 -1.07(13) . . . . ?
C16 S8 C18 S10 179.24(14) . . . . ?
C3 O1 C33 C32 170.69(17) . . . . ?
C12 O6 C32 C33 -170.39(17) . . . . ?
C8 O4 C9 C10 -174.99(17) . . . . ?
C9 O4 C8 C7 169.54(18) . . . . ?
C33 O1 C3 C4 178.84(18) . . . . ?
C32 O6 C12 C11 173.50(17) . . . . ?
C10 O5 C11 C12 -178.95(17) . . . . ?
C7 O3 C6 C5 -174.95(19) . . . . ?
C4 O2 C5 C6 -170.3(2) . . . . ?
C6 O3 C7 C8 -171.60(19) . . . . ?
C5 O2 C4 C3 173.4(2) . . . . ?
Br1 C2A C1A N1 -74(3) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.568
_oxdiff_exptl_absorpt_empirical_full_min 0.571
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_173k
_database_code_depnum_ccdc_archive 'CCDC 2053302'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-18 downloaded from the CCDC.
;
_audit_creation_date             2020-11-10
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C2 H7 Br1 N, C12 H24 O6'
_chemical_formula_sum            'C20 H31 Br N Ni O6 S10'
_chemical_formula_weight         840.68
_chemical_melting_point          ?
_chemical_oxdiff_formula         BrCHNONiS
_chemical_oxdiff_usercomment     223K
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.0374(3)
_cell_length_b                   12.0627(3)
_cell_length_c                   13.7656(4)
_cell_angle_alpha                64.349(3)
_cell_angle_beta                 79.574(2)
_cell_angle_gamma                78.920(2)
_cell_volume                     1611.42(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    18473
_cell_measurement_temperature    173
_cell_measurement_theta_max      31.2720
_cell_measurement_theta_min      1.9230
_shelx_estimated_absorpt_T_max   0.786
_shelx_estimated_absorpt_T_min   0.632
_exptl_absorpt_coefficient_mu    2.526
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             858
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.832
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            40700
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.832
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.031
_diffrn_reflns_theta_min         1.888
_diffrn_ambient_temperature      173
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.832
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -59.00  19.00   0.50    1.13    --    5.34 -33.00  42.65  156
  2  ω    -52.00  19.00   0.50    1.13    --    5.34 -25.00 151.04  142
  3  ω    -59.00  19.00   0.50    1.13    --    5.34 -25.00  85.83  156
  4  ω    -67.00  18.00   0.50    1.13    --    5.34 -19.00 -30.00  170
  5  ω    -67.00  19.00   0.50    1.13    --    5.34 -28.00 -79.37  172
  6  ω    -69.00  19.00   0.50    1.13    --    5.34 -24.00-160.80  176
  7  ω    -16.00  29.00   0.50    1.13    --   -4.79 -99.00  90.00   90
  8  ω    -16.00  28.00   0.50    1.13    --   -4.79 -99.00 150.00   88
  9  ω    -18.00  29.00   0.50    1.13    --   -4.79 -99.00  30.00   94
 10  ω    -15.00  26.00   0.50    1.13    --   -4.79 -99.00 -90.00   82
 11  ω    -13.00  28.00   0.50    1.13    --   -4.79 -99.00-150.00   82
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0300819000
_diffrn_orient_matrix_UB_12      0.0042747000
_diffrn_orient_matrix_UB_13      0.0394045000
_diffrn_orient_matrix_UB_21      -0.0299884000
_diffrn_orient_matrix_UB_22      -0.0495162000
_diffrn_orient_matrix_UB_23      0.0412541000
_diffrn_orient_matrix_UB_31      0.0503681000
_diffrn_orient_matrix_UB_32      -0.0430826000
_diffrn_orient_matrix_UB_33      -0.0072863000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6361
_reflns_number_total             8560
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT n/a (Sheldrick, 2015)'
_refine_diff_density_max         0.551
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         8560
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0333
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0249P)²+0.2350P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0746
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C9 \\sim C16 \\sim N1: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C2 \\sim C1 \\sim N1: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
C1A \\sim N1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
3. Others
 1*[Sof(Br1)]+1*[Sof(Br1B)]+1*[Sof(Br1A)]=1 with esd of 0.0001
 Sof(H1BD)=Sof(H1BE)=Sof(H1BF)=Sof(C1A)=Sof(H1AD)=Sof(H1AE)=Sof(C2A)=Sof(H2AA)=
 Sof(H2AB)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=
 Sof(H2B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C8(H8A,H8B), C11(H11A,H11B), C12(H12A,H12B), C9(H9A,H9B),
 C14(H14A,H14B), C3(H3A,H3B), C13(H13A,H13B), C7(H7A,H7B), C4(H4A,H4B), C6(H6A,
 H6B), C5(H5A,H5B), C1A(H1AD,H1AE), C1(H1A,H1B), C2(H2A,H2B), C2A(H2AA,H2AB)
4.b Idealised Me refined as rotating group:
 N1(H1BD,H1BE,H1BF), N1(H1AA,H1AB,H1AC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.13727(2) 0.46473(2) 0.88533(2) 0.02272(7) Uani 1 1 d . . . . .
S1 S 0.10389(4) 0.33991(4) 0.82043(4) 0.02474(11) Uani 1 1 d . . . . .
S3 S 0.20986(4) 0.07174(4) 0.87046(4) 0.02561(11) Uani 1 1 d . . . . .
S9 S 0.05775(5) 0.84554(4) 0.92143(4) 0.02665(11) Uani 1 1 d . . . . .
S4 S 0.35755(5) 0.06028(4) 1.02827(4) 0.02676(11) Uani 1 1 d . . . . .
S2 S 0.26712(5) 0.32768(4) 0.99115(4) 0.02860(12) Uani 1 1 d . . . . .
S7 S 0.16453(5) 0.58235(4) 0.95851(4) 0.02840(12) Uani 1 1 d . . . . .
S6 S 0.01331(5) 0.60776(4) 0.77621(4) 0.03002(12) Uani 1 1 d . . . . .
S8 S -0.07575(5) 0.87394(5) 0.74817(5) 0.03390(13) Uani 1 1 d . . . . .
S5 S 0.36395(5) -0.16586(4) 0.99120(5) 0.03420(13) Uani 1 1 d . . . . .
S10 S -0.08593(5) 1.08954(5) 0.80363(5) 0.03916(14) Uani 1 1 d . . . . .
Br1A Br 0.07488(14) 0.14617(18) 0.53377(17) 0.0523(7) Uani 0.1755(13) 1 d . . P
A 3
O5 O 0.36402(12) 0.39248(13) 0.62092(12) 0.0316(3) Uani 1 1 d . . . . .
O6 O 0.57583(13) 0.22207(12) 0.62582(11) 0.0315(3) Uani 1 1 d . . . . .
O4 O 0.25685(12) 0.53010(13) 0.42558(12) 0.0347(3) Uani 1 1 d . . . . .
O1 O 0.64664(13) 0.13825(13) 0.46140(12) 0.0337(3) Uani 1 1 d . . . . .
N1 N 0.39747(15) 0.28300(16) 0.47001(15) 0.0327(4) Uani 1 1 d . U . . .
H1BD H 0.352131 0.323121 0.412602 0.039 Uiso 0.739(5) 1 calc R U P B 2
H1BE H 0.477820 0.264389 0.445943 0.039 Uiso 0.739(5) 1 calc R U P B 2
H1BF H 0.394174 0.332685 0.505016 0.039 Uiso 0.739(5) 1 calc R U P B 2
H1AA H 0.393335 0.349592 0.404897 0.039 Uiso 0.261(5) 1 calc R U P B 1
H1AB H 0.478451 0.254132 0.481315 0.039 Uiso 0.261(5) 1 calc R U P B 1
H1AC H 0.358368 0.306054 0.523784 0.039 Uiso 0.261(5) 1 calc R U P B 1
O3 O 0.31628(13) 0.45256(14) 0.26140(13) 0.0396(4) Uani 1 1 d . . . . .
O2 O 0.54479(15) 0.29845(15) 0.26819(13) 0.0443(4) Uani 1 1 d . . . . .
C19 C 0.07251(16) 0.71678(16) 0.89177(16) 0.0229(4) Uani 1 1 d . . . . .
C15 C 0.19992(16) 0.20764(16) 0.88831(15) 0.0213(4) Uani 1 1 d . . . . .
C16 C 0.26936(17) 0.20205(16) 0.96234(16) 0.0230(4) Uani 1 1 d . . . . .
C18 C 0.00794(17) 0.72817(17) 0.81184(17) 0.0261(4) Uani 1 1 d . . . . .
C20 C -0.03705(18) 0.94377(17) 0.82339(17) 0.0284(4) Uani 1 1 d . . . . .
C17 C 0.31257(17) -0.01908(17) 0.96493(16) 0.0249(4) Uani 1 1 d . . . . .
C10 C 0.3064(2) 0.51783(19) 0.58963(19) 0.0362(5) Uani 1 1 d . . . . .
H10A H 0.368363 0.575333 0.546680 0.043 Uiso 1 1 calc R U . . .
H10B H 0.272742 0.533356 0.654972 0.043 Uiso 1 1 calc R U . . .
C8 C 0.17012(19) 0.5602(2) 0.35031(19) 0.0373(5) Uani 1 1 d . . . . .
H8A H 0.118907 0.640387 0.340883 0.045 Uiso 1 1 calc R U . . .
H8B H 0.114245 0.495391 0.377270 0.045 Uiso 1 1 calc R U . . .
C11 C 0.4542(2) 0.3627(2) 0.69375(18) 0.0347(5) Uani 1 1 d . . . . .
H11A H 0.413862 0.372900 0.760229 0.042 Uiso 1 1 calc R U . . .
H11B H 0.518479 0.419401 0.659198 0.042 Uiso 1 1 calc R U . . .
C12 C 0.5131(2) 0.2313(2) 0.72245(18) 0.0357(5) Uani 1 1 d . . . . .
H12A H 0.572832 0.208072 0.775919 0.043 Uiso 1 1 calc R U . . .
H12B H 0.448822 0.174540 0.754840 0.043 Uiso 1 1 calc R U . . .
C9 C 0.2037(2) 0.5398(2) 0.52349(19) 0.0380(5) Uani 1 1 d . . . . .
H9A H 0.145434 0.477583 0.563719 0.046 Uiso 1 1 calc R U . . .
H9B H 0.156993 0.623346 0.507918 0.046 Uiso 1 1 calc R U . . .
C14 C 0.7254(2) 0.1150(2) 0.5410(2) 0.0411(6) Uani 1 1 d . . . . .
H14A H 0.776517 0.183437 0.515741 0.049 Uiso 1 1 calc R U . . .
H14B H 0.781913 0.036994 0.552822 0.049 Uiso 1 1 calc R U . . .
C3 C 0.7144(2) 0.1676(2) 0.35677(19) 0.0374(5) Uani 1 1 d . . . . .
H3A H 0.779777 0.098124 0.358633 0.045 Uiso 1 1 calc R U . . .
H3B H 0.755046 0.242433 0.335296 0.045 Uiso 1 1 calc R U . . .
C13 C 0.6478(2) 0.1050(2) 0.64434(19) 0.0415(6) Uani 1 1 d . . . . .
H13A H 0.592699 0.040154 0.667522 0.050 Uiso 1 1 calc R U . . .
H13B H 0.701589 0.082206 0.702166 0.050 Uiso 1 1 calc R U . . .
C7 C 0.2410(2) 0.5684(2) 0.24504(19) 0.0389(5) Uani 1 1 d . . . . .
H7A H 0.182723 0.587513 0.191337 0.047 Uiso 1 1 calc R U . . .
H7B H 0.294084 0.635626 0.216761 0.047 Uiso 1 1 calc R U . . .
C4 C 0.6288(2) 0.1903(2) 0.2768(2) 0.0432(6) Uani 1 1 d . . . . .
H4A H 0.676355 0.202352 0.205507 0.052 Uiso 1 1 calc R U . . .
H4B H 0.582694 0.118467 0.301046 0.052 Uiso 1 1 calc R U . . .
C6 C 0.3993(3) 0.4618(3) 0.1664(2) 0.0572(8) Uani 1 1 d . . . . .
H6A H 0.458640 0.520565 0.151877 0.069 Uiso 1 1 calc R U . . .
H6B H 0.351912 0.493195 0.103101 0.069 Uiso 1 1 calc R U . . .
C5 C 0.4683(3) 0.3367(3) 0.1835(2) 0.0641(9) Uani 1 1 d . . . . .
H5A H 0.408839 0.276446 0.203176 0.077 Uiso 1 1 calc R U . . .
H5B H 0.520195 0.340170 0.115785 0.077 Uiso 1 1 calc R U . . .
C1A C 0.3438(3) 0.1624(3) 0.5487(3) 0.0382(8) Uani 0.739(5) 1 d . U P B 2
H1AD H 0.355785 0.105461 0.512267 0.046 Uiso 0.739(5) 1 calc R U P B 2
H1AE H 0.391031 0.121695 0.612599 0.046 Uiso 0.739(5) 1 calc R U P B 2
C1 C 0.3415(16) 0.1929(14) 0.4701(19) 0.121(7) Uani 0.261(5) 1 d . U P B 1
H1A H 0.394943 0.161998 0.418632 0.146 Uiso 0.261(5) 1 calc R U P B 1
H1B H 0.346162 0.124105 0.543001 0.146 Uiso 0.261(5) 1 calc R U P B 1
Br1B Br 0.10584(3) 0.22415(4) 0.47343(4) 0.04084(16) Uani 0.6853(12) 1 d . . P
B 2
Br1 Br 0.1168(2) 0.2037(2) 0.5704(2) 0.0603(10) Uani 0.1392(12) 1 d . . P B 1
C2 C 0.2250(9) 0.2084(10) 0.4474(9) 0.056(3) Uani 0.261(5) 1 d . U P B 1
H2A H 0.213107 0.141711 0.427745 0.067 Uiso 0.261(5) 1 calc R U P B 1
H2B H 0.207815 0.289071 0.385435 0.067 Uiso 0.261(5) 1 calc R U P B 1
C2A C 0.2098(3) 0.1816(3) 0.5865(3) 0.0383(9) Uani 0.739(5) 1 d . . P B 2
H2AA H 0.194907 0.248864 0.611861 0.046 Uiso 0.739(5) 1 calc R U P B 2
H2AB H 0.186709 0.104891 0.648716 0.046 Uiso 0.739(5) 1 calc R U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S1 2.1674(5) . ?
Ni1 S2 2.1608(5) . ?
Ni1 S7 2.1518(5) . ?
Ni1 S6 2.1675(5) . ?
S1 C15 1.7204(18) . ?
S3 C15 1.7406(18) . ?
S3 C17 1.732(2) . ?
S9 C19 1.7416(18) . ?
S9 C20 1.723(2) . ?
S4 C16 1.7412(18) . ?
S4 C17 1.728(2) . ?
S2 C16 1.7197(18) . ?
S7 C19 1.7088(18) . ?
S6 C18 1.711(2) . ?
S8 C18 1.7458(18) . ?
S8 C20 1.737(2) . ?
S5 C17 1.6496(18) . ?
S10 C20 1.6526(19) . ?
O5 C10 1.429(2) . ?
O5 C11 1.427(3) . ?
O6 C12 1.424(3) . ?
O6 C13 1.422(2) . ?
O4 C8 1.422(3) . ?
O4 C9 1.414(3) . ?
O1 C14 1.421(3) . ?
O1 C3 1.424(3) . ?
N1 H1BD 0.9100 . ?
N1 H1BE 0.9100 . ?
N1 H1BF 0.9100 . ?
N1 H1AA 0.9100 . ?
N1 H1AB 0.9100 . ?
N1 H1AC 0.9100 . ?
N1 C1A 1.542(4) . ?
N1 C1 1.349(15) . ?
O3 C7 1.429(2) . ?
O3 C6 1.429(3) . ?
O2 C4 1.420(3) . ?
O2 C5 1.424(3) . ?
C19 C18 1.361(3) . ?
C15 C16 1.354(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C9 1.494(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C7 1.489(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.498(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C13 1.491(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.481(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C5 1.492(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C1A H1AD 0.9900 . ?
C1A H1AE 0.9900 . ?
C1A C2A 1.485(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.337(18) . ?
Br1B C2A 1.932(3) . ?
Br1 C2 1.872(11) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2A H2AA 0.9900 . ?
C2A H2AB 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S2 Ni1 S1 93.390(19) . . ?
S2 Ni1 S6 177.44(2) . . ?
S7 Ni1 S1 176.67(2) . . ?
S7 Ni1 S2 85.53(2) . . ?
S7 Ni1 S6 93.092(19) . . ?
S6 Ni1 S1 88.11(2) . . ?
C15 S1 Ni1 101.72(7) . . ?
C17 S3 C15 97.43(9) . . ?
C20 S9 C19 97.18(9) . . ?
C17 S4 C16 97.27(9) . . ?
C16 S2 Ni1 101.95(7) . . ?
C19 S7 Ni1 102.47(7) . . ?
C18 S6 Ni1 101.91(7) . . ?
C20 S8 C18 97.62(9) . . ?
C11 O5 C10 111.44(16) . . ?
C13 O6 C12 113.44(16) . . ?
C9 O4 C8 114.04(16) . . ?
C14 O1 C3 111.56(16) . . ?
H1BD N1 H1BE 109.5 . . ?
H1BD N1 H1BF 109.5 . . ?
H1BE N1 H1BF 109.5 . . ?
H1AA N1 H1AB 109.5 . . ?
H1AA N1 H1AC 109.5 . . ?
H1AB N1 H1AC 109.5 . . ?
C1A N1 H1BD 109.5 . . ?
C1A N1 H1BE 109.5 . . ?
C1A N1 H1BF 109.5 . . ?
C1 N1 H1AA 109.5 . . ?
C1 N1 H1AB 109.5 . . ?
C1 N1 H1AC 109.5 . . ?
C6 O3 C7 110.84(18) . . ?
C4 O2 C5 112.13(18) . . ?
S7 C19 S9 121.97(12) . . ?
C18 C19 S9 116.90(13) . . ?
C18 C19 S7 121.12(14) . . ?
S1 C15 S3 122.58(11) . . ?
C16 C15 S1 121.51(14) . . ?
C16 C15 S3 115.87(13) . . ?
S2 C16 S4 122.22(12) . . ?
C15 C16 S4 116.35(14) . . ?
C15 C16 S2 121.42(13) . . ?
S6 C18 S8 123.55(12) . . ?
C19 C18 S6 121.38(14) . . ?
C19 C18 S8 115.05(14) . . ?
S9 C20 S8 113.21(10) . . ?
S10 C20 S9 123.09(13) . . ?
S10 C20 S8 123.70(13) . . ?
S4 C17 S3 113.08(10) . . ?
S5 C17 S3 123.75(12) . . ?
S5 C17 S4 123.17(12) . . ?
O5 C10 H10A 109.8 . . ?
O5 C10 H10B 109.8 . . ?
O5 C10 C9 109.15(18) . . ?
H10A C10 H10B 108.3 . . ?
C9 C10 H10A 109.8 . . ?
C9 C10 H10B 109.8 . . ?
O4 C8 H8A 110.1 . . ?
O4 C8 H8B 110.1 . . ?
O4 C8 C7 108.10(17) . . ?
H8A C8 H8B 108.4 . . ?
C7 C8 H8A 110.1 . . ?
C7 C8 H8B 110.1 . . ?
O5 C11 H11A 109.8 . . ?
O5 C11 H11B 109.8 . . ?
O5 C11 C12 109.26(17) . . ?
H11A C11 H11B 108.3 . . ?
C12 C11 H11A 109.8 . . ?
C12 C11 H11B 109.8 . . ?
O6 C12 C11 108.11(17) . . ?
O6 C12 H12A 110.1 . . ?
O6 C12 H12B 110.1 . . ?
C11 C12 H12A 110.1 . . ?
C11 C12 H12B 110.1 . . ?
H12A C12 H12B 108.4 . . ?
O4 C9 C10 108.13(16) . . ?
O4 C9 H9A 110.1 . . ?
O4 C9 H9B 110.1 . . ?
C10 C9 H9A 110.1 . . ?
C10 C9 H9B 110.1 . . ?
H9A C9 H9B 108.4 . . ?
O1 C14 H14A 109.8 . . ?
O1 C14 H14B 109.8 . . ?
O1 C14 C13 109.26(18) . . ?
H14A C14 H14B 108.3 . . ?
C13 C14 H14A 109.8 . . ?
C13 C14 H14B 109.8 . . ?
O1 C3 H3A 109.7 . . ?
O1 C3 H3B 109.7 . . ?
O1 C3 C4 109.63(18) . . ?
H3A C3 H3B 108.2 . . ?
C4 C3 H3A 109.7 . . ?
C4 C3 H3B 109.7 . . ?
O6 C13 C14 107.88(18) . . ?
O6 C13 H13A 110.1 . . ?
O6 C13 H13B 110.1 . . ?
C14 C13 H13A 110.1 . . ?
C14 C13 H13B 110.1 . . ?
H13A C13 H13B 108.4 . . ?
O3 C7 C8 108.96(18) . . ?
O3 C7 H7A 109.9 . . ?
O3 C7 H7B 109.9 . . ?
C8 C7 H7A 109.9 . . ?
C8 C7 H7B 109.9 . . ?
H7A C7 H7B 108.3 . . ?
O2 C4 C3 107.97(19) . . ?
O2 C4 H4A 110.1 . . ?
O2 C4 H4B 110.1 . . ?
C3 C4 H4A 110.1 . . ?
C3 C4 H4B 110.1 . . ?
H4A C4 H4B 108.4 . . ?
O3 C6 H6A 109.9 . . ?
O3 C6 H6B 109.9 . . ?
O3 C6 C5 109.1(2) . . ?
H6A C6 H6B 108.3 . . ?
C5 C6 H6A 109.9 . . ?
C5 C6 H6B 109.9 . . ?
O2 C5 C6 108.9(2) . . ?
O2 C5 H5A 109.9 . . ?
O2 C5 H5B 109.9 . . ?
C6 C5 H5A 109.9 . . ?
C6 C5 H5B 109.9 . . ?
H5A C5 H5B 108.3 . . ?
N1 C1A H1AD 108.8 . . ?
N1 C1A H1AE 108.8 . . ?
H1AD C1A H1AE 107.7 . . ?
C2A C1A N1 113.8(2) . . ?
C2A C1A H1AD 108.8 . . ?
C2A C1A H1AE 108.8 . . ?
N1 C1 H1A 106.2 . . ?
N1 C1 H1B 106.2 . . ?
H1A C1 H1B 106.4 . . ?
C2 C1 N1 124.3(15) . . ?
C2 C1 H1A 106.2 . . ?
C2 C1 H1B 106.2 . . ?
C1 C2 Br1 108.3(13) . . ?
C1 C2 H2A 110.0 . . ?
C1 C2 H2B 110.0 . . ?
Br1 C2 H2A 110.0 . . ?
Br1 C2 H2B 110.0 . . ?
H2A C2 H2B 108.4 . . ?
C1A C2A Br1B 112.0(2) . . ?
C1A C2A H2AA 109.2 . . ?
C1A C2A H2AB 109.2 . . ?
Br1B C2A H2AA 109.2 . . ?
Br1B C2A H2AB 109.2 . . ?
H2AA C2A H2AB 107.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S1 C15 S3 178.68(10) . . . . ?
Ni1 S1 C15 C16 1.14(17) . . . . ?
Ni1 S2 C16 S4 -178.30(10) . . . . ?
Ni1 S2 C16 C15 0.21(18) . . . . ?
Ni1 S7 C19 S9 178.99(10) . . . . ?
Ni1 S7 C19 C18 -1.59(18) . . . . ?
Ni1 S6 C18 S8 178.18(11) . . . . ?
Ni1 S6 C18 C19 -0.25(18) . . . . ?
S1 C15 C16 S4 177.63(10) . . . . ?
S1 C15 C16 S2 -1.0(2) . . . . ?
S3 C15 C16 S4 -0.1(2) . . . . ?
S3 C15 C16 S2 -178.67(10) . . . . ?
S9 C19 C18 S6 -179.24(11) . . . . ?
S9 C19 C18 S8 2.2(2) . . . . ?
S7 C19 C18 S6 1.3(3) . . . . ?
S7 C19 C18 S8 -177.23(11) . . . . ?
O5 C10 C9 O4 -65.8(2) . . . . ?
O5 C11 C12 O6 62.6(2) . . . . ?
O4 C8 C7 O3 58.3(2) . . . . ?
O1 C14 C13 O6 -64.3(2) . . . . ?
O1 C3 C4 O2 65.5(2) . . . . ?
N1 C1A C2A Br1B 72.0(3) . . . . ?
N1 C1 C2 Br1 -79(2) . . . . ?
O3 C6 C5 O2 -65.0(3) . . . . ?
C19 S9 C20 S8 1.74(13) . . . . ?
C19 S9 C20 S10 -178.35(13) . . . . ?
C15 S3 C17 S4 -0.84(12) . . . . ?
C15 S3 C17 S5 179.84(13) . . . . ?
C16 S4 C17 S3 0.81(12) . . . . ?
C16 S4 C17 S5 -179.87(13) . . . . ?
C18 S8 C20 S9 -0.81(13) . . . . ?
C18 S8 C20 S10 179.28(14) . . . . ?
C20 S9 C19 S7 177.02(13) . . . . ?
C20 S9 C19 C18 -2.42(18) . . . . ?
C20 S8 C18 S6 -179.34(13) . . . . ?
C20 S8 C18 C19 -0.83(17) . . . . ?
C17 S3 C15 S1 -177.11(12) . . . . ?
C17 S3 C15 C16 0.56(17) . . . . ?
C17 S4 C16 S2 178.13(12) . . . . ?
C17 S4 C16 C15 -0.46(17) . . . . ?
C10 O5 C11 C12 -179.08(16) . . . . ?
C8 O4 C9 C10 -174.58(17) . . . . ?
C11 O5 C10 C9 -173.88(17) . . . . ?
C12 O6 C13 C14 -170.04(18) . . . . ?
C9 O4 C8 C7 169.88(17) . . . . ?
C14 O1 C3 C4 179.69(18) . . . . ?
C3 O1 C14 C13 170.98(18) . . . . ?
C13 O6 C12 C11 173.07(18) . . . . ?
C7 O3 C6 C5 -175.2(2) . . . . ?
C4 O2 C5 C6 -170.0(2) . . . . ?
C6 O3 C7 C8 -171.5(2) . . . . ?
C5 O2 C4 C3 172.8(2) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.435
_oxdiff_exptl_absorpt_empirical_full_min 0.526
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_233k
_database_code_depnum_ccdc_archive 'CCDC 2053305'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-18 downloaded from the CCDC.
;
_audit_creation_date             2020-11-10
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C2 H7 Br1 N, C12 H24 O6'
_chemical_formula_sum            'C20 H31 Br N Ni O6 S10'
_chemical_formula_weight         840.68
_chemical_melting_point          ?
_chemical_oxdiff_formula         BrCHNONiS
_chemical_oxdiff_usercomment     223K
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.0760(3)
_cell_length_b                   12.0662(3)
_cell_length_c                   13.7164(5)
_cell_angle_alpha                65.106(3)
_cell_angle_beta                 80.573(3)
_cell_angle_gamma                78.719(2)
_cell_volume                     1623.84(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    15238
_cell_measurement_temperature    233
_cell_measurement_theta_max      30.7350
_cell_measurement_theta_min      2.3550
_shelx_estimated_absorpt_T_max   0.788
_shelx_estimated_absorpt_T_min   0.634
_exptl_absorpt_coefficient_mu    2.507
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34127
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             858
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0755
_diffrn_reflns_av_unetI/netI     0.0651
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.828
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            40270
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.828
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.058
_diffrn_reflns_theta_min         1.880
_diffrn_ambient_temperature      233
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.828
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -50.00  18.00   0.50    1.12    --    5.18 -29.00 128.67  136
  2  ω    -68.00  19.00   0.50    1.12    --    5.18 -33.00  -0.06  174
  3  ω    -69.00  19.00   0.50    1.12    --    5.18 -28.00  79.65  176
  4  ω    -70.00  18.00   0.50    1.12    --    5.18 -19.00 -60.00  176
  5  ω    -33.00  19.00   0.50    1.12    --    5.18 -33.00-124.12  104
  6  ω    -68.00 -38.00   0.50    1.12    --    5.18 -33.00-124.12   60
  7  ω    -45.00  19.00   0.50    1.12    --    5.18 -28.00-179.69  128
  8  ω    -18.00  27.00   0.50    1.12    --   -4.95 -99.00  90.00   90
  9  ω    -73.00  14.00   0.50    1.12    --   -4.95 -77.00  30.00  174
 10  ω     -7.00  29.00   0.50    1.12    --   -4.95 -99.00-120.00   72
 11  ω    -18.00  28.00   0.50    1.12    --   -4.95 -99.00-180.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0298907000
_diffrn_orient_matrix_UB_12      0.0037518000
_diffrn_orient_matrix_UB_13      0.0402425000
_diffrn_orient_matrix_UB_21      -0.0295532000
_diffrn_orient_matrix_UB_22      -0.0491029000
_diffrn_orient_matrix_UB_23      0.0400775000
_diffrn_orient_matrix_UB_31      0.0503329000
_diffrn_orient_matrix_UB_32      -0.0431323000
_diffrn_orient_matrix_UB_33      -0.0071958000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5728
_reflns_number_total             8614
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT n/a (Sheldrick, 2015)'
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         8614
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0405
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0416P)²+0.0911P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0923
_refine_ls_wR_factor_ref         0.1033
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C9 \\sim C16 \\sim N1: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C2 \\sim C1 \\sim N1: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
C1A \\sim N1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
3. Others
 1*[Sof(Br1)]+1*[Sof(Br1B)]+1*[Sof(Br1A)]=1 with esd of 0.0001
 Sof(H1BD)=Sof(H1BE)=Sof(H1BF)=Sof(C1A)=Sof(H1AD)=Sof(H1AE)=Sof(C2A)=Sof(H2AA)=
 Sof(H2AB)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=
 Sof(H2B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C8(H8A,H8B), C11(H11A,H11B), C12(H12A,H12B), C9(H9A,H9B),
 C14(H14A,H14B), C3(H3A,H3B), C13(H13A,H13B), C7(H7A,H7B), C4(H4A,H4B), C6(H6A,
 H6B), C5(H5A,H5B), C1A(H1AD,H1AE), C1(H1A,H1B), C2(H2A,H2B), C2A(H2AA,H2AB)
4.b Idealised Me refined as rotating group:
 N1(H1BD,H1BE,H1BF), N1(H1AA,H1AB,H1AC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.13485(3) 0.46462(2) 0.88379(2) 0.03078(9) Uani 1 1 d . . . . .
S1 S 0.10176(5) 0.33976(5) 0.81785(5) 0.03384(14) Uani 1 1 d . . . . .
S3 S 0.20872(6) 0.07211(5) 0.86760(5) 0.03568(15) Uani 1 1 d . . . . .
S9 S 0.05493(6) 0.84442(5) 0.92222(5) 0.03659(15) Uani 1 1 d . . . . .
S4 S 0.35724(6) 0.06189(5) 1.02590(5) 0.03676(15) Uani 1 1 d . . . . .
S2 S 0.26562(6) 0.32824(5) 0.98965(5) 0.03839(16) Uani 1 1 d . . . . .
S7 S 0.16170(6) 0.58161(5) 0.95876(5) 0.03856(16) Uani 1 1 d . . . . .
S6 S 0.01184(6) 0.60795(6) 0.77344(6) 0.04032(16) Uani 1 1 d . . . . .
S8 S -0.07877(6) 0.87273(6) 0.74794(6) 0.04578(18) Uani 1 1 d . . . . .
S5 S 0.36371(7) -0.16423(6) 0.98932(6) 0.04741(18) Uani 1 1 d . . . . .
S10 S -0.09185(7) 1.08614(6) 0.80742(7) 0.0547(2) Uani 1 1 d . . . . .
Br1A Br 0.07661(7) 0.14544(9) 0.53778(9) 0.0650(4) Uani 0.4244(16) 1 d . . P A
3
O5 O 0.36104(16) 0.39251(16) 0.62002(15) 0.0430(4) Uani 1 1 d . . . . .
O6 O 0.57144(16) 0.22169(16) 0.62553(14) 0.0458(4) Uani 1 1 d . . . . .
O4 O 0.25732(15) 0.53250(17) 0.42244(15) 0.0467(5) Uani 1 1 d . . . . .
O1 O 0.64564(16) 0.14035(18) 0.45892(15) 0.0486(5) Uani 1 1 d . . . . .
N1 N 0.40015(19) 0.2889(2) 0.46283(18) 0.0450(5) Uani 1 1 d . U . . .
H1BD H 0.342346 0.344745 0.421895 0.054 Uiso 0.477(8) 1 calc R U P B 2
H1BE H 0.463681 0.269646 0.419967 0.054 Uiso 0.477(8) 1 calc R U P B 2
H1BF H 0.427604 0.320716 0.502397 0.054 Uiso 0.477(8) 1 calc R U P B 2
H1AA H 0.401235 0.345312 0.394196 0.054 Uiso 0.523(8) 1 calc R U P B 1
H1AB H 0.477561 0.251018 0.477481 0.054 Uiso 0.523(8) 1 calc R U P B 1
H1AC H 0.369794 0.326516 0.507893 0.054 Uiso 0.523(8) 1 calc R U P B 1
O3 O 0.31964(17) 0.46015(19) 0.25525(16) 0.0558(5) Uani 1 1 d . . . . .
O2 O 0.54586(19) 0.3042(2) 0.26469(17) 0.0644(6) Uani 1 1 d . . . . .
C19 C 0.0706(2) 0.7161(2) 0.8913(2) 0.0314(5) Uani 1 1 d . . . . .
C15 C 0.1985(2) 0.20809(19) 0.88568(19) 0.0305(5) Uani 1 1 d . . . . .
C16 C 0.2681(2) 0.2026(2) 0.96001(19) 0.0311(5) Uani 1 1 d . . . . .
C18 C 0.0059(2) 0.7280(2) 0.8107(2) 0.0348(5) Uani 1 1 d . . . . .
C20 C -0.0416(2) 0.9419(2) 0.8248(2) 0.0399(6) Uani 1 1 d . . . . .
C17 C 0.3123(2) -0.0174(2) 0.9623(2) 0.0347(5) Uani 1 1 d . . . . .
C10 C 0.3040(3) 0.5182(3) 0.5893(2) 0.0491(7) Uani 1 1 d . . . . .
H10A H 0.365518 0.573705 0.549401 0.059 Uiso 1 1 calc R U . . .
H10B H 0.270127 0.533490 0.653856 0.059 Uiso 1 1 calc R U . . .
C8 C 0.1725(2) 0.5651(3) 0.3448(2) 0.0519(7) Uani 1 1 d . . . . .
H8A H 0.122023 0.644455 0.336140 0.062 Uiso 1 1 calc R U . . .
H8B H 0.117472 0.502373 0.368073 0.062 Uiso 1 1 calc R U . . .
C11 C 0.4509(3) 0.3612(3) 0.6939(2) 0.0475(7) Uani 1 1 d . . . . .
H11A H 0.411633 0.371406 0.759663 0.057 Uiso 1 1 calc R U . . .
H11B H 0.514463 0.415900 0.661584 0.057 Uiso 1 1 calc R U . . .
C12 C 0.5083(3) 0.2305(3) 0.7210(2) 0.0510(7) Uani 1 1 d . . . . .
H12A H 0.566397 0.205413 0.775815 0.061 Uiso 1 1 calc R U . . .
H12B H 0.444414 0.176135 0.749843 0.061 Uiso 1 1 calc R U . . .
C9 C 0.2029(2) 0.5421(3) 0.5201(2) 0.0514(7) Uani 1 1 d . . . . .
H9A H 0.145342 0.481637 0.557289 0.062 Uiso 1 1 calc R U . . .
H9B H 0.156816 0.624803 0.505028 0.062 Uiso 1 1 calc R U . . .
C14 C 0.7217(3) 0.1162(3) 0.5414(3) 0.0590(8) Uani 1 1 d . . . . .
H14A H 0.770823 0.183446 0.519725 0.071 Uiso 1 1 calc R U . . .
H14B H 0.778546 0.039437 0.553047 0.071 Uiso 1 1 calc R U . . .
C3 C 0.7129(3) 0.1710(3) 0.3555(3) 0.0559(8) Uani 1 1 d . . . . .
H3A H 0.777812 0.102390 0.356835 0.067 Uiso 1 1 calc R U . . .
H3B H 0.752622 0.243870 0.337476 0.067 Uiso 1 1 calc R U . . .
C13 C 0.6432(3) 0.1050(3) 0.6426(3) 0.0600(8) Uani 1 1 d . . . . .
H13A H 0.589088 0.042333 0.661632 0.072 Uiso 1 1 calc R U . . .
H13B H 0.695068 0.080383 0.701818 0.072 Uiso 1 1 calc R U . . .
C7 C 0.2442(3) 0.5740(3) 0.2412(2) 0.0521(7) Uani 1 1 d . . . . .
H7A H 0.187477 0.594541 0.186245 0.063 Uiso 1 1 calc R U . . .
H7B H 0.295913 0.639776 0.216410 0.063 Uiso 1 1 calc R U . . .
C4 C 0.6299(3) 0.1962(3) 0.2736(3) 0.0629(9) Uani 1 1 d . . . . .
H4A H 0.677705 0.208146 0.204038 0.076 Uiso 1 1 calc R U . . .
H4B H 0.584603 0.126250 0.294460 0.076 Uiso 1 1 calc R U . . .
C6 C 0.4027(3) 0.4691(4) 0.1628(3) 0.0733(11) Uani 1 1 d . . . . .
H6A H 0.460820 0.525960 0.151527 0.088 Uiso 1 1 calc R U . . .
H6B H 0.356606 0.501760 0.098893 0.088 Uiso 1 1 calc R U . . .
C5 C 0.4711(4) 0.3461(4) 0.1776(3) 0.0890(13) Uani 1 1 d . . . . .
H5A H 0.412867 0.288054 0.193010 0.107 Uiso 1 1 calc R U . . .
H5B H 0.523298 0.350769 0.111391 0.107 Uiso 1 1 calc R U . . .
C1A C 0.3407(9) 0.1661(9) 0.5421(8) 0.069(2) Uani 0.477(8) 1 d . U P B 2
H1AD H 0.348605 0.111828 0.503982 0.083 Uiso 0.477(8) 1 calc R U P B 2
H1AE H 0.389064 0.122369 0.604685 0.083 Uiso 0.477(8) 1 calc R U P B 2
C1 C 0.3274(11) 0.2038(10) 0.4763(14) 0.144(6) Uani 0.523(8) 1 d . U P B 1
H1A H 0.376352 0.152650 0.440150 0.173 Uiso 0.523(8) 1 calc R U P B 1
H1B H 0.323933 0.150926 0.553665 0.173 Uiso 0.523(8) 1 calc R U P B 1
Br1B Br 0.10538(8) 0.22724(10) 0.47400(9) 0.0560(4) Uani 0.3632(15) 1 d . . P B
2
Br1 Br 0.1199(2) 0.2049(2) 0.5687(2) 0.0863(11) Uani 0.2124(16) 1 d . . P B 1
C2 C 0.2179(8) 0.2193(9) 0.4514(8) 0.123(5) Uani 0.523(8) 1 d . U P B 1
H2A H 0.208413 0.156779 0.426223 0.147 Uiso 0.523(8) 1 calc R U P B 1
H2B H 0.198537 0.301162 0.393926 0.147 Uiso 0.523(8) 1 calc R U P B 1
C2A C 0.2149(7) 0.1863(7) 0.5798(6) 0.063(2) Uani 0.477(8) 1 d . . P B 2
H2AA H 0.203184 0.253217 0.604602 0.076 Uiso 0.477(8) 1 calc R U P B 2
H2AB H 0.194364 0.111547 0.641887 0.076 Uiso 0.477(8) 1 calc R U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S1 2.1665(7) . ?
Ni1 S2 2.1585(7) . ?
Ni1 S7 2.1505(7) . ?
Ni1 S6 2.1652(7) . ?
S1 C15 1.719(2) . ?
S3 C15 1.740(2) . ?
S3 C17 1.730(2) . ?
S9 C19 1.741(2) . ?
S9 C20 1.723(3) . ?
S4 C16 1.737(2) . ?
S4 C17 1.719(3) . ?
S2 C16 1.721(2) . ?
S7 C19 1.706(2) . ?
S6 C18 1.714(2) . ?
S8 C18 1.741(2) . ?
S8 C20 1.730(3) . ?
S5 C17 1.650(2) . ?
S10 C20 1.646(2) . ?
O5 C10 1.432(3) . ?
O5 C11 1.422(3) . ?
O6 C12 1.416(3) . ?
O6 C13 1.419(3) . ?
O4 C8 1.415(3) . ?
O4 C9 1.418(3) . ?
O1 C14 1.419(3) . ?
O1 C3 1.422(3) . ?
N1 H1BD 0.9000 . ?
N1 H1BE 0.9000 . ?
N1 H1BF 0.9000 . ?
N1 H1AA 0.9000 . ?
N1 H1AB 0.9000 . ?
N1 H1AC 0.9000 . ?
N1 C1A 1.613(10) . ?
N1 C1 1.361(10) . ?
O3 C7 1.416(3) . ?
O3 C6 1.417(4) . ?
O2 C4 1.417(4) . ?
O2 C5 1.421(4) . ?
C19 C18 1.357(4) . ?
C15 C16 1.349(3) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 C9 1.493(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 C7 1.482(4) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 C12 1.491(4) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 C13 1.480(4) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 C4 1.464(4) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 C5 1.475(5) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C1A H1AD 0.9800 . ?
C1A H1AE 0.9800 . ?
C1A C2A 1.416(12) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 C2 1.272(13) . ?
Br1B C2A 1.887(7) . ?
Br1 C2 1.750(11) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2A H2AA 0.9800 . ?
C2A H2AB 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S2 Ni1 S1 93.31(2) . . ?
S2 Ni1 S6 176.76(3) . . ?
S7 Ni1 S1 176.36(3) . . ?
S7 Ni1 S2 85.42(2) . . ?
S7 Ni1 S6 93.08(2) . . ?
S6 Ni1 S1 88.36(2) . . ?
C15 S1 Ni1 101.75(8) . . ?
C17 S3 C15 97.28(11) . . ?
C20 S9 C19 97.26(12) . . ?
C17 S4 C16 97.13(11) . . ?
C16 S2 Ni1 101.99(8) . . ?
C19 S7 Ni1 102.49(9) . . ?
C18 S6 Ni1 101.87(9) . . ?
C20 S8 C18 97.74(12) . . ?
C11 O5 C10 111.5(2) . . ?
C12 O6 C13 113.8(2) . . ?
C8 O4 C9 113.9(2) . . ?
C14 O1 C3 112.6(2) . . ?
H1BD N1 H1BE 109.5 . . ?
H1BD N1 H1BF 109.5 . . ?
H1BE N1 H1BF 109.5 . . ?
H1AA N1 H1AB 109.5 . . ?
H1AA N1 H1AC 109.5 . . ?
H1AB N1 H1AC 109.5 . . ?
C1A N1 H1BD 109.5 . . ?
C1A N1 H1BE 109.5 . . ?
C1A N1 H1BF 109.5 . . ?
C1 N1 H1AA 109.5 . . ?
C1 N1 H1AB 109.5 . . ?
C1 N1 H1AC 109.5 . . ?
C7 O3 C6 111.8(2) . . ?
C4 O2 C5 113.1(2) . . ?
S7 C19 S9 122.10(15) . . ?
C18 C19 S9 116.62(17) . . ?
C18 C19 S7 121.28(18) . . ?
S1 C15 S3 122.71(15) . . ?
C16 C15 S1 121.60(17) . . ?
C16 C15 S3 115.64(17) . . ?
S2 C16 S4 122.00(15) . . ?
C15 C16 S4 116.64(17) . . ?
C15 C16 S2 121.35(17) . . ?
S6 C18 S8 123.45(15) . . ?
C19 C18 S6 121.27(17) . . ?
C19 C18 S8 115.27(18) . . ?
S9 C20 S8 113.08(13) . . ?
S10 C20 S9 122.76(17) . . ?
S10 C20 S8 124.15(16) . . ?
S4 C17 S3 113.30(12) . . ?
S5 C17 S3 123.71(15) . . ?
S5 C17 S4 122.99(15) . . ?
O5 C10 H10A 109.9 . . ?
O5 C10 H10B 109.9 . . ?
O5 C10 C9 109.0(2) . . ?
H10A C10 H10B 108.3 . . ?
C9 C10 H10A 109.9 . . ?
C9 C10 H10B 109.9 . . ?
O4 C8 H8A 110.1 . . ?
O4 C8 H8B 110.1 . . ?
O4 C8 C7 108.0(2) . . ?
H8A C8 H8B 108.4 . . ?
C7 C8 H8A 110.1 . . ?
C7 C8 H8B 110.1 . . ?
O5 C11 H11A 109.9 . . ?
O5 C11 H11B 109.9 . . ?
O5 C11 C12 108.8(2) . . ?
H11A C11 H11B 108.3 . . ?
C12 C11 H11A 109.9 . . ?
C12 C11 H11B 109.9 . . ?
O6 C12 C11 108.1(2) . . ?
O6 C12 H12A 110.1 . . ?
O6 C12 H12B 110.1 . . ?
C11 C12 H12A 110.1 . . ?
C11 C12 H12B 110.1 . . ?
H12A C12 H12B 108.4 . . ?
O4 C9 C10 108.1(2) . . ?
O4 C9 H9A 110.1 . . ?
O4 C9 H9B 110.1 . . ?
C10 C9 H9A 110.1 . . ?
C10 C9 H9B 110.1 . . ?
H9A C9 H9B 108.4 . . ?
O1 C14 H14A 109.8 . . ?
O1 C14 H14B 109.8 . . ?
O1 C14 C13 109.5(2) . . ?
H14A C14 H14B 108.2 . . ?
C13 C14 H14A 109.8 . . ?
C13 C14 H14B 109.8 . . ?
O1 C3 H3A 109.6 . . ?
O1 C3 H3B 109.6 . . ?
O1 C3 C4 110.2(2) . . ?
H3A C3 H3B 108.1 . . ?
C4 C3 H3A 109.6 . . ?
C4 C3 H3B 109.6 . . ?
O6 C13 C14 107.9(2) . . ?
O6 C13 H13A 110.1 . . ?
O6 C13 H13B 110.1 . . ?
C14 C13 H13A 110.1 . . ?
C14 C13 H13B 110.1 . . ?
H13A C13 H13B 108.4 . . ?
O3 C7 C8 109.7(2) . . ?
O3 C7 H7A 109.7 . . ?
O3 C7 H7B 109.7 . . ?
C8 C7 H7A 109.7 . . ?
C8 C7 H7B 109.7 . . ?
H7A C7 H7B 108.2 . . ?
O2 C4 C3 108.5(3) . . ?
O2 C4 H4A 110.0 . . ?
O2 C4 H4B 110.0 . . ?
C3 C4 H4A 110.0 . . ?
C3 C4 H4B 110.0 . . ?
H4A C4 H4B 108.4 . . ?
O3 C6 H6A 109.7 . . ?
O3 C6 H6B 109.7 . . ?
O3 C6 C5 109.6(3) . . ?
H6A C6 H6B 108.2 . . ?
C5 C6 H6A 109.7 . . ?
C5 C6 H6B 109.7 . . ?
O2 C5 C6 109.4(3) . . ?
O2 C5 H5A 109.8 . . ?
O2 C5 H5B 109.8 . . ?
C6 C5 H5A 109.8 . . ?
C6 C5 H5B 109.8 . . ?
H5A C5 H5B 108.3 . . ?
N1 C1A H1AD 108.5 . . ?
N1 C1A H1AE 108.5 . . ?
H1AD C1A H1AE 107.5 . . ?
C2A C1A N1 115.3(7) . . ?
C2A C1A H1AD 108.5 . . ?
C2A C1A H1AE 108.5 . . ?
N1 C1 H1A 104.8 . . ?
N1 C1 H1B 104.8 . . ?
H1A C1 H1B 105.8 . . ?
C2 C1 N1 129.8(10) . . ?
C2 C1 H1A 104.8 . . ?
C2 C1 H1B 104.8 . . ?
C1 C2 Br1 106.4(11) . . ?
C1 C2 H2A 110.5 . . ?
C1 C2 H2B 110.5 . . ?
Br1 C2 H2A 110.5 . . ?
Br1 C2 H2B 110.5 . . ?
H2A C2 H2B 108.6 . . ?
C1A C2A Br1B 113.3(6) . . ?
C1A C2A H2AA 108.9 . . ?
C1A C2A H2AB 108.9 . . ?
Br1B C2A H2AA 108.9 . . ?
Br1B C2A H2AB 108.9 . . ?
H2AA C2A H2AB 107.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S1 C15 S3 178.45(12) . . . . ?
Ni1 S1 C15 C16 1.1(2) . . . . ?
Ni1 S2 C16 S4 -178.30(12) . . . . ?
Ni1 S2 C16 C15 0.2(2) . . . . ?
Ni1 S7 C19 S9 178.62(12) . . . . ?
Ni1 S7 C19 C18 -1.1(2) . . . . ?
Ni1 S6 C18 S8 178.98(13) . . . . ?
Ni1 S6 C18 C19 0.4(2) . . . . ?
S1 C15 C16 S4 177.65(12) . . . . ?
S1 C15 C16 S2 -0.9(3) . . . . ?
S3 C15 C16 S4 0.1(3) . . . . ?
S3 C15 C16 S2 -178.48(13) . . . . ?
S9 C19 C18 S6 -179.24(13) . . . . ?
S9 C19 C18 S8 2.1(3) . . . . ?
S7 C19 C18 S6 0.4(3) . . . . ?
S7 C19 C18 S8 -178.22(13) . . . . ?
O5 C10 C9 O4 -66.0(3) . . . . ?
O5 C11 C12 O6 63.7(3) . . . . ?
O4 C8 C7 O3 58.0(3) . . . . ?
O1 C14 C13 O6 -65.3(3) . . . . ?
O1 C3 C4 O2 65.9(3) . . . . ?
N1 C1A C2A Br1B 74.7(7) . . . . ?
N1 C1 C2 Br1 -96.9(18) . . . . ?
O3 C6 C5 O2 -64.4(4) . . . . ?
C19 S9 C20 S8 1.05(16) . . . . ?
C19 S9 C20 S10 -178.65(17) . . . . ?
C15 S3 C17 S4 -0.77(15) . . . . ?
C15 S3 C17 S5 179.35(16) . . . . ?
C16 S4 C17 S3 0.82(15) . . . . ?
C16 S4 C17 S5 -179.30(16) . . . . ?
C18 S8 C20 S9 -0.16(16) . . . . ?
C18 S8 C20 S10 179.53(18) . . . . ?
C20 S9 C19 S7 178.39(15) . . . . ?
C20 S9 C19 C18 -1.9(2) . . . . ?
C20 S8 C18 S6 -179.79(17) . . . . ?
C20 S8 C18 C19 -1.2(2) . . . . ?
C17 S3 C15 S1 -177.10(15) . . . . ?
C17 S3 C15 C16 0.4(2) . . . . ?
C17 S4 C16 S2 178.01(15) . . . . ?
C17 S4 C16 C15 -0.6(2) . . . . ?
C10 O5 C11 C12 -178.9(2) . . . . ?
C8 O4 C9 C10 -174.1(2) . . . . ?
C11 O5 C10 C9 -174.8(2) . . . . ?
C12 O6 C13 C14 -169.4(2) . . . . ?
C9 O4 C8 C7 169.4(2) . . . . ?
C14 O1 C3 C4 -179.4(3) . . . . ?
C3 O1 C14 C13 170.9(3) . . . . ?
C13 O6 C12 C11 172.6(2) . . . . ?
C7 O3 C6 C5 -175.0(3) . . . . ?
C4 O2 C5 C6 -170.3(3) . . . . ?
C6 O3 C7 C8 -171.7(3) . . . . ?
C5 O2 C4 C3 172.4(3) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.184
_oxdiff_exptl_absorpt_empirical_full_min 0.427
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_373k
_database_code_depnum_ccdc_archive 'CCDC 2053312'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-18 downloaded from the CCDC.
;
_audit_creation_date             2020-11-10
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C2 H7 Br N, C12 H24 O6'
_chemical_formula_sum            'C20 H31 Br N Ni O6 S10'
_chemical_formula_weight         840.68
_chemical_melting_point          ?
_chemical_oxdiff_formula         BrCHNONiS
_chemical_oxdiff_usercomment     223K
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.2167(4)
_cell_length_b                   12.1808(4)
_cell_length_c                   13.7373(5)
_cell_angle_alpha                65.696(3)
_cell_angle_beta                 81.308(3)
_cell_angle_gamma                78.012(3)
_cell_volume                     1668.72(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    12564
_cell_measurement_temperature    373
_cell_measurement_theta_max      28.3220
_cell_measurement_theta_min      1.8560
_shelx_estimated_absorpt_T_max   0.848
_shelx_estimated_absorpt_T_min   0.413
_exptl_absorpt_coefficient_mu    2.439
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             858
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0910
_diffrn_reflns_av_unetI/netI     0.0807
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.889
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            35265
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.889
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.055
_diffrn_reflns_theta_min         1.859
_diffrn_ambient_temperature      373
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.889
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     11.00  87.00   0.50    0.87    --   21.69-116.00   2.00  152
  2  ω     40.00 103.00   0.50    0.87    --   21.69-162.00-146.00  126
  3  ω    -59.00  44.00   0.50    0.87    --   21.69 -37.00-180.00  206
  4  ω    -25.00 101.00   0.50    0.87    --   21.69  19.00-150.00  252
  5  ω     55.00  80.00   0.50    0.87    --   21.69 162.00-119.00   50
  6  ω    -24.00  61.00   0.50    0.87    --  -21.62  19.00-120.00  170
  7  ω    -58.00  -8.00   0.50    0.87    --  -21.62 116.00  90.00  100
  8  ω    -25.00  55.00   0.50    0.87    --  -21.62  19.00  90.00  160
  9  ω   -100.00 -40.00   0.50    0.87    --  -21.62 162.00-119.00  120
 10  ω   -112.00  42.00   0.50    0.87    --  -21.62 -37.00-150.00  308
 11  ω    -16.00  22.00   0.50    0.87    --  -21.62 -99.00 -90.00   76
 12  ω    -13.00  38.00   0.50    0.87    --  -21.62 -99.00 -30.00  102
 13  ω   -102.00  20.00   0.50    0.87    --  -21.62 -57.00  90.00  244
 14  ω   -107.00 -81.00   0.50    0.87    --  -21.62-162.00-146.00   52
 15  ω   -105.00  20.00   0.50    0.87    --  -21.62 -57.00 -60.00  250
 16  ω    -17.00  35.00   0.50    0.87    --  -21.62 -99.00-180.00  104
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0302304000
_diffrn_orient_matrix_UB_12      0.0069553000
_diffrn_orient_matrix_UB_13      0.0383940000
_diffrn_orient_matrix_UB_21      -0.0239978000
_diffrn_orient_matrix_UB_22      -0.0502614000
_diffrn_orient_matrix_UB_23      0.0409747000
_diffrn_orient_matrix_UB_31      0.0520778000
_diffrn_orient_matrix_UB_32      -0.0402137000
_diffrn_orient_matrix_UB_33      -0.0086114000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4430
_reflns_number_total             7932
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         7932
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.1032
_refine_ls_R_factor_gt           0.0470
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0454P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1118
_refine_ls_wR_factor_ref         0.1318
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C15 \\sim C16: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C1A \\sim N1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
C1 \\sim C2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
3. Others
 1*[Sof(Br1)]+1*[Sof(Br1B)]+1*[Sof(Br1A)]=1 with esd of 0.0001
 Sof(H1BD)=Sof(H1BE)=Sof(H1BF)=Sof(C1A)=Sof(H1AD)=Sof(H1AE)=Sof(C2A)=Sof(H2AA)=
 Sof(H2AB)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=
 Sof(H2B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C8(H8A,H8B), C11(H11A,H11B), C12(H12A,H12B), C9(H9A,H9B),
 C14(H14A,H14B), C3(H3A,H3B), C13(H13A,H13B), C7(H7A,H7B), C4(H4A,H4B), C6(H6A,
 H6B), C5(H5A,H5B), C1A(H1AD,H1AE), C1(H1A,H1B), C2(H2A,H2B), C2A(H2AA,H2AB)
4.b Idealised Me refined as rotating group:
 N1(H1BD,H1BE,H1BF), N1(H1AA,H1AB,H1AC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.13298(4) 0.46357(3) 0.88304(3) 0.05131(14) Uani 1 1 d . . . . .
S1 S 0.09935(8) 0.33926(7) 0.81759(7) 0.0574(2) Uani 1 1 d . . . . .
S3 S 0.20688(8) 0.07297(8) 0.86718(7) 0.0602(2) Uani 1 1 d . . . . .
S9 S 0.05427(8) 0.84235(8) 0.92055(8) 0.0614(2) Uani 1 1 d . . . . .
S4 S 0.35611(8) 0.06341(8) 1.02433(7) 0.0595(2) Uani 1 1 d . . . . .
S2 S 0.26415(8) 0.32788(8) 0.98848(7) 0.0624(3) Uani 1 1 d . . . . .
S7 S 0.15942(9) 0.58020(8) 0.95813(7) 0.0645(3) Uani 1 1 d . . . . .
S6 S 0.01169(9) 0.60717(8) 0.77130(8) 0.0674(3) Uani 1 1 d . . . . .
S8 S -0.07948(10) 0.87000(9) 0.74657(8) 0.0756(3) Uani 1 1 d . . . . .
S5 S 0.36381(10) -0.16137(8) 0.98815(9) 0.0795(3) Uani 1 1 d . . . . .
S10 S -0.09641(10) 1.08080(9) 0.80822(10) 0.0860(3) Uani 1 1 d . . . . .
Br1A Br 0.07804(10) 0.14510(12) 0.54060(15) 0.1033(5) Uani 0.580(3) 1 d . . P A
3
O5 O 0.3589(2) 0.3932(3) 0.6182(2) 0.0790(8) Uani 1 1 d . . . . .
O6 O 0.5650(2) 0.2203(3) 0.6240(2) 0.0853(8) Uani 1 1 d . . . . .
O4 O 0.2563(2) 0.5353(3) 0.4211(2) 0.0920(9) Uani 1 1 d . . . . .
O1 O 0.6403(3) 0.1425(3) 0.4563(2) 0.0939(9) Uani 1 1 d . . . . .
N1 N 0.3964(3) 0.2937(3) 0.4586(2) 0.0698(8) Uani 1 1 d . U . . .
H1BD H 0.437376 0.273545 0.405972 0.084 Uiso 0.421(15) 1 calc R U P B 2
H1BE H 0.448945 0.294635 0.500598 0.084 Uiso 0.421(15) 1 calc R U P B 2
H1BF H 0.351545 0.367297 0.430818 0.084 Uiso 0.421(15) 1 calc R U P B 2
H1AA H 0.475139 0.262047 0.465896 0.084 Uiso 0.579(15) 1 calc R U P B 1
H1AB H 0.367398 0.320089 0.510432 0.084 Uiso 0.579(15) 1 calc R U P B 1
H1AC H 0.388003 0.355777 0.395217 0.084 Uiso 0.579(15) 1 calc R U P B 1
O3 O 0.3237(3) 0.4696(3) 0.2525(2) 0.1031(10) Uani 1 1 d . . . . .
O2 O 0.5400(3) 0.3056(4) 0.2632(2) 0.1247(14) Uani 1 1 d . . . . .
C19 C 0.0701(3) 0.7149(3) 0.8894(3) 0.0505(8) Uani 1 1 d . . . . .
C15 C 0.1964(3) 0.2081(3) 0.8852(2) 0.0479(7) Uani 1 1 d . U . . .
C16 C 0.2663(3) 0.2029(3) 0.9596(2) 0.0492(8) Uani 1 1 d . U . . .
C18 C 0.0067(3) 0.7265(3) 0.8088(3) 0.0551(8) Uani 1 1 d . . . . .
C20 C -0.0434(3) 0.9385(3) 0.8245(3) 0.0618(9) Uani 1 1 d . . . . .
C17 C 0.3112(3) -0.0158(3) 0.9615(3) 0.0558(8) Uani 1 1 d . . . . .
C10 C 0.3039(4) 0.5179(4) 0.5878(3) 0.0866(13) Uani 1 1 d . . . . .
H10A H 0.364441 0.570254 0.549278 0.104 Uiso 1 1 calc R U . . .
H10B H 0.272054 0.533994 0.651194 0.104 Uiso 1 1 calc R U . . .
C8 C 0.1784(4) 0.5756(4) 0.3409(4) 0.0998(15) Uani 1 1 d . . . . .
H8A H 0.136028 0.656987 0.331023 0.120 Uiso 1 1 calc R U . . .
H8B H 0.117790 0.522156 0.361227 0.120 Uiso 1 1 calc R U . . .
C11 C 0.4471(4) 0.3585(5) 0.6932(3) 0.0898(13) Uani 1 1 d . . . . .
H11A H 0.408758 0.367714 0.758196 0.108 Uiso 1 1 calc R U . . .
H11B H 0.509589 0.410282 0.663936 0.108 Uiso 1 1 calc R U . . .
C12 C 0.5028(4) 0.2298(5) 0.7177(3) 0.0925(14) Uani 1 1 d . . . . .
H12A H 0.559456 0.202742 0.772993 0.111 Uiso 1 1 calc R U . . .
H12B H 0.439886 0.178453 0.743742 0.111 Uiso 1 1 calc R U . . .
C9 C 0.2034(4) 0.5444(4) 0.5188(4) 0.0979(15) Uani 1 1 d . . . . .
H9A H 0.147340 0.486386 0.553928 0.117 Uiso 1 1 calc R U . . .
H9B H 0.158479 0.625889 0.504970 0.117 Uiso 1 1 calc R U . . .
C14 C 0.7136(4) 0.1167(5) 0.5398(4) 0.1041(16) Uani 1 1 d . . . . .
H14A H 0.761790 0.181223 0.520325 0.125 Uiso 1 1 calc R U . . .
H14B H 0.769387 0.040781 0.551151 0.125 Uiso 1 1 calc R U . . .
C3 C 0.7052(5) 0.1725(5) 0.3547(4) 0.1082(17) Uani 1 1 d . . . . .
H3A H 0.746375 0.240858 0.340160 0.130 Uiso 1 1 calc R U . . .
H3B H 0.767069 0.103604 0.355129 0.130 Uiso 1 1 calc R U . . .
C13 C 0.6368(5) 0.1065(4) 0.6395(4) 0.1073(16) Uani 1 1 d . . . . .
H13A H 0.584897 0.045381 0.657117 0.129 Uiso 1 1 calc R U . . .
H13B H 0.688102 0.081859 0.698247 0.129 Uiso 1 1 calc R U . . .
C7 C 0.2451(4) 0.5778(4) 0.2404(4) 0.0932(14) Uani 1 1 d . . . . .
H7A H 0.187037 0.593177 0.188800 0.112 Uiso 1 1 calc R U . . .
H7B H 0.291893 0.644494 0.211983 0.112 Uiso 1 1 calc R U . . .
C4 C 0.6270(5) 0.2034(6) 0.2725(4) 0.125(2) Uani 1 1 d . . . . .
H4A H 0.675582 0.218465 0.204950 0.149 Uiso 1 1 calc R U . . .
H4B H 0.586002 0.134881 0.287228 0.149 Uiso 1 1 calc R U . . .
C6 C 0.3994(5) 0.4708(6) 0.1617(4) 0.127(2) Uani 1 1 d . . . . .
H6A H 0.451659 0.531865 0.142731 0.152 Uiso 1 1 calc R U . . .
H6B H 0.349086 0.494453 0.102461 0.152 Uiso 1 1 calc R U . . .
C5 C 0.4735(6) 0.3565(7) 0.1759(4) 0.155(3) Uani 1 1 d . . . . .
H5A H 0.421348 0.299862 0.180788 0.186 Uiso 1 1 calc R U . . .
H5B H 0.529288 0.366794 0.112634 0.186 Uiso 1 1 calc R U . . .
C1A C 0.312(2) 0.199(2) 0.525(2) 0.108(6) Uani 0.421(15) 1 d . U P B 2
H1AD H 0.303418 0.164061 0.475154 0.130 Uiso 0.421(15) 1 calc R U P B 2
H1AE H 0.366054 0.136790 0.576555 0.130 Uiso 0.421(15) 1 calc R U P B 2
C1 C 0.3299(19) 0.2021(19) 0.465(2) 0.165(7) Uani 0.579(15) 1 d . U P B 1
H1A H 0.365959 0.172521 0.410082 0.198 Uiso 0.579(15) 1 calc R U P B 1
H1B H 0.343775 0.134284 0.533703 0.198 Uiso 0.579(15) 1 calc R U P B 1
Br1B Br 0.1058(3) 0.2298(4) 0.4748(4) 0.0996(16) Uani 0.182(2) 1 d . . P B 2
Br1 Br 0.1220(5) 0.2032(6) 0.5680(5) 0.164(2) Uani 0.239(3) 1 d . . P B 1
C2 C 0.2082(11) 0.2311(10) 0.4561(11) 0.154(7) Uani 0.579(15) 1 d . U P B 1
H2A H 0.186296 0.186707 0.418625 0.185 Uiso 0.579(15) 1 calc R U P B 1
H2B H 0.189400 0.317415 0.411762 0.185 Uiso 0.579(15) 1 calc R U P B 1
C2A C 0.220(2) 0.194(2) 0.5730(18) 0.157(9) Uani 0.421(15) 1 d . . P B 2
H2AA H 0.203204 0.252698 0.606128 0.188 Uiso 0.421(15) 1 calc R U P B 2
H2AB H 0.218203 0.112914 0.628581 0.188 Uiso 0.421(15) 1 calc R U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S1 2.1689(10) . ?
Ni1 S2 2.1582(9) . ?
Ni1 S7 2.1550(10) . ?
Ni1 S6 2.1677(9) . ?
S1 C15 1.721(3) . ?
S3 C15 1.742(3) . ?
S3 C17 1.730(3) . ?
S9 C19 1.742(3) . ?
S9 C20 1.715(4) . ?
S4 C16 1.735(3) . ?
S4 C17 1.717(4) . ?
S2 C16 1.718(3) . ?
S7 C19 1.708(3) . ?
S6 C18 1.719(3) . ?
S8 C18 1.743(3) . ?
S8 C20 1.736(4) . ?
S5 C17 1.651(3) . ?
S10 C20 1.644(3) . ?
O5 C10 1.424(5) . ?
O5 C11 1.413(5) . ?
O6 C12 1.405(5) . ?
O6 C13 1.401(5) . ?
O4 C8 1.373(5) . ?
O4 C9 1.422(5) . ?
O1 C14 1.404(5) . ?
O1 C3 1.414(5) . ?
N1 H1BD 0.8900 . ?
N1 H1BE 0.8900 . ?
N1 H1BF 0.8900 . ?
N1 H1AA 0.8900 . ?
N1 H1AB 0.8900 . ?
N1 H1AC 0.8900 . ?
N1 C1A 1.54(2) . ?
N1 C1 1.43(2) . ?
O3 C7 1.387(5) . ?
O3 C6 1.396(5) . ?
O2 C4 1.386(5) . ?
O2 C5 1.358(5) . ?
C19 C18 1.349(4) . ?
C15 C16 1.353(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C9 1.481(6) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C7 1.460(6) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.477(6) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C13 1.477(6) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.413(6) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C5 1.418(7) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C1A H1AD 0.9700 . ?
C1A H1AE 0.9700 . ?
C1A C2A 1.14(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.35(2) . ?
Br1B C2A 1.858(17) . ?
Br1 C2 1.634(15) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S2 Ni1 S1 93.20(3) . . ?
S2 Ni1 S6 175.93(4) . . ?
S7 Ni1 S1 176.04(4) . . ?
S7 Ni1 S2 85.63(3) . . ?
S7 Ni1 S6 92.84(3) . . ?
S6 Ni1 S1 88.57(3) . . ?
C15 S1 Ni1 101.84(11) . . ?
C17 S3 C15 97.26(15) . . ?
C20 S9 C19 97.28(16) . . ?
C17 S4 C16 97.55(15) . . ?
C16 S2 Ni1 102.19(11) . . ?
C19 S7 Ni1 102.74(12) . . ?
C18 S6 Ni1 101.72(11) . . ?
C20 S8 C18 97.58(16) . . ?
C11 O5 C10 112.1(3) . . ?
C13 O6 C12 114.5(3) . . ?
C8 O4 C9 115.7(3) . . ?
C14 O1 C3 113.6(4) . . ?
H1BD N1 H1BE 109.5 . . ?
H1BD N1 H1BF 109.5 . . ?
H1BE N1 H1BF 109.5 . . ?
H1AA N1 H1AB 109.5 . . ?
H1AA N1 H1AC 109.5 . . ?
H1AB N1 H1AC 109.5 . . ?
C1A N1 H1BD 109.5 . . ?
C1A N1 H1BE 109.5 . . ?
C1A N1 H1BF 109.5 . . ?
C1 N1 H1AA 109.5 . . ?
C1 N1 H1AB 109.5 . . ?
C1 N1 H1AC 109.5 . . ?
C7 O3 C6 115.2(4) . . ?
C5 O2 C4 117.8(4) . . ?
S7 C19 S9 122.2(2) . . ?
C18 C19 S9 116.9(2) . . ?
C18 C19 S7 120.9(2) . . ?
S1 C15 S3 122.83(19) . . ?
C16 C15 S1 121.4(2) . . ?
C16 C15 S3 115.7(2) . . ?
S2 C16 S4 122.34(19) . . ?
C15 C16 S4 116.3(2) . . ?
C15 C16 S2 121.4(2) . . ?
S6 C18 S8 123.1(2) . . ?
C19 C18 S6 121.8(2) . . ?
C19 C18 S8 115.2(3) . . ?
S9 C20 S8 113.05(18) . . ?
S10 C20 S9 123.2(2) . . ?
S10 C20 S8 123.7(2) . . ?
S4 C17 S3 113.16(17) . . ?
S5 C17 S3 123.8(2) . . ?
S5 C17 S4 123.0(2) . . ?
O5 C10 H10A 109.8 . . ?
O5 C10 H10B 109.8 . . ?
O5 C10 C9 109.2(4) . . ?
H10A C10 H10B 108.3 . . ?
C9 C10 H10A 109.8 . . ?
C9 C10 H10B 109.8 . . ?
O4 C8 H8A 109.4 . . ?
O4 C8 H8B 109.4 . . ?
O4 C8 C7 111.0(4) . . ?
H8A C8 H8B 108.0 . . ?
C7 C8 H8A 109.4 . . ?
C7 C8 H8B 109.4 . . ?
O5 C11 H11A 109.9 . . ?
O5 C11 H11B 109.9 . . ?
O5 C11 C12 108.9(4) . . ?
H11A C11 H11B 108.3 . . ?
C12 C11 H11A 109.9 . . ?
C12 C11 H11B 109.9 . . ?
O6 C12 C11 108.8(4) . . ?
O6 C12 H12A 109.9 . . ?
O6 C12 H12B 109.9 . . ?
C11 C12 H12A 109.9 . . ?
C11 C12 H12B 109.9 . . ?
H12A C12 H12B 108.3 . . ?
O4 C9 C10 107.8(3) . . ?
O4 C9 H9A 110.1 . . ?
O4 C9 H9B 110.1 . . ?
C10 C9 H9A 110.1 . . ?
C10 C9 H9B 110.1 . . ?
H9A C9 H9B 108.5 . . ?
O1 C14 H14A 109.6 . . ?
O1 C14 H14B 109.6 . . ?
O1 C14 C13 110.3(4) . . ?
H14A C14 H14B 108.1 . . ?
C13 C14 H14A 109.6 . . ?
C13 C14 H14B 109.6 . . ?
O1 C3 H3A 109.3 . . ?
O1 C3 H3B 109.3 . . ?
H3A C3 H3B 107.9 . . ?
C4 C3 O1 111.7(4) . . ?
C4 C3 H3A 109.3 . . ?
C4 C3 H3B 109.3 . . ?
O6 C13 C14 108.5(4) . . ?
O6 C13 H13A 110.0 . . ?
O6 C13 H13B 110.0 . . ?
C14 C13 H13A 110.0 . . ?
C14 C13 H13B 110.0 . . ?
H13A C13 H13B 108.4 . . ?
O3 C7 C8 112.6(4) . . ?
O3 C7 H7A 109.1 . . ?
O3 C7 H7B 109.1 . . ?
C8 C7 H7A 109.1 . . ?
C8 C7 H7B 109.1 . . ?
H7A C7 H7B 107.8 . . ?
O2 C4 C3 112.5(5) . . ?
O2 C4 H4A 109.1 . . ?
O2 C4 H4B 109.1 . . ?
C3 C4 H4A 109.1 . . ?
C3 C4 H4B 109.1 . . ?
H4A C4 H4B 107.8 . . ?
O3 C6 H6A 108.9 . . ?
O3 C6 H6B 108.9 . . ?
O3 C6 C5 113.3(5) . . ?
H6A C6 H6B 107.7 . . ?
C5 C6 H6A 108.9 . . ?
C5 C6 H6B 108.9 . . ?
O2 C5 C6 115.5(5) . . ?
O2 C5 H5A 108.4 . . ?
O2 C5 H5B 108.4 . . ?
C6 C5 H5A 108.4 . . ?
C6 C5 H5B 108.4 . . ?
H5A C5 H5B 107.5 . . ?
N1 C1A H1AD 102.1 . . ?
N1 C1A H1AE 102.1 . . ?
H1AD C1A H1AE 104.8 . . ?
C2A C1A N1 140(2) . . ?
C2A C1A H1AD 102.1 . . ?
C2A C1A H1AE 102.1 . . ?
N1 C1 H1A 107.5 . . ?
N1 C1 H1B 107.5 . . ?
H1A C1 H1B 107.0 . . ?
C2 C1 N1 119.2(16) . . ?
C2 C1 H1A 107.5 . . ?
C2 C1 H1B 107.5 . . ?
C1 C2 Br1 116.2(14) . . ?
C1 C2 H2A 108.2 . . ?
C1 C2 H2B 108.2 . . ?
Br1 C2 H2A 108.2 . . ?
Br1 C2 H2B 108.2 . . ?
H2A C2 H2B 107.4 . . ?
C1A C2A Br1B 105.6(17) . . ?
C1A C2A H2AA 110.6 . . ?
C1A C2A H2AB 110.6 . . ?
Br1B C2A H2AA 110.6 . . ?
Br1B C2A H2AB 110.6 . . ?
H2AA C2A H2AB 108.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S1 C15 S3 178.65(16) . . . . ?
Ni1 S1 C15 C16 1.3(3) . . . . ?
Ni1 S2 C16 S4 -178.79(17) . . . . ?
Ni1 S2 C16 C15 0.5(3) . . . . ?
Ni1 S7 C19 S9 178.21(17) . . . . ?
Ni1 S7 C19 C18 -0.8(3) . . . . ?
Ni1 S6 C18 S8 -179.57(19) . . . . ?
Ni1 S6 C18 C19 0.4(3) . . . . ?
S1 C15 C16 S4 178.04(17) . . . . ?
S1 C15 C16 S2 -1.3(4) . . . . ?
S3 C15 C16 S4 0.5(3) . . . . ?
S3 C15 C16 S2 -178.84(17) . . . . ?
S9 C19 C18 S6 -178.80(18) . . . . ?
S9 C19 C18 S8 1.2(4) . . . . ?
S7 C19 C18 S6 0.3(4) . . . . ?
S7 C19 C18 S8 -179.75(17) . . . . ?
O5 C10 C9 O4 -67.0(5) . . . . ?
O5 C11 C12 O6 63.6(5) . . . . ?
O4 C8 C7 O3 49.2(6) . . . . ?
O1 C14 C13 O6 -64.5(5) . . . . ?
O1 C3 C4 O2 62.2(7) . . . . ?
N1 C1A C2A Br1B 88(3) . . . . ?
N1 C1 C2 Br1 -93.5(19) . . . . ?
O3 C6 C5 O2 -52.1(8) . . . . ?
C19 S9 C20 S8 0.2(2) . . . . ?
C19 S9 C20 S10 -179.5(2) . . . . ?
C15 S3 C17 S4 -0.9(2) . . . . ?
C15 S3 C17 S5 179.7(2) . . . . ?
C16 S4 C17 S3 1.1(2) . . . . ?
C16 S4 C17 S5 -179.4(2) . . . . ?
C18 S8 C20 S9 0.3(2) . . . . ?
C18 S8 C20 S10 -180.0(2) . . . . ?
C20 S9 C19 S7 -179.9(2) . . . . ?
C20 S9 C19 C18 -0.9(3) . . . . ?
C20 S8 C18 S6 179.1(2) . . . . ?
C20 S8 C18 C19 -0.9(3) . . . . ?
C17 S3 C15 S1 -177.2(2) . . . . ?
C17 S3 C15 C16 0.2(3) . . . . ?
C17 S4 C16 S2 178.3(2) . . . . ?
C17 S4 C16 C15 -1.0(3) . . . . ?
C10 O5 C11 C12 -178.0(3) . . . . ?
C8 O4 C9 C10 -170.2(4) . . . . ?
C11 O5 C10 C9 -173.8(3) . . . . ?
C12 O6 C13 C14 -169.6(4) . . . . ?
C9 O4 C8 C7 172.2(4) . . . . ?
C14 O1 C3 C4 -177.2(5) . . . . ?
C3 O1 C14 C13 170.6(4) . . . . ?
C13 O6 C12 C11 171.2(4) . . . . ?
C7 O3 C6 C5 -176.9(5) . . . . ?
C4 O2 C5 C6 -170.8(5) . . . . ?
C6 O3 C7 C8 -173.5(4) . . . . ?
C5 O2 C4 C3 168.9(6) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.343
_oxdiff_exptl_absorpt_empirical_full_min 0.263
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_353k
_database_code_depnum_ccdc_archive 'CCDC 2053311'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-18 downloaded from the CCDC.
;
_audit_creation_date             2020-11-10
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C2 H7 Br N, C12 H24 O6'
_chemical_formula_sum            'C20 H31 Br N Ni O6 S10'
_chemical_formula_weight         840.68
_chemical_melting_point          ?
_chemical_oxdiff_formula         BrCHNONiS
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.2110(4)
_cell_length_b                   12.1703(4)
_cell_length_c                   13.7456(5)
_cell_angle_alpha                65.635(3)
_cell_angle_beta                 81.252(3)
_cell_angle_gamma                78.145(3)
_cell_volume                     1667.21(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    12629
_cell_measurement_temperature    353
_cell_measurement_theta_max      28.8600
_cell_measurement_theta_min      1.8610
_shelx_estimated_absorpt_T_max   0.848
_shelx_estimated_absorpt_T_min   0.442
_exptl_absorpt_coefficient_mu    2.442
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47546
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             858
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1174
_diffrn_reflns_av_unetI/netI     0.0905
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.892
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            34600
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.043
_diffrn_reflns_theta_min         1.860
_diffrn_ambient_temperature      353
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     55.00 101.00   0.50    1.20    --   21.69 162.00-119.00   92
  2  ω     61.00 104.00   0.50    1.20    --   21.69  37.00 -90.00   86
  3  ω    -40.00  42.00   0.50    1.20    --   21.69  37.00 -90.00  164
  4  ω    -25.00  61.00   0.50    1.20    --  -21.62  19.00 -30.00  172
  5  ω    -58.00  -8.00   0.50    1.20    --  -21.62 116.00  90.00  100
  6  ω   -100.00 -74.00   0.50    1.20    --  -21.62 162.00-119.00   52
  7  ω    -25.00  53.00   0.50    1.20    --  -21.62  19.00-120.00  156
  8  ω     27.00  88.00   0.50    1.20    --   21.69-116.00   2.00  122
  9  ω     74.00 103.00   0.50    1.20    --   21.69-162.00-147.00   58
 10  ω    -62.00  28.00   0.50    1.20    --   21.69 -19.00   0.00  180
 11  ω    -68.00 -42.00   0.50    1.20    --   21.69 -37.00-180.00   52
 12  ω     -1.00  41.00   0.50    1.20    --   21.69 -37.00-180.00   84
 13  ω   -103.00  19.00   0.50    1.20    --  -21.62 -57.00-120.00  244
 14  ω   -111.00 -85.00   0.50    1.20    --  -21.62 -37.00-150.00   52
 15  ω    -29.00  44.00   0.50    1.20    --  -21.62 -37.00-150.00  146
 16  ω      6.00  43.00   0.50    1.20    --  -21.62 -37.00   0.00   74
 17  ω   -112.00 -14.00   0.50    1.20    --  -21.62 -37.00   0.00  196
 18  ω   -103.00  19.00   0.50    1.20    --  -21.62 -57.00  90.00  244
 19  ω    -12.00  38.00   0.50    1.20    --  -21.62 -99.00 -30.00  100
 20  ω   -109.00 -84.00   0.50    1.20    --  -21.62-162.00-147.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0297695000
_diffrn_orient_matrix_UB_12      0.0067886000
_diffrn_orient_matrix_UB_13      0.0387192000
_diffrn_orient_matrix_UB_21      -0.0242447000
_diffrn_orient_matrix_UB_22      -0.0504897000
_diffrn_orient_matrix_UB_23      0.0406920000
_diffrn_orient_matrix_UB_31      0.0522416000
_diffrn_orient_matrix_UB_32      -0.0400443000
_diffrn_orient_matrix_UB_33      -0.0085043000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4614
_reflns_number_total             7944
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         7944
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.1044
_refine_ls_R_factor_gt           0.0522
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0546P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1510
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C15 \\sim C16: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C1A \\sim N1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
C1 \\sim C2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
3. Others
 1*[Sof(Br1)]+1*[Sof(Br1B)]+1*[Sof(Br1A)]=1 with esd of 0.0001
 Sof(H1BD)=Sof(H1BE)=Sof(H1BF)=Sof(C1A)=Sof(H1AD)=Sof(H1AE)=Sof(C2A)=Sof(H2AA)=
 Sof(H2AB)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=
 Sof(H2B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C8(H8A,H8B), C11(H11A,H11B), C12(H12A,H12B), C9(H9A,H9B),
 C14(H14A,H14B), C3(H3A,H3B), C13(H13A,H13B), C7(H7A,H7B), C4(H4A,H4B), C6(H6A,
 H6B), C5(H5A,H5B), C1A(H1AD,H1AE), C1(H1A,H1B), C2(H2A,H2B), C2A(H2AA,H2AB)
4.b Idealised Me refined as rotating group:
 N1(H1BD,H1BE,H1BF), N1(H1AA,H1AB,H1AC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.13321(4) 0.46385(4) 0.88312(3) 0.04837(15) Uani 1 1 d . . . . .
S1 S 0.09979(8) 0.33925(8) 0.81759(8) 0.0537(2) Uani 1 1 d . . . . .
S3 S 0.20705(9) 0.07283(8) 0.86698(8) 0.0563(3) Uani 1 1 d . . . . .
S9 S 0.05431(9) 0.84271(8) 0.92096(8) 0.0581(3) Uani 1 1 d . . . . .
S4 S 0.35630(8) 0.06324(8) 1.02447(8) 0.0560(3) Uani 1 1 d . . . . .
S2 S 0.26426(9) 0.32802(8) 0.98847(8) 0.0591(3) Uani 1 1 d . . . . .
S7 S 0.15978(9) 0.58050(8) 0.95814(8) 0.0610(3) Uani 1 1 d . . . . .
S6 S 0.01178(10) 0.60747(9) 0.77145(9) 0.0635(3) Uani 1 1 d . . . . .
S8 S -0.07946(10) 0.87051(9) 0.74697(9) 0.0709(3) Uani 1 1 d . . . . .
S5 S 0.36370(11) -0.16151(9) 0.98819(10) 0.0742(3) Uani 1 1 d . . . . .
S10 S -0.09615(11) 1.08156(10) 0.80854(11) 0.0804(4) Uani 1 1 d . . . . .
Br1A Br 0.07814(11) 0.14506(13) 0.54022(15) 0.0996(5) Uani 0.581(3) 1 d . . P A
3
O5 O 0.3589(2) 0.3933(3) 0.6182(2) 0.0718(8) Uani 1 1 d . . . . .
O6 O 0.5654(3) 0.2203(3) 0.6244(2) 0.0788(8) Uani 1 1 d . . . . .
O4 O 0.2564(3) 0.5354(3) 0.4212(2) 0.0839(9) Uani 1 1 d . . . . .
O1 O 0.6409(3) 0.1417(3) 0.4567(3) 0.0880(9) Uani 1 1 d . . . . .
N1 N 0.3975(3) 0.2935(3) 0.4589(3) 0.0654(9) Uani 1 1 d . U . . .
H1BD H 0.431380 0.279310 0.401394 0.078 Uiso 0.425(17) 1 calc R U P B 2
H1BE H 0.455878 0.293941 0.495852 0.078 Uiso 0.425(17) 1 calc R U P B 2
H1BF H 0.348994 0.365622 0.438293 0.078 Uiso 0.425(17) 1 calc R U P B 2
H1AA H 0.475979 0.260408 0.457594 0.078 Uiso 0.575(17) 1 calc R U P B 1
H1AB H 0.378873 0.315104 0.514470 0.078 Uiso 0.575(17) 1 calc R U P B 1
H1AC H 0.383792 0.359172 0.398487 0.078 Uiso 0.575(17) 1 calc R U P B 1
O3 O 0.3224(3) 0.4681(3) 0.2533(3) 0.0944(10) Uani 1 1 d . . . . .
O2 O 0.5410(3) 0.3056(4) 0.2634(3) 0.1120(13) Uani 1 1 d . . . . .
C19 C 0.0696(3) 0.7145(3) 0.8898(3) 0.0490(8) Uani 1 1 d . . . . .
C15 C 0.1967(3) 0.2087(3) 0.8852(3) 0.0454(8) Uani 1 1 d . U . . .
C16 C 0.2663(3) 0.2028(3) 0.9593(3) 0.0470(8) Uani 1 1 d . U . . .
C18 C 0.0061(3) 0.7274(3) 0.8089(3) 0.0532(9) Uani 1 1 d . . . . .
C20 C -0.0430(3) 0.9386(3) 0.8251(3) 0.0590(10) Uani 1 1 d . . . . .
C17 C 0.3114(3) -0.0155(3) 0.9611(3) 0.0518(9) Uani 1 1 d . . . . .
C10 C 0.3028(4) 0.5174(4) 0.5877(4) 0.0808(13) Uani 1 1 d . . . . .
H10A H 0.363134 0.570441 0.549740 0.097 Uiso 1 1 calc R U . . .
H10B H 0.270114 0.532975 0.651182 0.097 Uiso 1 1 calc R U . . .
C8 C 0.1785(4) 0.5737(5) 0.3410(4) 0.0946(16) Uani 1 1 d . . . . .
H8A H 0.134396 0.654518 0.331081 0.114 Uiso 1 1 calc R U . . .
H8B H 0.119250 0.518510 0.361746 0.114 Uiso 1 1 calc R U . . .
C11 C 0.4469(4) 0.3583(5) 0.6935(3) 0.0814(13) Uani 1 1 d . . . . .
H11A H 0.408126 0.367619 0.758340 0.098 Uiso 1 1 calc R U . . .
H11B H 0.509318 0.410488 0.664328 0.098 Uiso 1 1 calc R U . . .
C12 C 0.5035(4) 0.2296(5) 0.7189(4) 0.0841(14) Uani 1 1 d . . . . .
H12A H 0.560523 0.203695 0.773552 0.101 Uiso 1 1 calc R U . . .
H12B H 0.440989 0.177428 0.745844 0.101 Uiso 1 1 calc R U . . .
C9 C 0.2039(4) 0.5443(5) 0.5187(4) 0.0907(15) Uani 1 1 d . . . . .
H9A H 0.147251 0.486450 0.553600 0.109 Uiso 1 1 calc R U . . .
H9B H 0.159366 0.625875 0.504929 0.109 Uiso 1 1 calc R U . . .
C14 C 0.7154(4) 0.1172(5) 0.5391(4) 0.0941(16) Uani 1 1 d . . . . .
H14A H 0.762677 0.182754 0.519104 0.113 Uiso 1 1 calc R U . . .
H14B H 0.771804 0.041831 0.550328 0.113 Uiso 1 1 calc R U . . .
C3 C 0.7075(5) 0.1722(5) 0.3553(4) 0.0993(17) Uani 1 1 d . . . . .
H3A H 0.770328 0.103988 0.356042 0.119 Uiso 1 1 calc R U . . .
H3B H 0.747200 0.241816 0.340363 0.119 Uiso 1 1 calc R U . . .
C13 C 0.6380(5) 0.1063(5) 0.6394(4) 0.1021(17) Uani 1 1 d . . . . .
H13A H 0.586252 0.044863 0.656838 0.123 Uiso 1 1 calc R U . . .
H13B H 0.689146 0.081668 0.698094 0.123 Uiso 1 1 calc R U . . .
C7 C 0.2456(4) 0.5769(5) 0.2408(4) 0.0869(14) Uani 1 1 d . . . . .
H7A H 0.188007 0.593687 0.188544 0.104 Uiso 1 1 calc R U . . .
H7B H 0.293559 0.642848 0.213524 0.104 Uiso 1 1 calc R U . . .
C4 C 0.6277(5) 0.2010(6) 0.2736(5) 0.113(2) Uani 1 1 d . . . . .
H4A H 0.675581 0.214290 0.205898 0.136 Uiso 1 1 calc R U . . .
H4B H 0.585750 0.132369 0.290543 0.136 Uiso 1 1 calc R U . . .
C6 C 0.4003(5) 0.4712(6) 0.1616(4) 0.115(2) Uani 1 1 d . . . . .
H6A H 0.453812 0.530958 0.144977 0.138 Uiso 1 1 calc R U . . .
H6B H 0.351282 0.497244 0.101255 0.138 Uiso 1 1 calc R U . . .
C5 C 0.4732(6) 0.3548(7) 0.1758(5) 0.147(3) Uani 1 1 d . . . . .
H5A H 0.419821 0.298187 0.182595 0.176 Uiso 1 1 calc R U . . .
H5B H 0.528147 0.363747 0.112145 0.176 Uiso 1 1 calc R U . . .
C1A C 0.321(3) 0.192(2) 0.5301(19) 0.120(7) Uani 0.425(17) 1 d . U P B 2
H1AD H 0.328756 0.138977 0.492041 0.143 Uiso 0.425(17) 1 calc R U P B 2
H1AE H 0.366234 0.144885 0.593441 0.143 Uiso 0.425(17) 1 calc R U P B 2
C1 C 0.322(2) 0.2053(16) 0.469(2) 0.142(6) Uani 0.575(17) 1 d . U P B 1
H1A H 0.364030 0.165237 0.421900 0.171 Uiso 0.575(17) 1 calc R U P B 1
H1B H 0.329111 0.144014 0.541097 0.171 Uiso 0.575(17) 1 calc R U P B 1
Br1B Br 0.1048(3) 0.2299(4) 0.4748(4) 0.0923(15) Uani 0.189(2) 1 d . . P B 2
Br1 Br 0.1226(5) 0.2037(5) 0.5699(4) 0.153(2) Uani 0.230(3) 1 d . . P B 1
C2 C 0.2087(14) 0.2257(11) 0.4522(11) 0.139(7) Uani 0.575(17) 1 d . U P B 1
H2A H 0.193094 0.170845 0.422269 0.167 Uiso 0.575(17) 1 calc R U P B 1
H2B H 0.186890 0.308932 0.401293 0.167 Uiso 0.575(17) 1 calc R U P B 1
C2A C 0.2135(19) 0.203(2) 0.564(2) 0.184(13) Uani 0.425(17) 1 d . . P B 2
H2AA H 0.197377 0.268957 0.588081 0.221 Uiso 0.425(17) 1 calc R U P B 2
H2AB H 0.201444 0.128386 0.625917 0.221 Uiso 0.425(17) 1 calc R U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S1 2.1712(10) . ?
Ni1 S2 2.1592(10) . ?
Ni1 S7 2.1547(10) . ?
Ni1 S6 2.1700(10) . ?
S1 C15 1.717(3) . ?
S3 C15 1.751(3) . ?
S3 C17 1.730(3) . ?
S9 C19 1.752(3) . ?
S9 C20 1.713(4) . ?
S4 C16 1.738(3) . ?
S4 C17 1.718(4) . ?
S2 C16 1.723(3) . ?
S7 C19 1.706(3) . ?
S6 C18 1.724(4) . ?
S8 C18 1.737(3) . ?
S8 C20 1.736(4) . ?
S5 C17 1.653(3) . ?
S10 C20 1.650(4) . ?
O5 C10 1.422(5) . ?
O5 C11 1.415(5) . ?
O6 C12 1.413(5) . ?
O6 C13 1.408(5) . ?
O4 C8 1.377(5) . ?
O4 C9 1.418(5) . ?
O1 C14 1.406(5) . ?
O1 C3 1.417(6) . ?
N1 H1BD 0.8900 . ?
N1 H1BE 0.8900 . ?
N1 H1BF 0.8900 . ?
N1 H1AA 0.8900 . ?
N1 H1AB 0.8900 . ?
N1 H1AC 0.8900 . ?
N1 C1A 1.55(3) . ?
N1 C1 1.449(18) . ?
O3 C7 1.383(5) . ?
O3 C6 1.411(6) . ?
O2 C4 1.404(6) . ?
O2 C5 1.372(6) . ?
C19 C18 1.348(5) . ?
C15 C16 1.345(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C9 1.466(6) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C7 1.455(7) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.478(6) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C13 1.484(7) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.427(7) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C5 1.435(8) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C1A H1AD 0.9700 . ?
C1A H1AE 0.9700 . ?
C1A C2A 1.23(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.28(2) . ?
Br1B C2A 1.74(2) . ?
Br1 C2 1.701(18) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S2 Ni1 S1 93.11(3) . . ?
S2 Ni1 S6 176.02(5) . . ?
S7 Ni1 S1 176.11(4) . . ?
S7 Ni1 S2 85.66(4) . . ?
S7 Ni1 S6 92.88(4) . . ?
S6 Ni1 S1 88.58(4) . . ?
C15 S1 Ni1 101.70(11) . . ?
C17 S3 C15 97.07(16) . . ?
C20 S9 C19 97.14(17) . . ?
C17 S4 C16 97.15(16) . . ?
C16 S2 Ni1 102.16(12) . . ?
C19 S7 Ni1 102.43(12) . . ?
C18 S6 Ni1 101.90(12) . . ?
C20 S8 C18 97.43(17) . . ?
C11 O5 C10 112.8(3) . . ?
C13 O6 C12 114.8(4) . . ?
C8 O4 C9 116.1(4) . . ?
C14 O1 C3 112.1(4) . . ?
H1BD N1 H1BE 109.5 . . ?
H1BD N1 H1BF 109.5 . . ?
H1BE N1 H1BF 109.5 . . ?
H1AA N1 H1AB 109.5 . . ?
H1AA N1 H1AC 109.5 . . ?
H1AB N1 H1AC 109.5 . . ?
C1A N1 H1BD 109.5 . . ?
C1A N1 H1BE 109.5 . . ?
C1A N1 H1BF 109.5 . . ?
C1 N1 H1AA 109.5 . . ?
C1 N1 H1AB 109.5 . . ?
C1 N1 H1AC 109.5 . . ?
C7 O3 C6 114.3(4) . . ?
C5 O2 C4 117.2(4) . . ?
S7 C19 S9 121.8(2) . . ?
C18 C19 S9 116.3(2) . . ?
C18 C19 S7 121.9(3) . . ?
S1 C15 S3 122.57(19) . . ?
C16 C15 S1 121.9(2) . . ?
C16 C15 S3 115.5(2) . . ?
S2 C16 S4 122.0(2) . . ?
C15 C16 S4 116.9(2) . . ?
C15 C16 S2 121.1(2) . . ?
S6 C18 S8 123.3(2) . . ?
C19 C18 S6 120.9(3) . . ?
C19 C18 S8 115.8(3) . . ?
S9 C20 S8 113.29(19) . . ?
S10 C20 S9 123.2(2) . . ?
S10 C20 S8 123.5(2) . . ?
S4 C17 S3 113.46(19) . . ?
S5 C17 S3 123.8(2) . . ?
S5 C17 S4 122.8(2) . . ?
O5 C10 H10A 109.6 . . ?
O5 C10 H10B 109.6 . . ?
O5 C10 C9 110.1(4) . . ?
H10A C10 H10B 108.2 . . ?
C9 C10 H10A 109.6 . . ?
C9 C10 H10B 109.6 . . ?
O4 C8 H8A 109.4 . . ?
O4 C8 H8B 109.4 . . ?
O4 C8 C7 111.0(4) . . ?
H8A C8 H8B 108.0 . . ?
C7 C8 H8A 109.4 . . ?
C7 C8 H8B 109.4 . . ?
O5 C11 H11A 109.7 . . ?
O5 C11 H11B 109.7 . . ?
O5 C11 C12 109.6(4) . . ?
H11A C11 H11B 108.2 . . ?
C12 C11 H11A 109.7 . . ?
C12 C11 H11B 109.7 . . ?
O6 C12 C11 108.5(4) . . ?
O6 C12 H12A 110.0 . . ?
O6 C12 H12B 110.0 . . ?
C11 C12 H12A 110.0 . . ?
C11 C12 H12B 110.0 . . ?
H12A C12 H12B 108.4 . . ?
O4 C9 C10 108.2(4) . . ?
O4 C9 H9A 110.0 . . ?
O4 C9 H9B 110.0 . . ?
C10 C9 H9A 110.0 . . ?
C10 C9 H9B 110.0 . . ?
H9A C9 H9B 108.4 . . ?
O1 C14 H14A 109.7 . . ?
O1 C14 H14B 109.7 . . ?
O1 C14 C13 109.6(4) . . ?
H14A C14 H14B 108.2 . . ?
C13 C14 H14A 109.7 . . ?
C13 C14 H14B 109.7 . . ?
O1 C3 H3A 109.6 . . ?
O1 C3 H3B 109.6 . . ?
O1 C3 C4 110.3(5) . . ?
H3A C3 H3B 108.1 . . ?
C4 C3 H3A 109.6 . . ?
C4 C3 H3B 109.6 . . ?
O6 C13 C14 108.7(4) . . ?
O6 C13 H13A 109.9 . . ?
O6 C13 H13B 109.9 . . ?
C14 C13 H13A 109.9 . . ?
C14 C13 H13B 109.9 . . ?
H13A C13 H13B 108.3 . . ?
O3 C7 C8 112.1(4) . . ?
O3 C7 H7A 109.2 . . ?
O3 C7 H7B 109.2 . . ?
C8 C7 H7A 109.2 . . ?
C8 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
O2 C4 C3 111.9(5) . . ?
O2 C4 H4A 109.2 . . ?
O2 C4 H4B 109.2 . . ?
C3 C4 H4A 109.2 . . ?
C3 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
O3 C6 H6A 109.1 . . ?
O3 C6 H6B 109.1 . . ?
O3 C6 C5 112.5(5) . . ?
H6A C6 H6B 107.8 . . ?
C5 C6 H6A 109.1 . . ?
C5 C6 H6B 109.1 . . ?
O2 C5 C6 114.1(5) . . ?
O2 C5 H5A 108.7 . . ?
O2 C5 H5B 108.7 . . ?
C6 C5 H5A 108.7 . . ?
C6 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
N1 C1A H1AD 105.1 . . ?
N1 C1A H1AE 105.1 . . ?
H1AD C1A H1AE 105.9 . . ?
C2A C1A N1 129(2) . . ?
C2A C1A H1AD 105.1 . . ?
C2A C1A H1AE 105.1 . . ?
N1 C1 H1A 105.4 . . ?
N1 C1 H1B 105.4 . . ?
H1A C1 H1B 106.0 . . ?
C2 C1 N1 127.5(16) . . ?
C2 C1 H1A 105.4 . . ?
C2 C1 H1B 105.4 . . ?
C1 C2 Br1 109.5(14) . . ?
C1 C2 H2A 109.8 . . ?
C1 C2 H2B 109.8 . . ?
Br1 C2 H2A 109.8 . . ?
Br1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.2 . . ?
C1A C2A Br1B 117.0(17) . . ?
C1A C2A H2AA 108.0 . . ?
C1A C2A H2AB 108.0 . . ?
Br1B C2A H2AA 108.0 . . ?
Br1B C2A H2AB 108.0 . . ?
H2AA C2A H2AB 107.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S1 C15 S3 178.58(18) . . . . ?
Ni1 S1 C15 C16 1.4(3) . . . . ?
Ni1 S2 C16 S4 -178.73(18) . . . . ?
Ni1 S2 C16 C15 0.6(3) . . . . ?
Ni1 S7 C19 S9 178.59(19) . . . . ?
Ni1 S7 C19 C18 -1.4(3) . . . . ?
Ni1 S6 C18 S8 -179.8(2) . . . . ?
Ni1 S6 C18 C19 0.3(3) . . . . ?
S1 C15 C16 S4 177.95(19) . . . . ?
S1 C15 C16 S2 -1.4(5) . . . . ?
S3 C15 C16 S4 0.5(4) . . . . ?
S3 C15 C16 S2 -178.78(18) . . . . ?
S9 C19 C18 S6 -179.2(2) . . . . ?
S9 C19 C18 S8 0.9(4) . . . . ?
S7 C19 C18 S6 0.8(5) . . . . ?
S7 C19 C18 S8 -179.2(2) . . . . ?
O5 C10 C9 O4 -66.5(5) . . . . ?
O5 C11 C12 O6 62.9(5) . . . . ?
O4 C8 C7 O3 51.5(6) . . . . ?
O1 C14 C13 O6 -65.1(6) . . . . ?
O1 C3 C4 O2 64.1(7) . . . . ?
N1 C1A C2A Br1B 79(2) . . . . ?
N1 C1 C2 Br1 -94(2) . . . . ?
O3 C6 C5 O2 -55.0(8) . . . . ?
C19 S9 C20 S8 0.0(2) . . . . ?
C19 S9 C20 S10 -179.7(3) . . . . ?
C15 S3 C17 S4 -0.7(2) . . . . ?
C15 S3 C17 S5 179.4(2) . . . . ?
C16 S4 C17 S3 0.9(2) . . . . ?
C16 S4 C17 S5 -179.2(2) . . . . ?
C18 S8 C20 S9 0.3(3) . . . . ?
C18 S8 C20 S10 -179.9(3) . . . . ?
C20 S9 C19 S7 179.5(2) . . . . ?
C20 S9 C19 C18 -0.5(3) . . . . ?
C20 S8 C18 S6 179.3(3) . . . . ?
C20 S8 C18 C19 -0.7(3) . . . . ?
C17 S3 C15 S1 -177.3(2) . . . . ?
C17 S3 C15 C16 0.1(3) . . . . ?
C17 S4 C16 S2 178.4(2) . . . . ?
C17 S4 C16 C15 -0.9(3) . . . . ?
C10 O5 C11 C12 -178.5(4) . . . . ?
C8 O4 C9 C10 -171.6(4) . . . . ?
C11 O5 C10 C9 -174.0(4) . . . . ?
C12 O6 C13 C14 -169.0(4) . . . . ?
C9 O4 C8 C7 171.8(4) . . . . ?
C14 O1 C3 C4 -177.7(5) . . . . ?
C3 O1 C14 C13 170.7(4) . . . . ?
C13 O6 C12 C11 171.5(4) . . . . ?
C7 O3 C6 C5 -176.6(5) . . . . ?
C4 O2 C5 C6 -170.9(5) . . . . ?
C6 O3 C7 C8 -172.8(5) . . . . ?
C5 O2 C4 C3 168.9(6) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.763
_oxdiff_exptl_absorpt_empirical_full_min 0.254
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_113k-f
_database_code_depnum_ccdc_archive 'CCDC 2053392'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-18 downloaded from the CCDC.
;
_audit_creation_date             2020-11-24
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C2 H7 Cl N, C12 H24 O6'
_chemical_formula_sum            'C20 H31 Cl N Ni O6 S10'
_chemical_formula_weight         796.22
_chemical_melting_point          ?
_chemical_oxdiff_formula         C20H30NO6NiS10Cl
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.2193(3)
_cell_length_b                   12.3191(2)
_cell_length_c                   12.7473(3)
_cell_angle_alpha                92.239(2)
_cell_angle_beta                 111.956(2)
_cell_angle_gamma                96.066(2)
_cell_volume                     1618.98(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    28482
_cell_measurement_temperature    113
_cell_measurement_theta_max      30.9490
_cell_measurement_theta_min      2.2900
_shelx_estimated_absorpt_T_max   0.791
_shelx_estimated_absorpt_T_min   0.453
_exptl_absorpt_coefficient_mu    1.363
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             822
_exptl_crystal_size_max          0.69
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0916
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            37298
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         1.974
_diffrn_ambient_temperature      113
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      9.00  77.00   0.50    0.26    --    5.18  51.00 -78.00  136
  2  ω    -21.00  19.00   0.50    0.26    --    5.18 -28.00-171.52   80
  3  ω    -51.00 -25.00   0.50    0.26    --    5.18 -28.00-171.52   52
  4  ω    -64.00  18.00   0.50    0.26    --    5.18 -23.00 -77.67  164
  5  ω    -68.00  19.00   0.50    0.26    --    5.18 -28.00  13.21  174
  6  ω    -69.00  18.00   0.50    0.26    --    5.18 -19.00  60.00  174
  7  ω    -67.00  19.00   0.50    0.26    --    5.18 -51.00 135.00  172
  8  ω    -66.00  18.00   0.50    0.26    --    5.18 -19.00 150.00  168
  9  ω    -79.00   8.00   0.50    0.26    --   -5.03 -19.00 -30.00  174
 10  ω    -18.00  55.00   0.50    0.26    --   -5.03  51.00 -78.00  146
 11  ω      5.00  39.00   0.50    0.26    --    5.18 -99.00 -90.00   68
 12  ω    -18.00  28.00   0.50    0.26    --   -5.03 -99.00 120.00   92
 13  ω    -72.00 -35.00   0.50    0.26    --   -5.03 -51.00 135.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0542762000
_diffrn_orient_matrix_UB_12      -0.0318274000
_diffrn_orient_matrix_UB_13      0.0042190000
_diffrn_orient_matrix_UB_21      -0.0230247000
_diffrn_orient_matrix_UB_22      -0.0172823000
_diffrn_orient_matrix_UB_23      -0.0586853000
_diffrn_orient_matrix_UB_31      0.0353571000
_diffrn_orient_matrix_UB_32      -0.0454469000
_diffrn_orient_matrix_UB_33      0.0128022000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5734
_reflns_number_total             6613
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT n/a (Sheldrick, 2015)'
_refine_diff_density_max         0.839
_refine_diff_density_min         -1.057
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         6613
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0446
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0848P)²+0.5937P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1268
_refine_ls_wR_factor_ref         0.1323
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
2. Others
 Sof(H7BC)=Sof(H7BD)=Sof(O4A)=Sof(O1A)=Sof(O6A)=Sof(H9BC)=Sof(H9BD)=Sof(O2A)=
 Sof(H3BC)=Sof(H3BD)=Sof(O3A)=Sof(O5A)=Sof(C11A)=Sof(H11A)=Sof(H11B)=Sof(C7A)=
 Sof(H7AC)=Sof(H7AD)=Sof(C9A)=Sof(H9AC)=Sof(H9AD)=Sof(C12A)=Sof(H12C)=Sof(H12D)=
 Sof(C3A)=Sof(H3AC)=Sof(H3AD)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(C13A)=Sof(H13C)=
 Sof(H13D)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(C14A)=Sof(H14C)=Sof(H14D)=1-FVAR(1)
 Sof(H7AA)=Sof(H7AB)=Sof(O3)=Sof(O6)=Sof(O1)=Sof(H9AA)=Sof(H9AB)=Sof(O2)=
 Sof(H3AA)=Sof(H3AB)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C5)=Sof(H5A)=Sof(H5B)=
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(C4)=Sof(H4A)=
 Sof(H4B)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(O5)=
 Sof(O4)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C11)=Sof(H11C)=Sof(H11D)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C7(H7BC,H7BD), C7(H7AA,H7AB), C9(H9BC,H9BD), C9(H9AA,H9AB),
 C2(H2A,H2B), C3(H3AA,H3AB), C3(H3BC,H3BD), C13(H13A,H13B), C11A(H11A,H11B),
 C5(H5A,H5B), C7A(H7AC,H7AD), C12(H12A,H12B), C10(H10A,H10B), C9A(H9AC,H9AD),
 C12A(H12C,H12D), C4(H4A,H4B), C14(H14A,H14B), C8(H8A,H8B), C6(H6A,H6B),
 C3A(H3AC,H3AD), C5A(H5AA,H5AB), C13A(H13C,H13D), C11(H11C,H11D), C6A(H6AA,
 H6AB), C14A(H14C,H14D)
3.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.34546(3) 0.89088(2) 1.01193(3) 0.02122(12) Uani 1 1 d . . . . .
S1 S 0.50583(6) 0.81062(5) 1.00748(6) 0.02575(16) Uani 1 1 d . . . . .
S4 S 0.41266(7) 0.89401(5) 0.66579(6) 0.02726(16) Uani 1 1 d . . . . .
S9 S 0.11354(6) 1.02865(5) 1.22144(6) 0.02823(17) Uani 1 1 d . . . . .
S8 S 0.30080(6) 0.90052(5) 1.36729(6) 0.02597(16) Uani 1 1 d . . . . .
S6 S 0.39688(6) 0.84143(5) 1.18225(6) 0.02478(16) Uani 1 1 d . . . . .
S2 S 0.29539(6) 0.93766(5) 0.84066(6) 0.02630(16) Uani 1 1 d . . . . .
S3 S 0.60048(7) 0.77015(6) 0.81729(6) 0.03081(17) Uani 1 1 d . . . . .
S7 S 0.19192(7) 0.97869(5) 1.02215(6) 0.02862(17) Uani 1 1 d . . . . .
S5 S 0.59259(7) 0.78886(6) 0.58339(7) 0.03641(19) Uani 1 1 d . . . . .
S10 S 0.12509(7) 1.00323(6) 1.45628(6) 0.03392(18) Uani 1 1 d . . . . .
Cl1 Cl 0.33929(10) 0.45257(7) 1.01425(8) 0.0595(3) Uani 1 1 d . . . . .
N1 N 0.1686(2) 0.50270(16) 0.75536(19) 0.0229(4) Uani 1 1 d . . . . .
H1A H 0.164307 0.518221 0.684933 0.027 Uiso 1 1 calc R U . . .
H1B H 0.089308 0.504083 0.759079 0.027 Uiso 1 1 calc R U . . .
H1C H 0.193305 0.434977 0.769266 0.027 Uiso 1 1 calc R U . . .
C19 C 0.2087(2) 0.96693(19) 1.1608(2) 0.0239(5) Uani 1 1 d . . . . .
C16 C 0.4071(2) 0.88283(19) 0.7999(2) 0.0235(5) Uani 1 1 d . . . . .
C18 C 0.2964(2) 0.90711(19) 1.2299(2) 0.0220(5) Uani 1 1 d . . . . .
C17 C 0.5386(3) 0.8166(2) 0.6840(2) 0.0279(5) Uani 1 1 d . . . . .
C1 C 0.2643(3) 0.5854(2) 0.8413(2) 0.0304(6) Uani 1 1 d . . . . .
H1D H 0.241699 0.659492 0.821496 0.036 Uiso 1 1 calc R U . . .
H1E H 0.351225 0.580705 0.839877 0.036 Uiso 1 1 calc R U . . .
C15 C 0.4973(2) 0.8255(2) 0.8723(2) 0.0240(5) Uani 1 1 d . . . . .
C20 C 0.1771(3) 0.9792(2) 1.3535(2) 0.0269(5) Uani 1 1 d . . . . .
C7 C 0.1461(3) 0.2027(2) 0.7988(3) 0.0457(8) Uani 1 1 d . . . . .
H7BC H 0.215789 0.214038 0.875466 0.055 Uiso 0.498(3) 1 calc R U P A 2
H7BD H 0.097017 0.129328 0.791991 0.055 Uiso 0.498(3) 1 calc R U P A 2
H7AA H 0.204246 0.151927 0.843903 0.055 Uiso 0.502(3) 1 calc R U P A 1
H7AB H 0.082879 0.159502 0.729614 0.055 Uiso 0.502(3) 1 calc R U P A 1
O4A O 0.0599(4) 0.2847(3) 0.7880(3) 0.0278(9) Uani 0.498(3) 1 d . . P A 2
O1A O 0.1428(4) 0.6613(3) 0.5906(4) 0.0278(9) Uani 0.498(3) 1 d . . P A 2
O3 O 0.2202(3) 0.2807(3) 0.7655(3) 0.0267(9) Uani 0.502(3) 1 d . . P A 1
O6 O -0.0010(4) 0.6541(3) 0.6359(4) 0.0292(9) Uani 0.502(3) 1 d . . P A 1
O6A O -0.0447(4) 0.6348(3) 0.6895(4) 0.0283(9) Uani 0.498(3) 1 d . . P A 2
O1 O 0.2160(4) 0.6168(3) 0.5827(3) 0.0268(9) Uani 0.502(3) 1 d . . P A 1
C9 C -0.0826(4) 0.3620(2) 0.8552(4) 0.0491(9) Uani 1 1 d . . . . .
H9BC H -0.108406 0.364497 0.921400 0.059 Uiso 0.498(3) 1 calc R U P A 2
H9BD H -0.160158 0.330970 0.788202 0.059 Uiso 0.498(3) 1 calc R U P A 2
H9AA H -0.143336 0.299686 0.859872 0.059 Uiso 0.502(3) 1 calc R U P A 1
H9AB H -0.028985 0.392484 0.933803 0.059 Uiso 0.502(3) 1 calc R U P A 1
C2 C 0.2691(4) 0.5697(2) 0.9594(3) 0.0442(8) Uani 1 1 d . . . . .
H2A H 0.179897 0.563489 0.958247 0.053 Uiso 1 1 calc R U . . .
H2B H 0.319585 0.635097 1.010449 0.053 Uiso 1 1 calc R U . . .
O2A O 0.2744(4) 0.4828(3) 0.5778(3) 0.0259(9) Uani 0.498(3) 1 d . . P A 2
O2 O 0.2965(4) 0.4107(3) 0.6177(3) 0.0289(9) Uani 0.502(3) 1 d . . P A 1
C3 C 0.2942(4) 0.5790(3) 0.5348(4) 0.0616(12) Uani 1 1 d . . . . .
H3AA H 0.353930 0.642178 0.530225 0.074 Uiso 0.502(3) 1 calc R U P A 1
H3AB H 0.239603 0.549670 0.455945 0.074 Uiso 0.502(3) 1 calc R U P A 1
H3BC H 0.313301 0.562530 0.466440 0.074 Uiso 0.498(3) 1 calc R U P A 2
H3BD H 0.372659 0.622744 0.591398 0.074 Uiso 0.498(3) 1 calc R U P A 2
O3A O 0.2690(4) 0.3097(3) 0.7134(3) 0.0271(9) Uani 0.498(3) 1 d . . P A 2
O5A O -0.0438(4) 0.4730(3) 0.8365(4) 0.0292(9) Uani 0.498(3) 1 d . . P A 2
C13 C 0.0252(10) 0.7083(8) 0.5488(8) 0.036(2) Uani 0.502(3) 1 d . . P A 1
H13A H -0.056589 0.700044 0.480940 0.043 Uiso 0.502(3) 1 calc R U P A 1
H13B H 0.047806 0.787392 0.574037 0.043 Uiso 0.502(3) 1 calc R U P A 1
C11A C -0.1408(6) 0.5452(5) 0.8043(5) 0.0325(13) Uani 0.498(3) 1 d . . P A 2
H11A H -0.172992 0.556178 0.865956 0.039 Uiso 0.498(3) 1 calc R U P A 2
H11B H -0.214757 0.512786 0.735278 0.039 Uiso 0.498(3) 1 calc R U P A 2
C5 C 0.3219(7) 0.3052(5) 0.6287(7) 0.0319(14) Uani 0.502(3) 1 d . . P A 1
H5A H 0.283954 0.266881 0.551491 0.038 Uiso 0.502(3) 1 calc R U P A 1
H5B H 0.417056 0.307167 0.654316 0.038 Uiso 0.502(3) 1 calc R U P A 1
C7A C 0.2025(6) 0.2046(4) 0.7179(5) 0.0290(12) Uani 0.498(3) 1 d . . P A 2
H7AC H 0.133865 0.181694 0.642215 0.035 Uiso 0.498(3) 1 calc R U P A 2
H7AD H 0.264760 0.150289 0.734457 0.035 Uiso 0.498(3) 1 calc R U P A 2
C12 C -0.0577(6) 0.7011(6) 0.7069(6) 0.0337(14) Uani 0.502(3) 1 d . . P A 1
H12A H -0.107129 0.760089 0.669222 0.040 Uiso 0.502(3) 1 calc R U P A 1
H12B H 0.010878 0.733111 0.779522 0.040 Uiso 0.502(3) 1 calc R U P A 1
C10 C -0.1533(5) 0.4399(5) 0.8007(5) 0.0333(13) Uani 0.502(3) 1 d . . P A 1
H10A H -0.204153 0.464503 0.843924 0.040 Uiso 0.502(3) 1 calc R U P A 1
H10B H -0.214883 0.408500 0.724626 0.040 Uiso 0.502(3) 1 calc R U P A 1
C9A C 0.0093(6) 0.2924(5) 0.8737(6) 0.0315(13) Uani 0.498(3) 1 d . . P A 2
H9AC H -0.029145 0.218421 0.881074 0.038 Uiso 0.498(3) 1 calc R U P A 2
H9AD H 0.081653 0.317294 0.946723 0.038 Uiso 0.498(3) 1 calc R U P A 2
C12A C -0.0835(7) 0.6536(5) 0.7816(6) 0.0332(14) Uani 0.498(3) 1 d . . P A 2
H12C H -0.148720 0.705482 0.762569 0.040 Uiso 0.498(3) 1 calc R U P A 2
H12D H -0.007997 0.685500 0.849816 0.040 Uiso 0.498(3) 1 calc R U P A 2
C4 C 0.3696(6) 0.4975(5) 0.5882(5) 0.0323(13) Uani 0.502(3) 1 d . . P A 1
H4A H 0.441945 0.531336 0.657713 0.039 Uiso 0.502(3) 1 calc R U P A 1
H4B H 0.407562 0.466706 0.536599 0.039 Uiso 0.502(3) 1 calc R U P A 1
C14 C 0.1155(6) 0.6787(5) 0.5164(6) 0.0335(13) Uani 0.502(3) 1 d . . P A 1
H14A H 0.160129 0.746762 0.501971 0.040 Uiso 0.502(3) 1 calc R U P A 1
H14B H 0.070214 0.636007 0.441908 0.040 Uiso 0.502(3) 1 calc R U P A 1
C8 C 0.0782(6) 0.2393(5) 0.8617(6) 0.0376(14) Uani 0.502(3) 1 d . . P A 1
H8A H 0.140185 0.270522 0.937673 0.045 Uiso 0.502(3) 1 calc R U P A 1
H8B H 0.021972 0.176626 0.872175 0.045 Uiso 0.502(3) 1 calc R U P A 1
O5 O -0.0718(4) 0.5315(4) 0.7887(4) 0.0311(9) Uani 0.502(3) 1 d . . P A 1
O4 O 0.0006(4) 0.3204(3) 0.8066(4) 0.0315(9) Uani 0.502(3) 1 d . . P A 1
C6 C 0.2839(5) 0.2417(5) 0.6961(5) 0.0289(12) Uani 0.502(3) 1 d . . P A 1
H6A H 0.362092 0.212786 0.747566 0.035 Uiso 0.502(3) 1 calc R U P A 1
H6B H 0.225790 0.178066 0.646911 0.035 Uiso 0.502(3) 1 calc R U P A 1
C3A C 0.1934(6) 0.6446(5) 0.5048(6) 0.0331(13) Uani 0.498(3) 1 d . . P A 2
H3AC H 0.122206 0.610033 0.434929 0.040 Uiso 0.498(3) 1 calc R U P A 2
H3AD H 0.225740 0.716832 0.487322 0.040 Uiso 0.498(3) 1 calc R U P A 2
C5A C 0.3774(6) 0.4197(5) 0.6202(5) 0.0314(13) Uani 0.498(3) 1 d . . P A 2
H5AA H 0.393467 0.390375 0.553982 0.038 Uiso 0.498(3) 1 calc R U P A 2
H5AB H 0.455221 0.471317 0.666131 0.038 Uiso 0.498(3) 1 calc R U P A 2
C13A C -0.0154(6) 0.7343(5) 0.6453(5) 0.0316(13) Uani 0.498(3) 1 d . . P A 2
H13C H -0.097899 0.755512 0.592210 0.038 Uiso 0.498(3) 1 calc R U P A 2
H13D H 0.021211 0.792095 0.709094 0.038 Uiso 0.498(3) 1 calc R U P A 2
C11 C -0.1456(7) 0.6136(6) 0.7285(7) 0.0373(15) Uani 0.502(3) 1 d . . P A 1
H11C H -0.190208 0.645611 0.773834 0.045 Uiso 0.502(3) 1 calc R U P A 1
H11D H -0.212265 0.580068 0.655466 0.045 Uiso 0.502(3) 1 calc R U P A 1
C6A C 0.3733(6) 0.3354(5) 0.6830(7) 0.0304(14) Uani 0.498(3) 1 d . . P A 2
H6AA H 0.451489 0.348871 0.753944 0.036 Uiso 0.498(3) 1 calc R U P A 2
H6AB H 0.381982 0.269068 0.641287 0.036 Uiso 0.498(3) 1 calc R U P A 2
C14A C 0.0646(10) 0.7342(7) 0.5924(9) 0.034(2) Uani 0.498(3) 1 d . . P A 2
H14C H 0.121744 0.804844 0.618815 0.040 Uiso 0.498(3) 1 calc R U P A 2
H14D H 0.010428 0.739769 0.511649 0.040 Uiso 0.498(3) 1 calc R U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S1 2.1601(7) . ?
Ni1 S6 2.1584(7) . ?
Ni1 S2 2.1596(7) . ?
Ni1 S7 2.1691(7) . ?
S1 C15 1.708(3) . ?
S4 C16 1.744(3) . ?
S4 C17 1.737(3) . ?
S9 C19 1.748(2) . ?
S9 C20 1.729(3) . ?
S8 C18 1.739(3) . ?
S8 C20 1.735(2) . ?
S6 C18 1.721(2) . ?
S2 C16 1.713(3) . ?
S3 C17 1.725(3) . ?
S3 C15 1.741(2) . ?
S7 C19 1.720(3) . ?
S5 C17 1.649(3) . ?
S10 C20 1.650(3) . ?
Cl1 C2 1.760(3) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N1 C1 1.481(3) . ?
C19 C18 1.357(4) . ?
C16 C15 1.371(4) . ?
C1 H1D 0.9900 . ?
C1 H1E 0.9900 . ?
C1 C2 1.507(4) . ?
C7 H7BC 0.9900 . ?
C7 H7BD 0.9900 . ?
C7 H7AA 0.9900 . ?
C7 H7AB 0.9900 . ?
C7 O4A 1.447(5) . ?
C7 O3 1.386(4) . ?
C7 C7A 1.397(6) . ?
C7 C8 1.388(7) . ?
O4A C9A 1.410(7) . ?
O1A C3A 1.424(7) . ?
O1A C14A 1.325(10) . ?
O3 C6 1.427(6) . ?
O6 C13 1.424(10) . ?
O6 C12 1.423(7) . ?
O6A C12A 1.416(7) . ?
O6A C13A 1.426(7) . ?
O1 C3 1.351(5) . ?
O1 C14 1.444(7) . ?
C9 H9BC 0.9900 . ?
C9 H9BD 0.9900 . ?
C9 H9AA 0.9900 . ?
C9 H9AB 0.9900 . ?
C9 O5A 1.447(5) . ?
C9 C10 1.355(7) . ?
C9 C9A 1.369(7) . ?
C9 O4 1.424(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
O2A C3 1.357(5) . ?
O2A C5A 1.410(7) . ?
O2 C5 1.361(7) . ?
O2 C4 1.427(7) . ?
C3 H3AA 0.9900 . ?
C3 H3AB 0.9900 . ?
C3 H3BC 0.9900 . ?
C3 H3BD 0.9900 . ?
C3 C4 1.411(7) . ?
C3 C3A 1.405(7) . ?
O3A C7A 1.439(6) . ?
O3A C6A 1.375(7) . ?
O5A C11A 1.430(7) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.307(13) . ?
C11A H11A 0.9900 . ?
C11A H11B 0.9900 . ?
C11A C12A 1.505(9) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.338(8) . ?
C7A H7AC 0.9900 . ?
C7A H7AD 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C11 1.487(9) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 O5 1.425(7) . ?
C9A H9AC 0.9900 . ?
C9A H9AD 0.9900 . ?
C12A H12C 0.9900 . ?
C12A H12D 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 O4 1.425(7) . ?
O5 C11 1.436(7) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C3A H3AC 0.9900 . ?
C3A H3AD 0.9900 . ?
C5A H5AA 0.9900 . ?
C5A H5AB 0.9900 . ?
C5A C6A 1.343(9) . ?
C13A H13C 0.9900 . ?
C13A H13D 0.9900 . ?
C13A C14A 1.309(12) . ?
C11 H11C 0.9900 . ?
C11 H11D 0.9900 . ?
C6A H6AA 0.9900 . ?
C6A H6AB 0.9900 . ?
C14A H14C 0.9900 . ?
C14A H14D 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S1 Ni1 S7 176.92(3) . . ?
S6 Ni1 S1 85.97(2) . . ?
S6 Ni1 S2 178.91(3) . . ?
S6 Ni1 S7 93.25(3) . . ?
S2 Ni1 S1 93.09(3) . . ?
S2 Ni1 S7 87.72(3) . . ?
C15 S1 Ni1 102.37(9) . . ?
C17 S4 C16 97.19(13) . . ?
C20 S9 C19 97.32(12) . . ?
C20 S8 C18 97.10(12) . . ?
C18 S6 Ni1 102.16(9) . . ?
C16 S2 Ni1 102.38(9) . . ?
C17 S3 C15 97.68(13) . . ?
C19 S7 Ni1 101.71(9) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
S7 C19 S9 122.75(15) . . ?
C18 C19 S9 115.7(2) . . ?
C18 C19 S7 121.54(19) . . ?
S2 C16 S4 123.08(16) . . ?
C15 C16 S4 116.02(19) . . ?
C15 C16 S2 120.9(2) . . ?
S6 C18 S8 122.35(15) . . ?
C19 C18 S8 116.57(19) . . ?
C19 C18 S6 121.1(2) . . ?
S3 C17 S4 113.33(15) . . ?
S5 C17 S4 123.41(17) . . ?
S5 C17 S3 123.25(16) . . ?
N1 C1 H1D 109.1 . . ?
N1 C1 H1E 109.1 . . ?
N1 C1 C2 112.3(2) . . ?
H1D C1 H1E 107.9 . . ?
C2 C1 H1D 109.1 . . ?
C2 C1 H1E 109.1 . . ?
S1 C15 S3 123.06(16) . . ?
C16 C15 S1 121.19(19) . . ?
C16 C15 S3 115.7(2) . . ?
S9 C20 S8 113.28(15) . . ?
S10 C20 S9 123.61(15) . . ?
S10 C20 S8 123.11(17) . . ?
H7BC C7 H7BD 107.7 . . ?
H7AA C7 H7AB 107.2 . . ?
O4A C7 H7BC 108.8 . . ?
O4A C7 H7BD 108.8 . . ?
O3 C7 H7AA 107.9 . . ?
O3 C7 H7AB 107.9 . . ?
O3 C7 C8 117.7(4) . . ?
C7A C7 H7BC 108.8 . . ?
C7A C7 H7BD 108.8 . . ?
C7A C7 O4A 113.6(3) . . ?
C8 C7 H7AA 107.9 . . ?
C8 C7 H7AB 107.9 . . ?
C9A O4A C7 115.8(4) . . ?
C14A O1A C3A 125.8(6) . . ?
C7 O3 C6 116.8(4) . . ?
C12 O6 C13 124.2(6) . . ?
C12A O6A C13A 112.1(5) . . ?
C3 O1 C14 118.5(5) . . ?
H9BC C9 H9BD 107.4 . . ?
H9AA C9 H9AB 107.3 . . ?
O5A C9 H9BC 108.4 . . ?
O5A C9 H9BD 108.4 . . ?
C10 C9 H9AA 108.1 . . ?
C10 C9 H9AB 108.1 . . ?
C10 C9 O4 116.9(4) . . ?
C9A C9 H9BC 108.4 . . ?
C9A C9 H9BD 108.4 . . ?
C9A C9 O5A 115.6(3) . . ?
O4 C9 H9AA 108.1 . . ?
O4 C9 H9AB 108.1 . . ?
Cl1 C2 H2A 109.0 . . ?
Cl1 C2 H2B 109.0 . . ?
C1 C2 Cl1 112.9(2) . . ?
C1 C2 H2A 109.0 . . ?
C1 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
C3 O2A C5A 119.3(4) . . ?
C5 O2 C4 126.4(5) . . ?
O1 C3 H3AA 107.9 . . ?
O1 C3 H3AB 107.9 . . ?
O1 C3 C4 117.8(4) . . ?
O2A C3 H3BC 108.0 . . ?
O2A C3 H3BD 108.0 . . ?
O2A C3 C3A 117.3(4) . . ?
H3AA C3 H3AB 107.2 . . ?
H3BC C3 H3BD 107.2 . . ?
C4 C3 H3AA 107.9 . . ?
C4 C3 H3AB 107.9 . . ?
C3A C3 H3BC 108.0 . . ?
C3A C3 H3BD 108.0 . . ?
C6A O3A C7A 130.0(5) . . ?
C11A O5A C9 117.6(4) . . ?
O6 C13 H13A 107.5 . . ?
O6 C13 H13B 107.5 . . ?
H13A C13 H13B 107.0 . . ?
C14 C13 O6 119.4(8) . . ?
C14 C13 H13A 107.5 . . ?
C14 C13 H13B 107.5 . . ?
O5A C11A H11A 109.8 . . ?
O5A C11A H11B 109.8 . . ?
O5A C11A C12A 109.4(5) . . ?
H11A C11A H11B 108.2 . . ?
C12A C11A H11A 109.8 . . ?
C12A C11A H11B 109.8 . . ?
O2 C5 H5A 106.9 . . ?
O2 C5 H5B 106.9 . . ?
H5A C5 H5B 106.7 . . ?
C6 C5 O2 121.8(5) . . ?
C6 C5 H5A 106.9 . . ?
C6 C5 H5B 106.9 . . ?
C7 C7A O3A 114.3(4) . . ?
C7 C7A H7AC 108.7 . . ?
C7 C7A H7AD 108.7 . . ?
O3A C7A H7AC 108.7 . . ?
O3A C7A H7AD 108.7 . . ?
H7AC C7A H7AD 107.6 . . ?
O6 C12 H12A 110.0 . . ?
O6 C12 H12B 110.0 . . ?
O6 C12 C11 108.5(6) . . ?
H12A C12 H12B 108.4 . . ?
C11 C12 H12A 110.0 . . ?
C11 C12 H12B 110.0 . . ?
C9 C10 H10A 109.4 . . ?
C9 C10 H10B 109.4 . . ?
C9 C10 O5 111.1(5) . . ?
H10A C10 H10B 108.0 . . ?
O5 C10 H10A 109.4 . . ?
O5 C10 H10B 109.4 . . ?
O4A C9A H9AC 108.6 . . ?
O4A C9A H9AD 108.6 . . ?
C9 C9A O4A 114.7(6) . . ?
C9 C9A H9AC 108.6 . . ?
C9 C9A H9AD 108.6 . . ?
H9AC C9A H9AD 107.6 . . ?
O6A C12A C11A 107.8(5) . . ?
O6A C12A H12C 110.1 . . ?
O6A C12A H12D 110.1 . . ?
C11A C12A H12C 110.1 . . ?
C11A C12A H12D 110.1 . . ?
H12C C12A H12D 108.5 . . ?
O2 C4 H4A 109.1 . . ?
O2 C4 H4B 109.1 . . ?
C3 C4 O2 112.7(5) . . ?
C3 C4 H4A 109.1 . . ?
C3 C4 H4B 109.1 . . ?
H4A C4 H4B 107.8 . . ?
O1 C14 H14A 106.4 . . ?
O1 C14 H14B 106.4 . . ?
C13 C14 O1 123.8(7) . . ?
C13 C14 H14A 106.4 . . ?
C13 C14 H14B 106.4 . . ?
H14A C14 H14B 106.5 . . ?
C7 C8 H8A 109.4 . . ?
C7 C8 H8B 109.4 . . ?
C7 C8 O4 111.2(5) . . ?
H8A C8 H8B 108.0 . . ?
O4 C8 H8A 109.4 . . ?
O4 C8 H8B 109.4 . . ?
C10 O5 C11 111.7(5) . . ?
C9 O4 C8 118.9(5) . . ?
O3 C6 H6A 106.6 . . ?
O3 C6 H6B 106.6 . . ?
C5 C6 O3 122.7(6) . . ?
C5 C6 H6A 106.6 . . ?
C5 C6 H6B 106.6 . . ?
H6A C6 H6B 106.6 . . ?
O1A C3A H3AC 108.8 . . ?
O1A C3A H3AD 108.8 . . ?
C3 C3A O1A 114.0(5) . . ?
C3 C3A H3AC 108.8 . . ?
C3 C3A H3AD 108.8 . . ?
H3AC C3A H3AD 107.6 . . ?
O2A C5A H5AA 106.7 . . ?
O2A C5A H5AB 106.7 . . ?
H5AA C5A H5AB 106.6 . . ?
C6A C5A O2A 122.6(6) . . ?
C6A C5A H5AA 106.7 . . ?
C6A C5A H5AB 106.7 . . ?
O6A C13A H13C 107.9 . . ?
O6A C13A H13D 107.9 . . ?
H13C C13A H13D 107.2 . . ?
C14A C13A O6A 117.5(6) . . ?
C14A C13A H13C 107.9 . . ?
C14A C13A H13D 107.9 . . ?
C12 C11 H11C 109.8 . . ?
C12 C11 H11D 109.8 . . ?
O5 C11 C12 109.6(5) . . ?
O5 C11 H11C 109.8 . . ?
O5 C11 H11D 109.8 . . ?
H11C C11 H11D 108.2 . . ?
O3A C6A H6AA 107.1 . . ?
O3A C6A H6AB 107.1 . . ?
C5A C6A O3A 120.8(5) . . ?
C5A C6A H6AA 107.1 . . ?
C5A C6A H6AB 107.1 . . ?
H6AA C6A H6AB 106.8 . . ?
O1A C14A H14C 105.0 . . ?
O1A C14A H14D 105.0 . . ?
C13A C14A O1A 129.2(8) . . ?
C13A C14A H14C 105.0 . . ?
C13A C14A H14D 105.0 . . ?
H14C C14A H14D 105.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S1 C15 S3 -177.02(13) . . . . ?
Ni1 S1 C15 C16 3.0(2) . . . . ?
Ni1 S6 C18 S8 -177.39(13) . . . . ?
Ni1 S6 C18 C19 2.8(2) . . . . ?
Ni1 S2 C16 S4 179.42(13) . . . . ?
Ni1 S2 C16 C15 0.3(2) . . . . ?
Ni1 S7 C19 S9 176.97(13) . . . . ?
Ni1 S7 C19 C18 -4.0(2) . . . . ?
S4 C16 C15 S1 178.46(13) . . . . ?
S4 C16 C15 S3 -1.5(3) . . . . ?
S9 C19 C18 S8 0.1(3) . . . . ?
S9 C19 C18 S6 179.97(13) . . . . ?
S2 C16 C15 S1 -2.4(3) . . . . ?
S2 C16 C15 S3 177.64(13) . . . . ?
S7 C19 C18 S8 -178.94(13) . . . . ?
S7 C19 C18 S6 0.9(3) . . . . ?
N1 C1 C2 Cl1 70.7(3) . . . . ?
C19 S9 C20 S8 1.89(17) . . . . ?
C19 S9 C20 S10 -177.61(18) . . . . ?
C16 S4 C17 S3 -1.70(17) . . . . ?
C16 S4 C17 S5 177.63(18) . . . . ?
C18 S8 C20 S9 -1.83(17) . . . . ?
C18 S8 C20 S10 177.67(18) . . . . ?
C17 S4 C16 S2 -177.18(16) . . . . ?
C17 S4 C16 C15 1.9(2) . . . . ?
C17 S3 C15 S1 -179.70(17) . . . . ?
C17 S3 C15 C16 0.3(2) . . . . ?
C15 S3 C17 S4 1.05(17) . . . . ?
C15 S3 C17 S5 -178.28(18) . . . . ?
C20 S9 C19 S7 177.83(17) . . . . ?
C20 S9 C19 C18 -1.2(2) . . . . ?
C20 S8 C18 S6 -178.80(16) . . . . ?
C20 S8 C18 C19 1.0(2) . . . . ?
C7 O4A C9A C9 -173.2(4) . . . . ?
C7 O3 C6 C5 157.7(6) . . . . ?
C7 C8 O4 C9 175.8(4) . . . . ?
O4A C7 C7A O3A 54.2(6) . . . . ?
O3 C7 C8 O4 52.6(6) . . . . ?
O6 C13 C14 O1 -18.3(12) . . . . ?
O6 C12 C11 O5 62.9(7) . . . . ?
O6A C13A C14A O1A -13.9(13) . . . . ?
O1 C3 C4 O2 47.1(7) . . . . ?
C9 O5A C11A C12A -176.3(4) . . . . ?
C9 C10 O5 C11 178.5(5) . . . . ?
O2A C3 C3A O1A 49.0(7) . . . . ?
O2A C5A C6A O3A -3.2(11) . . . . ?
O2 C5 C6 O3 -3.2(11) . . . . ?
C3 O1 C14 C13 171.8(7) . . . . ?
C3 O2A C5A C6A 167.0(6) . . . . ?
O5A C9 C9A O4A -55.3(6) . . . . ?
O5A C11A C12A O6A 62.3(7) . . . . ?
C13 O6 C12 C11 143.1(7) . . . . ?
C5 O2 C4 C3 153.1(6) . . . . ?
C7A C7 O4A C9A -174.7(4) . . . . ?
C7A O3A C6A C5A 139.6(7) . . . . ?
C12 O6 C13 C14 155.6(7) . . . . ?
C10 C9 O4 C8 179.2(5) . . . . ?
C10 O5 C11 C12 -173.6(5) . . . . ?
C9A C9 O5A C11A 173.2(5) . . . . ?
C12A O6A C13A C14A 155.1(7) . . . . ?
C4 O2 C5 C6 153.6(7) . . . . ?
C14 O1 C3 C4 -164.7(5) . . . . ?
C8 C7 O3 C6 -176.9(5) . . . . ?
O4 C9 C10 O5 -56.7(6) . . . . ?
C3A O1A C14A C13A 157.3(8) . . . . ?
C5A O2A C3 C3A -173.3(5) . . . . ?
C13A O6A C12A C11A 167.3(5) . . . . ?
C6A O3A C7A C7 150.9(6) . . . . ?
C14A O1A C3A C3 167.4(6) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.420
_oxdiff_exptl_absorpt_empirical_full_min 0.414
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_133k-f
_database_code_depnum_ccdc_archive 'CCDC 2053393'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-18 downloaded from the CCDC.
;
_audit_creation_date             2020-11-24
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C2 H7 Cl N, C12 H24 O6'
_chemical_formula_sum            'C20 H31 Cl N Ni O6 S10'
_chemical_formula_weight         796.22
_chemical_melting_point          ?
_chemical_oxdiff_formula         C20H30NO6NiS10Cl
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.2216(3)
_cell_length_b                   12.3162(3)
_cell_length_c                   12.7541(3)
_cell_angle_alpha                92.155(2)
_cell_angle_beta                 111.864(2)
_cell_angle_gamma                96.100(2)
_cell_volume                     1620.96(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    27165
_cell_measurement_temperature    133
_cell_measurement_theta_max      31.2380
_cell_measurement_theta_min      2.0800
_shelx_estimated_absorpt_T_max   0.792
_shelx_estimated_absorpt_T_min   0.454
_exptl_absorpt_coefficient_mu    1.361
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38683
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             822
_exptl_crystal_size_max          0.69
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0897
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            35045
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.972
_diffrn_ambient_temperature      133
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      1.00  27.00   0.50    0.33    --    5.18  51.00 -79.00   52
  2  ω     31.00  78.00   0.50    0.33    --    5.18  51.00 -79.00   94
  3  ω    -47.00  19.00   0.50    0.33    --    5.18 -33.00-163.59  132
  4  ω    -65.00  19.00   0.50    0.33    --    5.18 -33.00 -40.51  168
  5  ω    -66.00  19.00   0.50    0.33    --    5.18 -28.00 -93.66  170
  6  ω    -48.00  18.00   0.50    0.33    --    5.18 -31.00  -1.90  132
  7  ω    -65.00  19.00   0.50    0.33    --    5.18 -33.00  62.15  168
  8  ω    -67.00  19.00   0.50    0.33    --    5.18 -51.00 134.00  172
  9  ω    -63.00  18.00   0.50    0.33    --    5.18 -37.00 150.00  162
 10  ω    -16.00  29.00   0.50    0.33    --   -4.95 -99.00 -30.00   90
 11  ω    -18.00  29.00   0.50    0.33    --   -4.95 -99.00  30.00   94
 12  ω    -77.00 -17.00   0.50    0.33    --   -4.95 -51.00 134.00  120
 13  ω     38.00  68.00   0.50    0.33    --   -4.95  51.00 -79.00   60
 14  ω    -11.00  25.00   0.50    0.33    --   -4.95  51.00 -79.00   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0546308000
_diffrn_orient_matrix_UB_12      -0.0320699000
_diffrn_orient_matrix_UB_13      0.0033679000
_diffrn_orient_matrix_UB_21      -0.0223232000
_diffrn_orient_matrix_UB_22      -0.0164773000
_diffrn_orient_matrix_UB_23      -0.0587354000
_diffrn_orient_matrix_UB_31      0.0351435000
_diffrn_orient_matrix_UB_32      -0.0455878000
_diffrn_orient_matrix_UB_33      0.0124486000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5723
_reflns_number_total             6623
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT n/a (Sheldrick, 2015)'
_refine_diff_density_max         0.836
_refine_diff_density_min         -0.772
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         6623
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0419
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0845P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1168
_refine_ls_wR_factor_ref         0.1216
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
2. Rigid body (RIGU) restrains
 Cl1A, C2A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Others
 Sof(Cl1A)=Sof(H1BC)=Sof(H1BD)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(Cl1)=FVAR(1)
 Sof(H3BC)=Sof(H3BD)=Sof(O5A)=Sof(O4A)=Sof(C10A)=Sof(H10C)=Sof(H10D)=Sof(C9A)=
 Sof(H9AA)=Sof(H9AB)=Sof(H11C)=Sof(H11D)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(O3A)=
 Sof(C12A)=Sof(H12C)=Sof(H12D)=Sof(C13A)=Sof(H13C)=Sof(H13D)=Sof(C6A)=Sof(H6AA)=
 Sof(H6AB)=Sof(O6A)=Sof(O2A)=Sof(C14A)=Sof(H14C)=Sof(H14D)=Sof(C4A)=Sof(H4AA)=
 Sof(H4AB)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(O1A)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=1-
 FVAR(2)
 Sof(O4)=Sof(O1)=Sof(O3)=Sof(O6)=Sof(H3AA)=Sof(H3AB)=Sof(O5)=Sof(O2)=Sof(C9)=
 Sof(H9A)=Sof(H9B)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C13)=Sof(H13A)=Sof(H13B)=
 Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C7)=Sof(H7A)=
 Sof(H7B)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C8)=
 Sof(H8A)=Sof(H8B)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H11A)=Sof(H11B)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1BC,H1BD), C1(H1AA,H1AB), C3(H3AA,H3AB), C3(H3BC,H3BD), C9(H9A,H9B),
 C5(H5A,H5B), C13(H13A,H13B), C14(H14A,H14B), C4(H4A,H4B), C7(H7A,H7B), C2(H2A,
 H2B), C12(H12A,H12B), C6(H6A,H6B), C2A(H2AA,H2AB), C8(H8A,H8B), C10(H10A,H10B),
  C10A(H10C,H10D), C9A(H9AA,H9AB), C11(H11A,H11B), C11(H11C,H11D), C8A(H8AA,
 H8AB), C12A(H12C,H12D), C13A(H13C,H13D), C6A(H6AA,H6AB), C14A(H14C,H14D),
 C4A(H4AA,H4AB), C5A(H5AA,H5AB), C7A(H7AA,H7AB)
4.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.84539(2) 0.89079(2) 0.51197(2) 0.02358(11) Uani 1 1 d . . . . .
S6 S 0.69194(6) 0.97833(5) 0.52226(5) 0.03142(15) Uani 1 1 d . . . . .
S2 S 1.00572(5) 0.81081(4) 0.50736(5) 0.02867(15) Uani 1 1 d . . . . .
S1 S 0.79499(6) 0.93685(4) 0.34068(5) 0.02932(15) Uani 1 1 d . . . . .
S7 S 0.89704(5) 0.84168(4) 0.68224(5) 0.02791(14) Uani 1 1 d . . . . .
S8 S 0.61350(6) 1.02830(4) 0.72137(5) 0.03100(15) Uani 1 1 d . . . . .
S9 S 0.80093(6) 0.90082(4) 0.86706(5) 0.02917(15) Uani 1 1 d . . . . .
S4 S 1.10045(6) 0.77033(5) 0.31745(5) 0.03405(16) Uani 1 1 d . . . . .
S3 S 0.91215(6) 0.89324(5) 0.16595(5) 0.03066(15) Uani 1 1 d . . . . .
S10 S 0.62516(6) 1.00328(5) 0.95605(6) 0.03726(16) Uani 1 1 d . . . . .
S5 S 1.09219(6) 0.78863(6) 0.08352(6) 0.04024(17) Uani 1 1 d . . . . .
Cl1A Cl 0.8110(12) 0.4663(9) 0.5145(8) 0.054(3) Uani 0.158(6) 1 d . . P A 2
N1 N 0.66809(17) 0.50260(13) 0.25490(16) 0.0257(4) Uani 1 1 d . . . . .
H1A H 0.664456 0.517690 0.184552 0.031 Uiso 1 1 calc R U . . .
H1B H 0.588847 0.504925 0.258356 0.031 Uiso 1 1 calc R U . . .
H1C H 0.691848 0.434606 0.269136 0.031 Uiso 1 1 calc R U . . .
C18 C 0.7087(2) 0.96685(16) 0.66081(19) 0.0253(4) Uani 1 1 d . . . . .
C19 C 0.7964(2) 0.90726(16) 0.72988(19) 0.0241(4) Uani 1 1 d . . . . .
C15 C 0.9067(2) 0.88206(16) 0.30002(19) 0.0261(4) Uani 1 1 d . . . . .
C17 C 1.0380(2) 0.81627(18) 0.1840(2) 0.0309(5) Uani 1 1 d . . . . .
C20 C 0.6780(2) 0.97945(17) 0.8538(2) 0.0285(5) Uani 1 1 d . . . . .
C16 C 0.9971(2) 0.82588(16) 0.3722(2) 0.0265(5) Uani 1 1 d . . . . .
O4 O 0.7149(3) 0.6170(3) 0.0826(3) 0.0303(8) Uani 0.500(3) 1 d . . P B 1
O1 O 0.5010(4) 0.3201(3) 0.3068(4) 0.0357(8) Uani 0.500(3) 1 d . . P B 1
O3 O 0.4984(3) 0.6543(3) 0.1363(3) 0.0334(8) Uani 0.500(3) 1 d . . P B 1
O6 O 0.7204(3) 0.2811(2) 0.2654(3) 0.0292(8) Uani 0.500(3) 1 d . . P B 1
C1 C 0.7646(2) 0.58515(18) 0.3408(2) 0.0344(5) Uani 1 1 d . . . . .
H1BC H 0.795946 0.643449 0.302452 0.041 Uiso 0.158(6) 1 calc R U P A 2
H1BD H 0.723674 0.619337 0.388115 0.041 Uiso 0.158(6) 1 calc R U P A 2
H1AA H 0.742569 0.659410 0.321120 0.041 Uiso 0.842(6) 1 calc R U P A 1
H1AB H 0.851309 0.579948 0.339130 0.041 Uiso 0.842(6) 1 calc R U P A 1
C3 C 0.6461(3) 0.2028(2) 0.2994(3) 0.0519(8) Uani 1 1 d . . . . .
H3AA H 0.582864 0.159445 0.230494 0.062 Uiso 0.500(3) 1 calc R U P B 1
H3AB H 0.704195 0.152139 0.344587 0.062 Uiso 0.500(3) 1 calc R U P B 1
H3BC H 0.715982 0.214292 0.375697 0.062 Uiso 0.500(3) 1 calc R U P B 2
H3BD H 0.596946 0.129555 0.293120 0.062 Uiso 0.500(3) 1 calc R U P B 2
O5 O 0.7957(4) 0.4112(3) 0.1172(3) 0.0323(8) Uani 0.500(3) 1 d . . P B 1
O2 O 0.4277(4) 0.5311(3) 0.2889(3) 0.0354(8) Uani 0.500(3) 1 d . . P B 1
C9 C 0.5638(8) 0.7340(6) 0.0920(7) 0.0361(17) Uani 0.500(3) 1 d . . P B 1
H9A H 0.635140 0.778368 0.154942 0.043 Uiso 0.500(3) 1 calc R U P B 1
H9B H 0.502858 0.783718 0.048707 0.043 Uiso 0.500(3) 1 calc R U P B 1
C5 C 0.4351(11) 0.3611(14) 0.3668(14) 0.035(3) Uani 0.500(3) 1 d . . P B 1
H5A H 0.497648 0.399478 0.439037 0.042 Uiso 0.500(3) 1 calc R U P B 1
H5B H 0.383346 0.299994 0.385042 0.042 Uiso 0.500(3) 1 calc R U P B 1
C13 C 0.8211(7) 0.3047(5) 0.1295(6) 0.0372(13) Uani 0.500(3) 1 d . . P B 1
H13A H 0.784260 0.266042 0.052648 0.045 Uiso 0.500(3) 1 calc R U P B 1
H13B H 0.916272 0.306650 0.155996 0.045 Uiso 0.500(3) 1 calc R U P B 1
C14 C 0.7829(5) 0.2418(5) 0.1955(4) 0.0338(11) Uani 0.500(3) 1 d . . P B 1
H14A H 0.860381 0.211740 0.246272 0.041 Uiso 0.500(3) 1 calc R U P B 1
H14B H 0.723737 0.179031 0.145937 0.041 Uiso 0.500(3) 1 calc R U P B 1
C4 C 0.5785(5) 0.2397(4) 0.3621(5) 0.0402(12) Uani 0.500(3) 1 d . . P B 1
H4A H 0.640475 0.271373 0.437674 0.048 Uiso 0.500(3) 1 calc R U P B 1
H4B H 0.522480 0.177184 0.373162 0.048 Uiso 0.500(3) 1 calc R U P B 1
C7 C 0.3542(6) 0.6127(5) 0.2292(6) 0.0423(13) Uani 0.500(3) 1 d . . P B 1
H7A H 0.310292 0.644930 0.275026 0.051 Uiso 0.500(3) 1 calc R U P B 1
H7B H 0.287142 0.579078 0.156720 0.051 Uiso 0.500(3) 1 calc R U P B 1
C2 C 0.7695(3) 0.5694(2) 0.4592(2) 0.0377(8) Uani 0.842(6) 1 d . . P A 1
H2A H 0.680357 0.562283 0.458292 0.045 Uiso 0.842(6) 1 calc R U P A 1
H2B H 0.819400 0.634937 0.510123 0.045 Uiso 0.842(6) 1 calc R U P A 1
C12 C 0.8683(5) 0.4976(4) 0.0874(5) 0.0383(12) Uani 0.500(3) 1 d . . P B 1
H12A H 0.940643 0.531427 0.156652 0.046 Uiso 0.500(3) 1 calc R U P B 1
H12B H 0.906018 0.466840 0.035696 0.046 Uiso 0.500(3) 1 calc R U P B 1
C6 C 0.3470(5) 0.4393(4) 0.3012(5) 0.0383(12) Uani 0.500(3) 1 d . . P B 1
H6A H 0.288547 0.404029 0.225914 0.046 Uiso 0.500(3) 1 calc R U P B 1
H6B H 0.293614 0.462664 0.342553 0.046 Uiso 0.500(3) 1 calc R U P B 1
C2A C 0.864(2) 0.5369(19) 0.406(2) 0.071(7) Uani 0.158(6) 1 d . . P A 2
H2AA H 0.940501 0.592122 0.444711 0.086 Uiso 0.158(6) 1 calc R U P A 2
H2AB H 0.886554 0.482716 0.359786 0.086 Uiso 0.158(6) 1 calc R U P A 2
C8 C 0.4428(5) 0.7009(5) 0.2063(5) 0.0385(13) Uani 0.500(3) 1 d . . P B 1
H8A H 0.393146 0.759801 0.168535 0.046 Uiso 0.500(3) 1 calc R U P B 1
H8B H 0.511465 0.733304 0.278555 0.046 Uiso 0.500(3) 1 calc R U P B 1
C10 C 0.6162(6) 0.6789(4) 0.0173(6) 0.0379(12) Uani 0.500(3) 1 d . . P B 1
H10A H 0.545886 0.629666 -0.041869 0.045 Uiso 0.500(3) 1 calc R U P B 1
H10B H 0.652728 0.734208 -0.020703 0.045 Uiso 0.500(3) 1 calc R U P B 1
O5A O 0.7745(3) 0.4821(3) 0.0779(3) 0.0301(8) Uani 0.500(3) 1 d . . P B 2
O4A O 0.6439(4) 0.6609(3) 0.0909(3) 0.0323(8) Uani 0.500(3) 1 d . . P B 2
C10A C 0.6939(6) 0.6430(4) 0.0052(5) 0.0386(12) Uani 0.500(3) 1 d . . P B 2
H10C H 0.622438 0.607722 -0.063911 0.046 Uiso 0.500(3) 1 calc R U P B 2
H10D H 0.725506 0.714948 -0.013514 0.046 Uiso 0.500(3) 1 calc R U P B 2
C9A C 0.5259(8) 0.7106(6) 0.0483(7) 0.0363(17) Uani 0.500(3) 1 d . . P B 2
H9AA H 0.457509 0.660310 -0.011266 0.044 Uiso 0.500(3) 1 calc R U P B 2
H9AB H 0.540879 0.779377 0.014695 0.044 Uiso 0.500(3) 1 calc R U P B 2
C11 C 0.7938(4) 0.5785(2) 0.0346(3) 0.0664(10) Uani 1 1 d . . . . .
H11A H 0.853626 0.641669 0.030039 0.080 Uiso 0.500(3) 1 calc R U P B 1
H11B H 0.739335 0.549336 -0.044101 0.080 Uiso 0.500(3) 1 calc R U P B 1
H11C H 0.812741 0.562213 -0.033760 0.080 Uiso 0.500(3) 1 calc R U P B 2
H11D H 0.872061 0.622518 0.090924 0.080 Uiso 0.500(3) 1 calc R U P B 2
C8A C 0.4841(5) 0.7344(4) 0.1442(5) 0.0363(11) Uani 0.500(3) 1 d . . P B 2
H8AA H 0.553650 0.783202 0.204424 0.044 Uiso 0.500(3) 1 calc R U P B 2
H8AB H 0.406001 0.772427 0.117064 0.044 Uiso 0.500(3) 1 calc R U P B 2
O3A O 0.4560(3) 0.6345(3) 0.1891(3) 0.0317(8) Uani 0.500(3) 1 d . . P B 2
C12A C 0.8777(6) 0.4181(4) 0.1204(5) 0.0379(12) Uani 0.500(3) 1 d . . P B 2
H12C H 0.893462 0.388452 0.054191 0.045 Uiso 0.500(3) 1 calc R U P B 2
H12D H 0.955818 0.469402 0.166090 0.045 Uiso 0.500(3) 1 calc R U P B 2
C13A C 0.8727(6) 0.3354(5) 0.1822(6) 0.0350(13) Uani 0.500(3) 1 d . . P B 2
H13C H 0.951116 0.348670 0.252797 0.042 Uiso 0.500(3) 1 calc R U P B 2
H13D H 0.881102 0.269022 0.140523 0.042 Uiso 0.500(3) 1 calc R U P B 2
C6A C 0.3593(6) 0.5453(4) 0.3037(5) 0.0374(12) Uani 0.500(3) 1 d . . P B 2
H6AA H 0.326659 0.556233 0.365049 0.045 Uiso 0.500(3) 1 calc R U P B 2
H6AB H 0.285670 0.512669 0.234726 0.045 Uiso 0.500(3) 1 calc R U P B 2
O6A O 0.7685(3) 0.3089(3) 0.2141(3) 0.0314(8) Uani 0.500(3) 1 d . . P B 2
O2A O 0.4564(3) 0.4731(3) 0.3364(3) 0.0339(8) Uani 0.500(3) 1 d . . P B 2
C14A C 0.7015(5) 0.2041(4) 0.2186(4) 0.0335(11) Uani 0.500(3) 1 d . . P B 2
H14C H 0.632579 0.181622 0.143233 0.040 Uiso 0.500(3) 1 calc R U P B 2
H14D H 0.763180 0.149379 0.234851 0.040 Uiso 0.500(3) 1 calc R U P B 2
C4A C 0.5097(5) 0.2927(4) 0.3752(6) 0.0371(12) Uani 0.500(3) 1 d . . P B 2
H4AA H 0.579710 0.325053 0.446711 0.045 Uiso 0.500(3) 1 calc R U P B 2
H4AB H 0.477839 0.218272 0.388043 0.045 Uiso 0.500(3) 1 calc R U P B 2
C5A C 0.3985(13) 0.3634(12) 0.3433(15) 0.040(3) Uani 0.500(3) 1 d . . P B 2
H5AA H 0.329822 0.334980 0.269546 0.048 Uiso 0.500(3) 1 calc R U P B 2
H5AB H 0.360267 0.363927 0.401841 0.048 Uiso 0.500(3) 1 calc R U P B 2
O1A O 0.5600(4) 0.2852(3) 0.2886(3) 0.0320(8) Uani 0.500(3) 1 d . . P B 2
C7A C 0.4161(7) 0.6537(4) 0.2808(5) 0.0384(13) Uani 0.500(3) 1 d . . P B 2
H7AA H 0.350621 0.705264 0.261027 0.046 Uiso 0.500(3) 1 calc R U P B 2
H7AB H 0.491109 0.686036 0.348949 0.046 Uiso 0.500(3) 1 calc R U P B 2
Cl1 Cl 0.8421(2) 0.45110(15) 0.51337(19) 0.0580(6) Uani 0.842(6) 1 d . . P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S6 2.1673(6) . ?
Ni1 S2 2.1591(6) . ?
Ni1 S1 2.1576(6) . ?
Ni1 S7 2.1572(6) . ?
S6 C18 1.719(2) . ?
S2 C16 1.708(2) . ?
S1 C15 1.713(2) . ?
S7 C19 1.722(2) . ?
S8 C18 1.747(2) . ?
S8 C20 1.731(2) . ?
S9 C19 1.736(2) . ?
S9 C20 1.730(2) . ?
S4 C17 1.725(2) . ?
S4 C16 1.743(2) . ?
S3 C15 1.744(2) . ?
S3 C17 1.733(2) . ?
S10 C20 1.650(2) . ?
S5 C17 1.650(2) . ?
Cl1A C2A 1.90(2) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N1 C1 1.485(3) . ?
C18 C19 1.356(3) . ?
C15 C16 1.362(3) . ?
O4 C10 1.430(7) . ?
O4 C11 1.361(4) . ?
O1 C5 1.363(16) . ?
O1 C4 1.418(6) . ?
O3 C9 1.421(9) . ?
O3 C8 1.404(6) . ?
O6 C3 1.394(4) . ?
O6 C14 1.422(6) . ?
C1 H1BC 0.9900 . ?
C1 H1BD 0.9900 . ?
C1 H1AA 0.9900 . ?
C1 H1AB 0.9900 . ?
C1 C2 1.511(4) . ?
C1 C2A 1.33(3) . ?
C3 H3AA 0.9900 . ?
C3 H3AB 0.9900 . ?
C3 H3BC 0.9900 . ?
C3 H3BD 0.9900 . ?
C3 C4 1.386(6) . ?
C3 C14A 1.387(6) . ?
C3 O1A 1.450(5) . ?
O5 C13 1.374(6) . ?
O5 C12 1.420(6) . ?
O2 C7 1.426(7) . ?
O2 C6 1.423(6) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.472(11) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.501(16) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.319(8) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.505(8) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 Cl1 1.782(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C11 1.398(6) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C2A H2AA 0.9900 . ?
C2A H2AB 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
O5A C11 1.360(4) . ?
O5A C12A 1.420(6) . ?
O4A C10A 1.422(6) . ?
O4A C9A 1.444(10) . ?
C10A H10C 0.9900 . ?
C10A H10D 0.9900 . ?
C10A C11 1.388(7) . ?
C9A H9AA 0.9900 . ?
C9A H9AB 0.9900 . ?
C9A C8A 1.493(10) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 H11C 0.9900 . ?
C11 H11D 0.9900 . ?
C8A H8AA 0.9900 . ?
C8A H8AB 0.9900 . ?
C8A O3A 1.431(5) . ?
O3A C7A 1.420(6) . ?
C12A H12C 0.9900 . ?
C12A H12D 0.9900 . ?
C12A C13A 1.321(8) . ?
C13A H13C 0.9900 . ?
C13A H13D 0.9900 . ?
C13A O6A 1.387(6) . ?
C6A H6AA 0.9900 . ?
C6A H6AB 0.9900 . ?
C6A O2A 1.432(6) . ?
C6A C7A 1.504(7) . ?
O6A C14A 1.437(5) . ?
O2A C5A 1.456(16) . ?
C14A H14C 0.9900 . ?
C14A H14D 0.9900 . ?
C4A H4AA 0.9900 . ?
C4A H4AB 0.9900 . ?
C4A C5A 1.537(15) . ?
C4A O1A 1.419(7) . ?
C5A H5AA 0.9900 . ?
C5A H5AB 0.9900 . ?
C7A H7AA 0.9900 . ?
C7A H7AB 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S2 Ni1 S6 176.91(2) . . ?
S1 Ni1 S6 87.79(2) . . ?
S1 Ni1 S2 93.00(2) . . ?
S7 Ni1 S6 93.23(2) . . ?
S7 Ni1 S2 86.01(2) . . ?
S7 Ni1 S1 178.82(2) . . ?
C18 S6 Ni1 101.78(8) . . ?
C16 S2 Ni1 102.33(8) . . ?
C15 S1 Ni1 102.36(8) . . ?
C19 S7 Ni1 102.19(8) . . ?
C20 S8 C18 97.28(10) . . ?
C20 S9 C19 97.23(11) . . ?
C17 S4 C16 97.48(11) . . ?
C17 S3 C15 97.18(11) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
S6 C18 S8 122.83(13) . . ?
C19 C18 S6 121.54(16) . . ?
C19 C18 S8 115.62(17) . . ?
S7 C19 S9 122.37(13) . . ?
C18 C19 S7 121.01(17) . . ?
C18 C19 S9 116.62(16) . . ?
S1 C15 S3 122.97(14) . . ?
C16 C15 S1 120.97(17) . . ?
C16 C15 S3 116.05(16) . . ?
S4 C17 S3 113.35(13) . . ?
S5 C17 S4 123.17(14) . . ?
S5 C17 S3 123.48(15) . . ?
S9 C20 S8 113.23(12) . . ?
S10 C20 S8 123.33(13) . . ?
S10 C20 S9 123.43(14) . . ?
S2 C16 S4 122.83(14) . . ?
C15 C16 S2 121.28(16) . . ?
C15 C16 S4 115.89(17) . . ?
C11 O4 C10 118.7(4) . . ?
C5 O1 C4 113.4(8) . . ?
C8 O3 C9 112.9(5) . . ?
C3 O6 C14 116.7(3) . . ?
N1 C1 H1BC 109.7 . . ?
N1 C1 H1BD 109.7 . . ?
N1 C1 H1AA 109.1 . . ?
N1 C1 H1AB 109.1 . . ?
N1 C1 C2 112.33(18) . . ?
H1BC C1 H1BD 108.2 . . ?
H1AA C1 H1AB 107.9 . . ?
C2 C1 H1AA 109.1 . . ?
C2 C1 H1AB 109.1 . . ?
C2A C1 N1 109.7(10) . . ?
C2A C1 H1BC 109.7 . . ?
C2A C1 H1BD 109.7 . . ?
O6 C3 H3AA 107.9 . . ?
O6 C3 H3AB 107.9 . . ?
H3AA C3 H3AB 107.2 . . ?
H3BC C3 H3BD 107.7 . . ?
C4 C3 O6 117.6(3) . . ?
C4 C3 H3AA 107.9 . . ?
C4 C3 H3AB 107.9 . . ?
C14A C3 H3BC 108.8 . . ?
C14A C3 H3BD 108.8 . . ?
C14A C3 O1A 113.7(3) . . ?
O1A C3 H3BC 108.8 . . ?
O1A C3 H3BD 108.8 . . ?
C13 O5 C12 127.0(4) . . ?
C6 O2 C7 111.9(4) . . ?
O3 C9 H9A 109.8 . . ?
O3 C9 H9B 109.8 . . ?
O3 C9 C10 109.6(5) . . ?
H9A C9 H9B 108.2 . . ?
C10 C9 H9A 109.8 . . ?
C10 C9 H9B 109.8 . . ?
O1 C5 H5A 109.3 . . ?
O1 C5 H5B 109.3 . . ?
O1 C5 C6 111.4(11) . . ?
H5A C5 H5B 108.0 . . ?
C6 C5 H5A 109.3 . . ?
C6 C5 H5B 109.3 . . ?
O5 C13 H13A 106.7 . . ?
O5 C13 H13B 106.7 . . ?
H13A C13 H13B 106.6 . . ?
C14 C13 O5 122.4(5) . . ?
C14 C13 H13A 106.7 . . ?
C14 C13 H13B 106.7 . . ?
O6 C14 H14A 106.7 . . ?
O6 C14 H14B 106.7 . . ?
C13 C14 O6 122.7(5) . . ?
C13 C14 H14A 106.7 . . ?
C13 C14 H14B 106.7 . . ?
H14A C14 H14B 106.6 . . ?
O1 C4 H4A 109.4 . . ?
O1 C4 H4B 109.4 . . ?
C3 C4 O1 111.2(5) . . ?
C3 C4 H4A 109.4 . . ?
C3 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
O2 C7 H7A 109.8 . . ?
O2 C7 H7B 109.8 . . ?
O2 C7 C8 109.6(5) . . ?
H7A C7 H7B 108.2 . . ?
C8 C7 H7A 109.8 . . ?
C8 C7 H7B 109.8 . . ?
C1 C2 H2A 109.2 . . ?
C1 C2 H2B 109.2 . . ?
C1 C2 Cl1 112.0(2) . . ?
H2A C2 H2B 107.9 . . ?
Cl1 C2 H2A 109.2 . . ?
Cl1 C2 H2B 109.2 . . ?
O5 C12 H12A 109.0 . . ?
O5 C12 H12B 109.0 . . ?
H12A C12 H12B 107.8 . . ?
C11 C12 O5 112.9(4) . . ?
C11 C12 H12A 109.0 . . ?
C11 C12 H12B 109.0 . . ?
O2 C6 C5 106.8(6) . . ?
O2 C6 H6A 110.4 . . ?
O2 C6 H6B 110.4 . . ?
C5 C6 H6A 110.4 . . ?
C5 C6 H6B 110.4 . . ?
H6A C6 H6B 108.6 . . ?
Cl1A C2A H2AA 110.3 . . ?
Cl1A C2A H2AB 110.3 . . ?
C1 C2A Cl1A 107.1(14) . . ?
C1 C2A H2AA 110.3 . . ?
C1 C2A H2AB 110.3 . . ?
H2AA C2A H2AB 108.6 . . ?
O3 C8 C7 108.6(5) . . ?
O3 C8 H8A 110.0 . . ?
O3 C8 H8B 110.0 . . ?
C7 C8 H8A 110.0 . . ?
C7 C8 H8B 110.0 . . ?
H8A C8 H8B 108.3 . . ?
O4 C10 C9 109.6(6) . . ?
O4 C10 H10A 109.7 . . ?
O4 C10 H10B 109.7 . . ?
C9 C10 H10A 109.7 . . ?
C9 C10 H10B 109.7 . . ?
H10A C10 H10B 108.2 . . ?
C11 O5A C12A 119.7(4) . . ?
C10A O4A C9A 111.6(6) . . ?
O4A C10A H10C 108.7 . . ?
O4A C10A H10D 108.7 . . ?
H10C C10A H10D 107.6 . . ?
C11 C10A O4A 114.4(5) . . ?
C11 C10A H10C 108.7 . . ?
C11 C10A H10D 108.7 . . ?
O4A C9A H9AA 109.9 . . ?
O4A C9A H9AB 109.9 . . ?
O4A C9A C8A 108.8(6) . . ?
H9AA C9A H9AB 108.3 . . ?
C8A C9A H9AA 109.9 . . ?
C8A C9A H9AB 109.9 . . ?
O4 C11 C12 118.0(3) . . ?
O4 C11 H11A 107.8 . . ?
O4 C11 H11B 107.8 . . ?
C12 C11 H11A 107.8 . . ?
C12 C11 H11B 107.8 . . ?
O5A C11 C10A 117.2(3) . . ?
O5A C11 H11C 108.0 . . ?
O5A C11 H11D 108.0 . . ?
C10A C11 H11C 108.0 . . ?
C10A C11 H11D 108.0 . . ?
H11A C11 H11B 107.1 . . ?
H11C C11 H11D 107.2 . . ?
C9A C8A H8AA 109.7 . . ?
C9A C8A H8AB 109.7 . . ?
H8AA C8A H8AB 108.2 . . ?
O3A C8A C9A 110.0(5) . . ?
O3A C8A H8AA 109.7 . . ?
O3A C8A H8AB 109.7 . . ?
C7A O3A C8A 111.7(4) . . ?
O5A C12A H12C 106.8 . . ?
O5A C12A H12D 106.8 . . ?
H12C C12A H12D 106.6 . . ?
C13A C12A O5A 122.2(5) . . ?
C13A C12A H12C 106.8 . . ?
C13A C12A H12D 106.8 . . ?
C12A C13A H13C 106.9 . . ?
C12A C13A H13D 106.9 . . ?
C12A C13A O6A 121.9(5) . . ?
H13C C13A H13D 106.7 . . ?
O6A C13A H13C 106.9 . . ?
O6A C13A H13D 106.9 . . ?
H6AA C6A H6AB 108.2 . . ?
O2A C6A H6AA 109.8 . . ?
O2A C6A H6AB 109.8 . . ?
O2A C6A C7A 109.6(5) . . ?
C7A C6A H6AA 109.8 . . ?
C7A C6A H6AB 109.8 . . ?
C13A O6A C14A 130.6(4) . . ?
C6A O2A C5A 110.1(6) . . ?
C3 C14A O6A 114.1(4) . . ?
C3 C14A H14C 108.7 . . ?
C3 C14A H14D 108.7 . . ?
O6A C14A H14C 108.7 . . ?
O6A C14A H14D 108.7 . . ?
H14C C14A H14D 107.6 . . ?
H4AA C4A H4AB 108.0 . . ?
C5A C4A H4AA 109.4 . . ?
C5A C4A H4AB 109.4 . . ?
O1A C4A H4AA 109.4 . . ?
O1A C4A H4AB 109.4 . . ?
O1A C4A C5A 111.3(9) . . ?
O2A C5A C4A 105.6(9) . . ?
O2A C5A H5AA 110.6 . . ?
O2A C5A H5AB 110.6 . . ?
C4A C5A H5AA 110.6 . . ?
C4A C5A H5AB 110.6 . . ?
H5AA C5A H5AB 108.8 . . ?
C4A O1A C3 115.5(4) . . ?
O3A C7A C6A 107.6(4) . . ?
O3A C7A H7AA 110.2 . . ?
O3A C7A H7AB 110.2 . . ?
C6A C7A H7AA 110.2 . . ?
C6A C7A H7AB 110.2 . . ?
H7AA C7A H7AB 108.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S6 C18 S8 177.07(11) . . . . ?
Ni1 S6 C18 C19 -4.0(2) . . . . ?
Ni1 S2 C16 S4 -176.91(11) . . . . ?
Ni1 S2 C16 C15 2.5(2) . . . . ?
Ni1 S1 C15 S3 179.61(11) . . . . ?
Ni1 S1 C15 C16 0.0(2) . . . . ?
Ni1 S7 C19 S9 -177.41(11) . . . . ?
Ni1 S7 C19 C18 2.7(2) . . . . ?
S6 C18 C19 S7 0.9(3) . . . . ?
S6 C18 C19 S9 -178.92(11) . . . . ?
S1 C15 C16 S2 -1.8(3) . . . . ?
S1 C15 C16 S4 177.63(11) . . . . ?
S8 C18 C19 S7 179.92(11) . . . . ?
S8 C18 C19 S9 0.1(2) . . . . ?
S3 C15 C16 S2 178.59(11) . . . . ?
S3 C15 C16 S4 -2.0(2) . . . . ?
N1 C1 C2 Cl1 71.6(3) . . . . ?
N1 C1 C2A Cl1A -79.6(12) . . . . ?
C18 S8 C20 S9 1.47(14) . . . . ?
C18 S8 C20 S10 -177.26(15) . . . . ?
C19 S9 C20 S8 -1.44(14) . . . . ?
C19 S9 C20 S10 177.29(15) . . . . ?
C15 S3 C17 S4 -1.87(14) . . . . ?
C15 S3 C17 S5 177.66(15) . . . . ?
C17 S4 C16 S2 179.99(14) . . . . ?
C17 S4 C16 C15 0.56(19) . . . . ?
C17 S3 C15 S1 -177.27(14) . . . . ?
C17 S3 C15 C16 2.34(19) . . . . ?
C20 S8 C18 S6 178.03(14) . . . . ?
C20 S8 C18 C19 -0.93(19) . . . . ?
C20 S9 C19 S7 -179.01(14) . . . . ?
C20 S9 C19 C18 0.85(19) . . . . ?
C16 S4 C17 S3 1.03(14) . . . . ?
C16 S4 C17 S5 -178.50(15) . . . . ?
O1 C5 C6 O2 -65.6(10) . . . . ?
O3 C9 C10 O4 -66.0(6) . . . . ?
O6 C3 C4 O1 52.8(5) . . . . ?
C3 O6 C14 C13 158.3(5) . . . . ?
O5 C13 C14 O6 -4.6(10) . . . . ?
O5 C12 C11 O4 47.0(6) . . . . ?
O2 C7 C8 O3 62.6(6) . . . . ?
C9 O3 C8 C7 168.6(5) . . . . ?
C5 O1 C4 C3 -178.4(7) . . . . ?
C13 O5 C12 C11 153.8(5) . . . . ?
C14 O6 C3 C4 -176.4(4) . . . . ?
C4 O1 C5 C6 -175.7(6) . . . . ?
C7 O2 C6 C5 -178.9(8) . . . . ?
C12 O5 C13 C14 153.9(6) . . . . ?
C6 O2 C7 C8 -173.2(5) . . . . ?
C8 O3 C9 C10 -178.5(5) . . . . ?
C10 O4 C11 C12 -165.1(4) . . . . ?
O5A C12A C13A O6A -3.2(9) . . . . ?
O4A C10A C11 O5A 49.7(6) . . . . ?
O4A C9A C8A O3A -62.5(6) . . . . ?
C10A O4A C9A C8A -176.0(4) . . . . ?
C9A O4A C10A C11 -169.3(5) . . . . ?
C9A C8A O3A C7A 179.8(5) . . . . ?
C11 O4 C10 C9 -166.6(4) . . . . ?
C11 O5A C12A C13A 167.0(5) . . . . ?
C8A O3A C7A C6A 166.8(5) . . . . ?
C12A O5A C11 C10A -173.5(4) . . . . ?
C12A C13A O6A C14A 139.0(6) . . . . ?
C13A O6A C14A C3 151.6(5) . . . . ?
C6A O2A C5A C4A 178.3(8) . . . . ?
O2A C6A C7A O3A 62.1(6) . . . . ?
C14A C3 O1A C4A -175.0(4) . . . . ?
C5A C4A O1A C3 -167.7(6) . . . . ?
O1A C3 C14A O6A 54.6(5) . . . . ?
O1A C4A C5A O2A -64.2(11) . . . . ?
C7A C6A O2A C5A -172.0(8) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.972
_oxdiff_exptl_absorpt_empirical_full_min 0.401
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_213k-f
_database_code_depnum_ccdc_archive 'CCDC 2053397'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-18 downloaded from the CCDC.
;
_audit_creation_date             2020-11-24
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C2 H7 Cl N, 1(C12 H24 O6)'
_chemical_formula_sum            'C20 H31 Cl N Ni O6 S10'
_chemical_formula_weight         796.22
_chemical_melting_point          ?
_chemical_oxdiff_formula         C20H31NO6NiS10Cl
_chemical_oxdiff_usercomment     '213K friedel mates as non-equivalent'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.2637(2)
_cell_length_b                   12.34200(10)
_cell_length_c                   12.8337(2)
_cell_angle_alpha                91.3720(10)
_cell_angle_beta                 110.9960(10)
_cell_angle_gamma                96.4500(10)
_cell_volume                     1651.13(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    28392
_cell_measurement_temperature    213
_cell_measurement_theta_max      72.4910
_cell_measurement_theta_min      3.6050
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    7.815
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             822
_exptl_crystal_size_max          0.291
_exptl_crystal_size_mid          0.249
_exptl_crystal_size_min          0.153
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            42270
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.738
_diffrn_reflns_theta_min         3.613
_diffrn_ambient_temperature      213
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -1.00  71.00   0.50    0.50    --  -18.00  53.00  60.93  144
  2  ω   -104.00 -17.00   0.50    0.50    --  -18.00  53.00  60.93  174
  3  ω    -82.00 -56.00   0.50    0.50    --  -30.00  53.00 174.93   52
  4  ω     25.00  58.00   0.50    0.50    --  -30.00  53.00 174.93   66
  5  ω    -88.00 -63.00   0.50    0.50    --  -38.00  55.00 -52.83   50
  6  ω     22.00  50.00   0.50    0.50    --  -38.00  55.00 -52.83   56
  7  ω   -134.00 -88.00   0.50    0.50    --  -46.00  55.00 -90.71   92
  8  ω    -84.00   4.00   0.50    0.50    --  -46.00  55.00 -90.71  176
  9  ω     12.00  43.00   0.50    0.50    --  -46.00  55.00 -90.71   62
 10  ω     13.00  43.00   0.50    0.50    --  -46.00  55.00  38.00   60
 11  ω      9.00  39.00   0.50    0.50    --  -50.00  54.00  77.48   60
 12  ω      7.00  35.00   0.50    0.50    --  -54.00  55.00 146.66   56
 13  ω     -3.00  35.00   0.50    0.50    --  -54.00  55.00-174.84   76
 14  ω      2.00  31.00   0.50    0.50    --  -58.00  55.00  22.77   58
 15  ω     -6.00  26.00   0.50    0.50    --  -62.00  55.00-110.54   64
 16  ω    -11.00  27.00   0.50    0.50    --  -62.00  55.00   0.36   76
 17  ω      2.00  27.00   0.50    0.50    --  -62.00  55.00 -58.51   50
 18  ω     -2.00  27.00   0.50    0.50    --  -62.00  55.00 137.86   58
 19  ω   -138.00-112.00   0.50    0.50    --  -62.00  55.00   0.36   52
 20  ω      0.00  26.00   0.50    0.50    --  -62.00  55.00 -27.78   52
 21  ω    -64.00 -23.00   0.50    0.50    --  -62.00  55.00   0.36   82
 22  ω     -7.00  19.00   0.50    0.50    --  -70.00  54.00  91.98   52
 23  ω    -22.00  19.00   0.50    0.50    --  -70.00  55.00-153.98   82
 24  ω    -32.00  19.00   0.50    0.50    --  -70.00  55.00 116.69  102
 25  ω    -14.00  18.00   0.50    0.50    --  -70.00  55.00  75.10   64
 26  ω    -13.00  15.00   0.50    0.50    --  -74.00  52.00  38.56   56
 27  ω   -160.00-135.00   0.50    0.50    --  -74.00  52.00  38.56   50
 28  ω    -20.00  14.00   0.50    0.50    --  -74.00  55.00 -29.52   68
 29  ω    -17.00  10.00   0.50    0.50    --  -78.00  55.00 140.76   54
 30  ω    -76.00 -50.00   0.50    0.50    --  -78.00  55.00 140.76   52
 31  ω    -27.00  11.00   0.50    0.50    --  -78.00  54.00 -70.29   76
 32  ω    -32.00   6.00   0.50    0.50    --  -82.00  55.00  96.85   76
 33  ω    -23.00   5.00   0.50    0.50    --  -82.00  55.00-125.27   56
 34  ω    -24.00   7.00   0.50    0.50    --  -82.00  55.00-173.94   62
 35  ω    -20.00   7.00   0.50    0.50    --  -82.00  51.00-159.78   54
 36  ω   -129.00-103.00   0.50    0.50    --  -82.00  51.00-159.78   52
 37  ω    -24.00   7.00   0.50    0.50    --  -82.00  55.00-112.98   62
 38  ω    -43.00   3.00   0.50    0.50    --  -86.00  55.00 -36.76   92
 39  ω   -154.00-128.00   0.50    0.50    --  -86.00  55.00 -36.76   52
 40  ω   -178.00  -2.00   0.50    0.50    --  -90.00  54.00 134.64  352
 41  ω    -29.00  -1.00   0.50    0.50    --  -90.00  55.00  43.18   56
 42  ω    -29.00  -4.00   0.50    0.50    --  -90.00  52.00-158.22   50
 43  ω    -76.00 -50.00   0.50    0.50    --  -90.00  52.00-158.22   52
 44  ω    -99.00  -3.00   0.50    0.50    --  -90.00  50.00 163.25  192
 45  ω   -135.00-109.00   0.50    0.50    --  -90.00  50.00 163.25   52
 46  ω    -33.00  -1.00   0.50    0.50    --  -90.00  54.00  23.56   64
 47  ω    -92.00 -66.00   0.50    0.50    --  -90.00  54.00  23.56   52
 48  ω   -156.00-131.00   0.50    0.50    --  -90.00  54.00  23.56   50
 49  ω   -180.00-139.00   0.50    0.50    --  -94.70  55.00 -78.67   82
 50  ω   -166.00  -6.00   0.50    0.50    --  -94.70  55.00-176.23  320
 51  ω    -70.00 -32.00   0.50    0.50    --  -94.70   0.00 -60.00   76
 52  ω   -126.00-100.00   0.50    0.50    --  -94.70   0.00 -60.00   52
 53  ω   -123.00  -6.00   0.50    0.50    --  -94.70  55.00  62.17  234
 54  ω   -183.00-141.00   0.50    0.50    --  -94.70  55.00  62.17   84
 55  ω   -153.00  -5.00   0.50    0.50    --  -94.70  52.00 -98.91  296
 56  ω    -61.00  -5.00   0.50    0.50    --  -94.70  55.00 -62.11  112
 57  ω   -177.00  -5.00   0.50    0.50    --  -94.70  53.00  82.44  344
 58  ω   -132.00 -78.00   0.50    0.50    --  -94.70  55.00 -62.11  108
 59  ω   -183.00  -7.00   0.50    0.50    --  -94.70  55.00  -8.81  352
 60  ω   -113.00  -8.00   0.50    0.50    --  -94.70  55.00-123.56  210
 61  ω   -169.00-143.00   0.50    0.50    --  -94.70  55.00-123.56   52
 62  ω   -112.00  -5.00   0.50    0.50    --  -94.70  55.00 125.23  214
 63  ω   -175.00-149.00   0.50    0.50    --  -94.70  55.00 125.23   52
 64  ω   -123.00  -7.00   0.50    0.50    --  -94.70  54.00  11.95  232
 65  ω    -98.00  -5.00   0.50    0.50    --  -94.70  55.00 -78.67  186
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0737264000
_diffrn_orient_matrix_UB_12      -0.0641685000
_diffrn_orient_matrix_UB_13      -0.0556791000
_diffrn_orient_matrix_UB_21      0.1118378000
_diffrn_orient_matrix_UB_22      0.0035014000
_diffrn_orient_matrix_UB_23      0.1132271000
_diffrn_orient_matrix_UB_31      -0.0623292000
_diffrn_orient_matrix_UB_32      -0.1082864000
_diffrn_orient_matrix_UB_33      0.0262855000
_diffrn_oxdiff_digest_frames     
;
013a4eda4640e4bdb21471fcaf4e14a3520670477a2
;
_diffrn_oxdiff_digest_hkl        
;
0148df7b613291ed60056540b4060fcc91d988
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5870
_reflns_number_total             6349
_reflns_odcompleteness_completeness 98.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.111
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         6349
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0310
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0505P)²+0.3777P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0815
_refine_ls_wR_factor_ref         0.0831
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
2. Others
 Sof(H20C)=Sof(H20D)=Sof(C19A)=Sof(H19C)=Sof(H19D)=Sof(Cl)=1-FVAR(1)
 Sof(Cl18)=Sof(H20A)=Sof(H20B)=Sof(C19)=Sof(H19A)=Sof(H19B)=FVAR(1)
 Sof(O1A)=Sof(O23A)=Sof(C22A)=Sof(H22C)=Sof(H22D)=Sof(C27A)=Sof(H27C)=
 Sof(H27D)=Sof(C24A)=Sof(H24C)=Sof(H24D)=Sof(C26A)=Sof(H26C)=Sof(H26D)=Sof(C8A)=
 Sof(H8AA)=Sof(H8AB)=Sof(O6A)=Sof(C32A)=Sof(H32C)=Sof(H32D)=Sof(C40A)=Sof(H40C)=
 Sof(H40D)=Sof(O28A)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(C31A)=Sof(H31C)=Sof(H31D)=
 Sof(O2A)=Sof(C30A)=Sof(H30C)=Sof(H30D)=Sof(C37A)=Sof(H37C)=Sof(H37D)=Sof(O3A)=
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=1-FVAR(2)
 Sof(O23)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(C22)=
 Sof(H22A)=Sof(H22B)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(O28)=Sof(C27)=Sof(H27A)=
 Sof(H27B)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(C31)=
 Sof(H31A)=Sof(H31B)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(O1)=Sof(O2)=Sof(O3)=
 Sof(O6)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C1)=Sof(H1A)=
 Sof(H1B)=FVAR(2)
3.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C20(H20C,H20D), C30(H30A,H30B), C32(H32A,H32B), C22(H22A,
 H22B), C37(H37A,H37B), C19(H19A,H19B), C27(H27A,H27B), C40(H40A,H40B),
 C24(H24A,H24B), C31(H31A,H31B), C26(H26A,H26B), C19A(H19C,H19D), C8(H8A,H8B),
 C4(H4A,H4B), C1(H1A,H1B), C22A(H22C,H22D), C27A(H27C,H27D), C24A(H24C,H24D),
 C26A(H26C,H26D), C8A(H8AA,H8AB), C32A(H32C,H32D), C40A(H40C,H40D), C4A(H4AA,
 H4AB), C31A(H31C,H31D), C30A(H30C,H30D), C37A(H37C,H37D), C1A(H1AA,H1AB)
3.b Idealised Me refined as rotating group:
 N21(H21A,H21B,H21C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.34530(2) 0.88988(2) 0.51227(2) 0.03758(9) Uani 1 1 d . . . . .
S6 S 0.11408(4) 1.02636(4) 0.72102(3) 0.04582(11) Uani 1 1 d . . . . .
S9 S 0.39844(4) 0.84359(4) 0.68262(3) 0.04695(11) Uani 1 1 d . . . . .
S7 S 0.19206(4) 0.97605(4) 0.52299(3) 0.04662(11) Uani 1 1 d . . . . .
S16 S 0.50579(4) 0.81186(4) 0.50739(3) 0.04632(11) Uani 1 1 d . . . . .
S15 S 0.29161(4) 0.93103(4) 0.34016(3) 0.04697(11) Uani 1 1 d . . . . .
S4 S 0.30176(4) 0.90197(4) 0.86615(3) 0.04904(12) Uani 1 1 d . . . . .
S13 S 0.59956(4) 0.77107(4) 0.31781(4) 0.05129(12) Uani 1 1 d . . . . .
S11 S 0.40899(5) 0.88813(4) 0.16617(3) 0.05067(12) Uani 1 1 d . . . . .
S8 S 0.12630(5) 1.00315(4) 0.95482(4) 0.05719(13) Uani 1 1 d . . . . .
S17 S 0.59019(5) 0.78658(5) 0.08458(4) 0.06295(14) Uani 1 1 d . . . . .
Cl18 Cl 0.6600(3) 0.54690(19) 0.4855(2) 0.0808(6) Uani 0.709(5) 1 d . . P A 1
N21 N 0.83440(14) 0.49778(11) 0.74474(11) 0.0443(3) Uani 1 1 d . . . . .
H21A H 0.811616 0.564282 0.731144 0.053 Uiso 1 1 calc GR . . . .
H21B H 0.910297 0.495188 0.738627 0.053 Uiso 1 1 calc GR . . . .
H21C H 0.839657 0.482912 0.813660 0.053 Uiso 1 1 calc GR . . . .
C3 C 0.29727(15) 0.90746(13) 0.72960(13) 0.0395(3) Uani 1 1 d . . . . .
C2 C 0.20869(15) 0.96556(13) 0.66072(13) 0.0387(3) Uani 1 1 d . . . . .
C12 C 0.53582(17) 0.81396(15) 0.18428(14) 0.0478(4) Uani 1 1 d . . . . .
C10 C 0.40407(16) 0.87836(13) 0.29987(13) 0.0413(3) Uani 1 1 d . . . . .
C5 C 0.17824(16) 0.97878(14) 0.85276(14) 0.0441(4) Uani 1 1 d . . . . .
C14 C 0.49551(15) 0.82496(13) 0.37201(13) 0.0410(3) Uani 1 1 d . . . . .
O23 O 0.8531(4) 0.3434(3) 0.9108(3) 0.0572(9) Uani 0.462(3) 1 d . . P B 1
C20 C 0.7369(2) 0.41589(16) 0.66259(16) 0.0605(5) Uani 1 1 d . . . . .
H20A H 0.653200 0.423496 0.665080 0.073 Uiso 0.709(5) 1 calc R . P A 1
H20B H 0.756144 0.343088 0.683734 0.073 Uiso 0.709(5) 1 calc R . P A 1
H20C H 0.776542 0.377997 0.619159 0.073 Uiso 0.291(5) 1 calc R . P A 2
H20D H 0.702195 0.362320 0.701716 0.073 Uiso 0.291(5) 1 calc R . P A 2
C30 C 0.8508(16) 0.7862(10) 0.6811(11) 0.059(3) Uani 0.462(3) 1 d . . P B 1
H30A H 0.780584 0.760259 0.612052 0.070 Uiso 0.462(3) 1 calc R . P B 1
H30B H 0.889616 0.857200 0.670182 0.070 Uiso 0.462(3) 1 calc R . P B 1
C32 C 0.6790(6) 0.7003(5) 0.8647(5) 0.0616(14) Uani 0.462(3) 1 d . . P B 1
H32A H 0.612456 0.747797 0.842682 0.074 Uiso 0.462(3) 1 calc R . P B 1
H32B H 0.743762 0.730356 0.935352 0.074 Uiso 0.462(3) 1 calc R . P B 1
C22 C 0.6853(9) 0.4209(9) 0.9471(7) 0.068(2) Uani 0.462(3) 1 d . . P B 1
H22A H 0.623535 0.379292 0.881130 0.082 Uiso 0.462(3) 1 calc R . P B 1
H22B H 0.645006 0.428438 1.001760 0.082 Uiso 0.462(3) 1 calc R . P B 1
C37 C 1.0992(15) 0.6310(13) 0.6574(12) 0.075(4) Uani 0.462(3) 1 d . . P B 1
H37A H 1.139988 0.630756 0.602470 0.090 Uiso 0.462(3) 1 calc R . P B 1
H37B H 1.163842 0.658462 0.729094 0.090 Uiso 0.462(3) 1 calc R . P B 1
C19 C 0.7325(4) 0.4281(2) 0.5454(2) 0.0671(10) Uani 0.709(5) 1 d . . P A 1
H19A H 0.684059 0.363119 0.499038 0.080 Uiso 0.709(5) 1 calc R . P A 1
H19B H 0.819080 0.433886 0.545361 0.080 Uiso 0.709(5) 1 calc R . P A 1
O28 O 0.7349(4) 0.6947(3) 0.7820(3) 0.0554(9) Uani 0.462(3) 1 d . . P B 1
C27 C 0.9675(10) 0.2943(7) 0.9532(7) 0.070(2) Uani 0.462(3) 1 d . . P B 1
H27A H 0.952074 0.228084 0.988132 0.084 Uiso 0.462(3) 1 calc R . P B 1
H27B H 1.033570 0.344000 1.009277 0.084 Uiso 0.462(3) 1 calc R . P B 1
C40 C 1.1490(6) 0.3927(6) 0.7665(7) 0.0723(18) Uani 0.462(3) 1 d . . P B 1
H40A H 1.227536 0.416137 0.829744 0.087 Uiso 0.462(3) 1 calc R . P B 1
H40B H 1.160489 0.324178 0.735084 0.087 Uiso 0.462(3) 1 calc R . P B 1
C24 C 0.8036(7) 0.3623(5) 0.9956(5) 0.0714(16) Uani 0.462(3) 1 d . . P B 1
H24A H 0.868007 0.406870 1.057843 0.086 Uiso 0.462(3) 1 calc R . P B 1
H24B H 0.780789 0.293381 1.022722 0.086 Uiso 0.462(3) 1 calc R . P B 1
C31 C 0.7999(5) 0.7972(4) 0.7749(4) 0.0646(14) Uani 0.462(3) 1 d . . P B 1
H31A H 0.870128 0.819281 0.845086 0.078 Uiso 0.462(3) 1 calc R . P B 1
H31B H 0.741722 0.852085 0.759485 0.078 Uiso 0.462(3) 1 calc R . P B 1
C26 C 1.0110(6) 0.2677(5) 0.8597(5) 0.0684(14) Uani 0.462(3) 1 d . . P B 1
H26A H 1.085626 0.229293 0.887064 0.082 Uiso 0.462(3) 1 calc R . P B 1
H26B H 0.943455 0.220724 0.801901 0.082 Uiso 0.462(3) 1 calc R . P B 1
C19A C 0.6373(6) 0.4692(6) 0.5907(6) 0.061(2) Uani 0.291(5) 1 d . . P A 2
H19C H 0.617657 0.526285 0.632814 0.074 Uiso 0.291(5) 1 calc R . P A 2
H19D H 0.560522 0.417340 0.556329 0.074 Uiso 0.291(5) 1 calc R . P A 2
Cl Cl 0.6888(7) 0.5266(6) 0.4860(4) 0.0854(17) Uani 0.291(5) 1 d . . P A 2
O1 O 0.7246(4) 0.5239(4) 0.9191(3) 0.0574(9) Uani 0.462(3) 1 d . . P B 1
O2 O 1.0471(4) 0.5257(4) 0.6650(3) 0.0616(9) Uani 0.462(3) 1 d . . P B 1
O3 O 0.9404(4) 0.7143(3) 0.7062(3) 0.0564(9) Uani 0.462(3) 1 d . . P B 1
O6 O 1.0420(4) 0.3660(3) 0.8149(3) 0.0554(9) Uani 0.462(3) 1 d . . P B 1
C8 C 0.6232(6) 0.5884(5) 0.8778(5) 0.0711(16) Uani 0.462(3) 1 d . . P B 1
H8A H 0.578535 0.591883 0.929618 0.085 Uiso 0.462(3) 1 calc R . P B 1
H8B H 0.562295 0.556283 0.806215 0.085 Uiso 0.462(3) 1 calc R . P B 1
C4 C 1.1432(7) 0.4543(6) 0.7017(5) 0.0744(17) Uani 0.462(3) 1 d . . P B 1
H4A H 1.139663 0.413282 0.635009 0.089 Uiso 0.462(3) 1 calc R . P B 1
H4B H 1.224848 0.500917 0.728536 0.089 Uiso 0.462(3) 1 calc R . P B 1
C1 C 0.9938(6) 0.7049(5) 0.6233(6) 0.0694(16) Uani 0.462(3) 1 d . . P B 1
H1A H 1.029013 0.776735 0.611064 0.083 Uiso 0.462(3) 1 calc R . P B 1
H1B H 0.927112 0.674963 0.553545 0.083 Uiso 0.462(3) 1 calc R . P B 1
O1A O 0.7089(3) 0.5847(3) 0.8832(3) 0.0567(7) Uani 0.538(3) 1 d . . P B 2
O23A O 0.7936(3) 0.3804(2) 0.9203(3) 0.0558(7) Uani 0.538(3) 1 d . . P B 2
C22A C 0.6387(6) 0.4973(5) 0.9152(4) 0.0695(12) Uani 0.538(3) 1 d . . P B 2
H22C H 0.577641 0.454965 0.849382 0.083 Uiso 0.538(3) 1 calc R . P B 2
H22D H 0.591906 0.525613 0.957973 0.083 Uiso 0.538(3) 1 calc R . P B 2
C27A C 0.8933(6) 0.3207(4) 0.9833(5) 0.0688(12) Uani 0.538(3) 1 d . . P B 2
H27C H 0.860029 0.266337 1.022632 0.083 Uiso 0.538(3) 1 calc R . P B 2
H27D H 0.961069 0.369957 1.038393 0.083 Uiso 0.538(3) 1 calc R . P B 2
C24A C 0.7346(8) 0.4256(7) 0.9862(6) 0.0649(18) Uani 0.538(3) 1 d . . P B 2
H24C H 0.798436 0.469076 1.049620 0.078 Uiso 0.538(3) 1 calc R . P B 2
H24D H 0.690716 0.367954 1.014250 0.078 Uiso 0.538(3) 1 calc R . P B 2
C26A C 0.9457(8) 0.2663(5) 0.9087(6) 0.0664(18) Uani 0.538(3) 1 d . . P B 2
H26C H 1.006999 0.219365 0.950796 0.080 Uiso 0.538(3) 1 calc R . P B 2
H26D H 0.877060 0.221378 0.849791 0.080 Uiso 0.538(3) 1 calc R . P B 2
C8A C 0.6323(5) 0.6623(5) 0.8237(5) 0.0579(12) Uani 0.538(3) 1 d . . P B 2
H8AA H 0.583764 0.688487 0.865944 0.069 Uiso 0.538(3) 1 calc R . P B 2
H8AB H 0.572244 0.629032 0.752264 0.069 Uiso 0.538(3) 1 calc R . P B 2
O6A O 1.0072(3) 0.3479(3) 0.8611(3) 0.0594(8) Uani 0.538(3) 1 d . . P B 2
C32A C 0.7180(4) 0.7546(4) 0.8058(4) 0.0565(11) Uani 0.538(3) 1 d . . P B 2
H32C H 0.668397 0.812555 0.772196 0.068 Uiso 0.538(3) 1 calc R . P B 2
H32D H 0.782299 0.783735 0.876993 0.068 Uiso 0.538(3) 1 calc R . P B 2
C40A C 1.0610(5) 0.3022(4) 0.7893(5) 0.0737(14) Uani 0.538(3) 1 d . . P B 2
H40C H 1.137592 0.273777 0.836839 0.088 Uiso 0.538(3) 1 calc R . P B 2
H40D H 1.000988 0.239574 0.748158 0.088 Uiso 0.538(3) 1 calc R . P B 2
O28A O 0.7787(2) 0.7175(2) 0.7344(2) 0.0492(7) Uani 0.538(3) 1 d . . P B 2
C4A C 1.0881(9) 0.3488(7) 0.7274(6) 0.0847(18) Uani 0.538(3) 1 d . . P B 2
H4AA H 1.042792 0.307952 0.655908 0.102 Uiso 0.538(3) 1 calc R . P B 2
H4AB H 1.178412 0.343651 0.744973 0.102 Uiso 0.538(3) 1 calc R . P B 2
C31A C 0.8578(14) 0.8049(10) 0.7121(10) 0.064(3) Uani 0.538(3) 1 d . . P B 2
H31C H 0.925559 0.835061 0.781001 0.077 Uiso 0.538(3) 1 calc R . P B 2
H31D H 0.807373 0.862471 0.678843 0.077 Uiso 0.538(3) 1 calc R . P B 2
O2A O 1.0715(4) 0.4706(3) 0.7056(3) 0.0650(8) Uani 0.538(3) 1 d . . P B 2
C30A C 0.9144(5) 0.7602(3) 0.6325(4) 0.0641(11) Uani 0.538(3) 1 d . . P B 2
H30C H 0.846381 0.727326 0.564865 0.077 Uiso 0.538(3) 1 calc R . P B 2
H30D H 0.964970 0.818787 0.611972 0.077 Uiso 0.538(3) 1 calc R . P B 2
C37A C 1.1493(5) 0.5646(5) 0.6913(4) 0.0737(13) Uani 0.538(3) 1 d . . P B 2
H37C H 1.202891 0.542773 0.651949 0.088 Uiso 0.538(3) 1 calc R . P B 2
H37D H 1.204800 0.598742 0.763925 0.088 Uiso 0.538(3) 1 calc R . P B 2
O3A O 0.9939(3) 0.6797(3) 0.6864(3) 0.0571(7) Uani 0.538(3) 1 d . . P B 2
C1A C 1.0640(12) 0.6456(11) 0.6250(9) 0.064(2) Uani 0.538(3) 1 d . . P B 2
H1AA H 1.116228 0.707891 0.611769 0.077 Uiso 0.538(3) 1 calc R . P B 2
H1AB H 1.006578 0.611179 0.553217 0.077 Uiso 0.538(3) 1 calc R . P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S9 2.1594(5) . ?
Ni1 S7 2.1691(5) . ?
Ni1 S16 2.1606(5) . ?
Ni1 S15 2.1606(5) . ?
S6 C2 1.7438(16) . ?
S6 C5 1.7300(17) . ?
S9 C3 1.7189(16) . ?
S7 C2 1.7191(16) . ?
S16 C14 1.7122(16) . ?
S15 C10 1.7126(17) . ?
S4 C3 1.7382(16) . ?
S4 C5 1.7311(17) . ?
S13 C12 1.7262(19) . ?
S13 C14 1.7426(16) . ?
S11 C12 1.7317(19) . ?
S11 C10 1.7431(16) . ?
S8 C5 1.6486(16) . ?
S17 C12 1.6473(17) . ?
Cl18 C19 1.812(4) . ?
N21 C20 1.486(2) . ?
C3 C2 1.360(2) . ?
C10 C14 1.360(2) . ?
O23 C27 1.418(11) . ?
O23 C24 1.414(7) . ?
C20 C19 1.498(3) . ?
C20 C19A 1.413(7) . ?
C30 C31 1.517(15) . ?
C30 O3 1.376(16) . ?
C32 O28 1.418(7) . ?
C32 C8 1.491(9) . ?
C22 C24 1.527(12) . ?
C22 O1 1.397(12) . ?
C37 O2 1.386(16) . ?
C37 C1 1.524(15) . ?
O28 C31 1.410(7) . ?
C27 C26 1.492(11) . ?
C40 O6 1.551(8) . ?
C40 C4 1.129(9) . ?
C26 O6 1.416(7) . ?
C19A Cl 1.776(9) . ?
O1 C8 1.418(8) . ?
O2 C4 1.427(9) . ?
O3 C1 1.406(7) . ?
O1A C22A 1.422(7) . ?
O1A C8A 1.412(6) . ?
O23A C27A 1.421(6) . ?
O23A C24A 1.390(10) . ?
C22A C24A 1.526(10) . ?
C27A C26A 1.476(10) . ?
C26A O6A 1.430(9) . ?
C8A C32A 1.486(7) . ?
O6A C40A 1.409(7) . ?
C32A O28A 1.419(5) . ?
C40A C4A 1.100(8) . ?
O28A C31A 1.422(14) . ?
C4A O2A 1.556(8) . ?
C31A C30A 1.508(13) . ?
O2A C37A 1.429(7) . ?
C30A O3A 1.433(6) . ?
C37A C1A 1.523(11) . ?
O3A C1A 1.388(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S9 Ni1 S7 93.102(17) . . ?
S9 Ni1 S16 86.034(17) . . ?
S9 Ni1 S15 178.26(2) . . ?
S16 Ni1 S7 176.68(2) . . ?
S15 Ni1 S7 87.930(17) . . ?
S15 Ni1 S16 93.014(17) . . ?
C5 S6 C2 97.47(8) . . ?
C3 S9 Ni1 102.29(5) . . ?
C2 S7 Ni1 101.98(6) . . ?
C14 S16 Ni1 102.19(6) . . ?
C10 S15 Ni1 102.36(6) . . ?
C5 S4 C3 97.35(8) . . ?
C12 S13 C14 97.59(8) . . ?
C12 S11 C10 97.46(8) . . ?
S9 C3 S4 122.49(9) . . ?
C2 C3 S9 121.17(12) . . ?
C2 C3 S4 116.33(12) . . ?
S7 C2 S6 123.02(9) . . ?
C3 C2 S6 115.71(12) . . ?
C3 C2 S7 121.27(12) . . ?
S13 C12 S11 113.06(9) . . ?
S17 C12 S13 123.26(11) . . ?
S17 C12 S11 123.68(11) . . ?
S15 C10 S11 123.09(10) . . ?
C14 C10 S15 121.01(13) . . ?
C14 C10 S11 115.90(12) . . ?
S6 C5 S4 113.10(9) . . ?
S8 C5 S6 123.49(10) . . ?
S8 C5 S4 123.42(10) . . ?
S16 C14 S13 122.68(10) . . ?
C10 C14 S16 121.39(13) . . ?
C10 C14 S13 115.93(12) . . ?
C24 O23 C27 111.1(6) . . ?
N21 C20 C19 112.67(18) . . ?
C19A C20 N21 109.5(3) . . ?
O3 C30 C31 110.4(9) . . ?
O28 C32 C8 109.3(5) . . ?
O1 C22 C24 108.0(6) . . ?
O2 C37 C1 109.7(11) . . ?
C20 C19 Cl18 112.6(2) . . ?
C31 O28 C32 111.0(5) . . ?
O23 C27 C26 109.4(6) . . ?
C4 C40 O6 122.9(6) . . ?
O23 C24 C22 108.8(6) . . ?
O28 C31 C30 108.0(6) . . ?
O6 C26 C27 109.1(5) . . ?
C20 C19A Cl 108.3(5) . . ?
C22 O1 C8 113.2(6) . . ?
C37 O2 C4 111.8(7) . . ?
C30 O3 C1 112.3(7) . . ?
C26 O6 C40 127.9(5) . . ?
O1 C8 C32 108.2(6) . . ?
C40 C4 O2 125.0(6) . . ?
O3 C1 C37 111.0(8) . . ?
C8A O1A C22A 113.5(5) . . ?
C24A O23A C27A 112.1(5) . . ?
O1A C22A C24A 107.7(5) . . ?
O23A C27A C26A 110.3(5) . . ?
O23A C24A C22A 108.7(5) . . ?
O6A C26A C27A 108.9(5) . . ?
O1A C8A C32A 108.3(4) . . ?
C40A O6A C26A 112.3(5) . . ?
O28A C32A C8A 109.6(4) . . ?
C4A C40A O6A 123.1(6) . . ?
C32A O28A C31A 111.0(6) . . ?
C40A C4A O2A 125.8(5) . . ?
O28A C31A C30A 107.9(8) . . ?
C37A O2A C4A 135.9(5) . . ?
O3A C30A C31A 108.7(7) . . ?
O2A C37A C1A 109.7(7) . . ?
C1A O3A C30A 112.3(6) . . ?
O3A C1A C37A 108.3(9) . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.788
_oxdiff_exptl_absorpt_empirical_full_min 0.798
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_233k-f
_database_code_depnum_ccdc_archive 'CCDC 2053398'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-18 downloaded from the CCDC.
;
_audit_creation_date             2020-11-24
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C2 H7 Cl N, 1(C12 H24 O6)'
_chemical_formula_sum            'C20 H31 Cl N Ni O6 S10'
_chemical_formula_weight         796.22
_chemical_melting_point          ?
_chemical_oxdiff_formula         C20H31NO6NiS10Cl
_chemical_oxdiff_usercomment     '233K friedel mates as non-equivalent'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.27140(10)
_cell_length_b                   12.34060(10)
_cell_length_c                   12.84520(10)
_cell_angle_alpha                91.2410(10)
_cell_angle_beta                 110.8230(10)
_cell_angle_gamma                96.4520(10)
_cell_volume                     1655.78(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    27269
_cell_measurement_temperature    233
_cell_measurement_theta_max      72.6800
_cell_measurement_theta_min      3.7000
_shelx_estimated_absorpt_T_max   0.382
_shelx_estimated_absorpt_T_min   0.210
_exptl_absorpt_coefficient_mu    7.793
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54371
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             822
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.291
_exptl_crystal_size_mid          0.249
_exptl_crystal_size_min          0.153
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            41408
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.085
_diffrn_reflns_theta_min         3.612
_diffrn_ambient_temperature      233
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -104.00 -41.00   0.50    0.50    --  -16.00  54.00  46.88  126
  2  ω      5.00  71.00   0.50    0.50    --  -16.00  54.00  46.88  132
  3  ω     16.00  49.00   0.50    0.50    --  -40.00  55.00 -70.41   66
  4  ω    -79.00 -53.00   0.50    0.50    --  -40.00  55.00 -70.41   52
  5  ω    -62.00 -37.00   0.50    0.50    --  -44.00  55.00-173.06   50
  6  ω   -132.00-107.00   0.50    0.50    --  -44.00  55.00-173.06   50
  7  ω    -11.00  45.00   0.50    0.50    --  -44.00  55.00-173.06  112
  8  ω     15.00  41.00   0.50    0.50    --  -48.00  55.00 -84.90   52
  9  ω      5.00  37.00   0.50    0.50    --  -52.00  55.00  54.78   64
 10  ω    -57.00 -25.00   0.50    0.50    --  -56.00  55.00 111.80   64
 11  ω     -3.00  32.00   0.50    0.50    --  -56.00  55.00 111.80   70
 12  ω      3.00  29.00   0.50    0.50    --  -60.00  55.00-108.67   52
 13  ω     -4.00  28.00   0.50    0.50    --  -60.00  55.00  44.85   64
 14  ω      4.00  29.00   0.50    0.50    --  -60.00  55.00 155.44   50
 15  ω    -78.00 -26.00   0.50    0.50    --  -60.00  55.00   9.77  104
 16  ω      4.00  29.00   0.50    0.50    --  -60.00  55.00   9.77   50
 17  ω   -122.00  -6.00   0.50    0.50    --  -60.00  55.00-108.67  232
 18  ω    -10.00  28.00   0.50    0.50    --  -60.00  55.00  -1.93   76
 19  ω      0.00  25.00   0.50    0.50    --  -64.00  55.00-143.92   50
 20  ω     -6.00  20.00   0.50    0.50    --  -68.00  53.00 -64.05   52
 21  ω     -4.00  21.00   0.50    0.50    --  -68.00  55.00  14.55   50
 22  ω     -5.00  21.00   0.50    0.50    --  -68.00  55.00 -23.49   52
 23  ω     -4.00  21.00   0.50    0.50    --  -68.00  55.00 141.58   50
 24  ω    -12.00  17.00   0.50    0.50    --  -72.00  55.00 -34.87   58
 25  ω    -13.00  16.00   0.50    0.50    --  -72.00  55.00 -86.14   58
 26  ω    -18.00  13.00   0.50    0.50    --  -76.00  55.00-142.61   62
 27  ω    -82.00   9.00   0.50    0.50    --  -80.00  55.00 133.67  182
 28  ω    -18.00   8.00   0.50    0.50    --  -80.00  54.00  87.07   52
 29  ω    -31.00   5.00   0.50    0.50    --  -84.00  55.00 -93.15   72
 30  ω   -109.00 -37.00   0.50    0.50    --  -84.00  55.00 -93.15  144
 31  ω    -39.00   4.00   0.50    0.50    --  -84.00  54.00-116.85   86
 32  ω   -142.00-117.00   0.50    0.50    --  -84.00  55.00 -93.15   50
 33  ω    -68.00 -42.00   0.50    0.50    --  -84.00  54.00-116.85   52
 34  ω   -173.00   4.00   0.50    0.50    --  -84.00  55.00  68.10  354
 35  ω    -33.00   5.00   0.50    0.50    --  -84.00  55.00 164.80   76
 36  ω   -129.00 -42.00   0.50    0.50    --  -84.00  55.00 164.80  174
 37  ω    -27.00   5.00   0.50    0.50    --  -84.00  55.00 109.95   64
 38  ω    -22.00   4.00   0.50    0.50    --  -84.00  54.00  20.74   52
 39  ω   -116.00 -42.00   0.50    0.50    --  -84.00  55.00 109.95  148
 40  ω    -24.00   1.00   0.50    0.50    --  -88.00  55.00 -39.08   50
 41  ω   -163.00 -39.00   0.50    0.50    --  -88.00  55.00 -39.08  248
 42  ω   -102.00  -3.00   0.50    0.50    --  -92.00  55.00  -2.09  198
 43  ω   -161.00-135.00   0.50    0.50    --  -92.00  55.00  -2.09   52
 44  ω   -121.00  -3.00   0.50    0.50    --  -92.00  53.00-160.89  236
 45  ω   -133.00  -4.00   0.50    0.50    --  -93.60  55.00-139.64  258
 46  ω   -174.00-137.00   0.50    0.50    --  -93.60  55.00-139.64   74
 47  ω   -106.00  -4.00   0.50    0.50    --  -93.60  55.00  55.22  204
 48  ω   -109.00  -6.00   0.50    0.50    --  -93.60  54.00 -51.52  206
 49  ω   -163.00  -4.00   0.50    0.50    --  -93.60  55.00  98.23  318
 50  ω   -174.00-149.00   0.50    0.50    --  -93.60  55.00  55.22   50
 51  ω   -180.00 -17.00   0.50    0.50    --  -93.60  55.00 146.72  326
 52  ω    -29.00  -4.00   0.50    0.50    --  -93.60  55.00 -78.80   50
 53  ω   -173.00 -42.00   0.50    0.50    --  -93.60  55.00 -78.80  262
 54  ω   -133.00  -4.00   0.50    0.50    --  -93.60  54.00  11.79  258
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0759469000
_diffrn_orient_matrix_UB_12      -0.0638953000
_diffrn_orient_matrix_UB_13      -0.0535028000
_diffrn_orient_matrix_UB_21      0.1097172000
_diffrn_orient_matrix_UB_22      0.0039705000
_diffrn_orient_matrix_UB_23      0.1140560000
_diffrn_orient_matrix_UB_31      -0.0627418000
_diffrn_orient_matrix_UB_32      -0.1084195000
_diffrn_orient_matrix_UB_33      0.0258029000
_diffrn_oxdiff_digest_frames     
;
010341f349be7fad7c79cb0d6852f66c1d000276335
;
_diffrn_oxdiff_digest_hkl        
;
015bc4d3fe33dbbd68afa1e0601d3def6f89e1
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5843
_reflns_number_total             6351
_reflns_odcompleteness_completeness 98.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         6351
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0319
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0516P)²+0.3362P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0854
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups
2. Others
 Sof(H20C)=Sof(H20D)=Sof(C19A)=Sof(H19C)=Sof(H19D)=Sof(Cl)=1-FVAR(1)
 Sof(Cl18)=Sof(H20A)=Sof(H20B)=Sof(C19)=Sof(H19A)=Sof(H19B)=FVAR(1)
 Sof(O1A)=Sof(O23A)=Sof(C22A)=Sof(H22C)=Sof(H22D)=Sof(C27A)=Sof(H27C)=
 Sof(H27D)=Sof(C24A)=Sof(H24C)=Sof(H24D)=Sof(C26A)=Sof(H26C)=Sof(H26D)=Sof(C8A)=
 Sof(H8AA)=Sof(H8AB)=Sof(O6A)=Sof(C32A)=Sof(H32C)=Sof(H32D)=Sof(C40A)=Sof(H40C)=
 Sof(H40D)=Sof(O28A)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(C31A)=Sof(H31C)=Sof(H31D)=
 Sof(O2A)=Sof(C30A)=Sof(H30C)=Sof(H30D)=Sof(C37A)=Sof(H37C)=Sof(H37D)=Sof(O3A)=
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=1-FVAR(2)
 Sof(O23)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(C22)=
 Sof(H22A)=Sof(H22B)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(O28)=Sof(C27)=Sof(H27A)=
 Sof(H27B)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(C31)=
 Sof(H31A)=Sof(H31B)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(O1)=Sof(O2)=Sof(O3)=
 Sof(O6)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C1)=Sof(H1A)=
 Sof(H1B)=FVAR(2)
3.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C20(H20C,H20D), C30(H30A,H30B), C32(H32A,H32B), C22(H22A,
 H22B), C37(H37A,H37B), C19(H19A,H19B), C27(H27A,H27B), C40(H40A,H40B),
 C24(H24A,H24B), C31(H31A,H31B), C26(H26A,H26B), C19A(H19C,H19D), C8(H8A,H8B),
 C4(H4A,H4B), C1(H1A,H1B), C22A(H22C,H22D), C27A(H27C,H27D), C24A(H24C,H24D),
 C26A(H26C,H26D), C8A(H8AA,H8AB), C32A(H32C,H32D), C40A(H40C,H40D), C4A(H4AA,
 H4AB), C31A(H31C,H31D), C30A(H30C,H30D), C37A(H37C,H37D), C1A(H1AA,H1AB)
3.b Idealised Me refined as rotating group:
 N21(H21A,H21B,H21C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.34531(2) 0.88975(2) 0.51233(2) 0.03986(9) Uani 1 1 d . . . . .
S6 S 0.11410(4) 1.02603(4) 0.72091(4) 0.04874(11) Uani 1 1 d . . . . .
S9 S 0.39872(4) 0.84397(4) 0.68265(3) 0.05038(12) Uani 1 1 d . . . . .
S7 S 0.19211(4) 0.97573(4) 0.52313(3) 0.04937(11) Uani 1 1 d . . . . .
S16 S 0.50570(4) 0.81197(4) 0.50730(3) 0.04943(11) Uani 1 1 d . . . . .
S15 S 0.29101(4) 0.92998(4) 0.34009(3) 0.04985(11) Uani 1 1 d . . . . .
S4 S 0.30192(5) 0.90225(4) 0.86592(3) 0.05250(12) Uani 1 1 d . . . . .
S13 S 0.59949(4) 0.77113(4) 0.31789(4) 0.05431(12) Uani 1 1 d . . . . .
S11 S 0.40841(5) 0.88711(4) 0.16625(4) 0.05398(12) Uani 1 1 d . . . . .
S8 S 0.12638(5) 1.00307(4) 0.95445(4) 0.06108(14) Uani 1 1 d . . . . .
S17 S 0.58990(5) 0.78615(5) 0.08491(4) 0.06690(15) Uani 1 1 d . . . . .
Cl18 Cl 0.6620(3) 0.5467(2) 0.4866(2) 0.0867(7) Uani 0.692(5) 1 d . . P A 1
N21 N 0.83469(14) 0.49783(11) 0.74466(12) 0.0472(3) Uani 1 1 d . . . . .
H21A H 0.813838 0.565428 0.728815 0.071 Uiso 1 1 calc GR . . . .
H21B H 0.911935 0.492760 0.740493 0.071 Uiso 1 1 calc GR . . . .
H21C H 0.837336 0.484776 0.814059 0.071 Uiso 1 1 calc GR . . . .
C3 C 0.29768(16) 0.90769(13) 0.72965(13) 0.0420(3) Uani 1 1 d . . . . .
C2 C 0.20868(15) 0.96545(13) 0.66060(13) 0.0408(3) Uani 1 1 d . . . . .
C12 C 0.53537(17) 0.81344(15) 0.18445(15) 0.0502(4) Uani 1 1 d . . . . .
C10 C 0.40362(16) 0.87770(13) 0.29984(13) 0.0434(3) Uani 1 1 d . . . . .
C5 C 0.17835(17) 0.97871(14) 0.85244(14) 0.0468(4) Uani 1 1 d . . . . .
C14 C 0.49550(16) 0.82470(14) 0.37203(14) 0.0432(3) Uani 1 1 d . . . . .
O23 O 0.8536(5) 0.3438(4) 0.9112(3) 0.0619(10) Uani 0.453(4) 1 d . . P B 1
C20 C 0.7372(2) 0.41614(17) 0.66310(17) 0.0654(5) Uani 1 1 d . . . . .
H20A H 0.652791 0.424457 0.665552 0.078 Uiso 0.692(5) 1 calc R . P A 1
H20B H 0.756064 0.342547 0.684896 0.078 Uiso 0.692(5) 1 calc R . P A 1
H20C H 0.777194 0.377560 0.619444 0.078 Uiso 0.308(5) 1 calc R . P A 2
H20D H 0.702136 0.362248 0.702953 0.078 Uiso 0.308(5) 1 calc R . P A 2
C30 C 0.8525(15) 0.7855(9) 0.6824(12) 0.065(4) Uani 0.453(4) 1 d . . P B 1
H30A H 0.781874 0.759931 0.612704 0.079 Uiso 0.453(4) 1 calc R . P B 1
H30B H 0.892188 0.857040 0.671526 0.079 Uiso 0.453(4) 1 calc R . P B 1
C32 C 0.6797(7) 0.7010(6) 0.8648(6) 0.0661(16) Uani 0.453(4) 1 d . . P B 1
H32A H 0.612722 0.749182 0.842713 0.079 Uiso 0.453(4) 1 calc R . P B 1
H32B H 0.745141 0.731172 0.935779 0.079 Uiso 0.453(4) 1 calc R . P B 1
C22 C 0.6871(10) 0.4206(10) 0.9480(8) 0.072(3) Uani 0.453(4) 1 d . . P B 1
H22A H 0.624999 0.378452 0.881711 0.086 Uiso 0.453(4) 1 calc R . P B 1
H22B H 0.646435 0.427728 1.003317 0.086 Uiso 0.453(4) 1 calc R . P B 1
C37 C 1.0988(16) 0.6308(14) 0.6572(13) 0.081(4) Uani 0.453(4) 1 d . . P B 1
H37A H 1.140718 0.630559 0.602164 0.098 Uiso 0.453(4) 1 calc R . P B 1
H37B H 1.163356 0.658711 0.729504 0.098 Uiso 0.453(4) 1 calc R . P B 1
C19 C 0.7332(4) 0.4275(2) 0.5465(2) 0.0706(10) Uani 0.692(5) 1 d . . P A 1
H19A H 0.683879 0.362020 0.500061 0.085 Uiso 0.692(5) 1 calc R . P A 1
H19B H 0.820511 0.432669 0.546253 0.085 Uiso 0.692(5) 1 calc R . P A 1
O28 O 0.7351(4) 0.6949(3) 0.7818(3) 0.0592(10) Uani 0.453(4) 1 d . . P B 1
C27 C 0.9692(10) 0.2942(7) 0.9531(7) 0.072(2) Uani 0.453(4) 1 d . . P B 1
H27A H 0.953911 0.227313 0.988663 0.087 Uiso 0.453(4) 1 calc R . P B 1
H27B H 1.035844 0.344411 1.009337 0.087 Uiso 0.453(4) 1 calc R . P B 1
C40 C 1.1492(7) 0.3943(8) 0.7654(8) 0.079(2) Uani 0.453(4) 1 d . . P B 1
H40A H 1.228635 0.417654 0.828700 0.095 Uiso 0.453(4) 1 calc R . P B 1
H40B H 1.160680 0.325350 0.733146 0.095 Uiso 0.453(4) 1 calc R . P B 1
C24 C 0.8041(7) 0.3625(5) 0.9957(6) 0.0764(17) Uani 0.453(4) 1 d . . P B 1
H24A H 0.868860 0.407378 1.058384 0.092 Uiso 0.453(4) 1 calc R . P B 1
H24B H 0.781025 0.292768 1.023128 0.092 Uiso 0.453(4) 1 calc R . P B 1
C31 C 0.8002(6) 0.7976(4) 0.7744(5) 0.0690(15) Uani 0.453(4) 1 d . . P B 1
H31A H 0.870168 0.820425 0.845431 0.083 Uiso 0.453(4) 1 calc R . P B 1
H31B H 0.741295 0.852906 0.757538 0.083 Uiso 0.453(4) 1 calc R . P B 1
C26 C 1.0121(7) 0.2679(5) 0.8605(5) 0.0736(15) Uani 0.453(4) 1 d . . P B 1
H26A H 1.087546 0.229174 0.887999 0.088 Uiso 0.453(4) 1 calc R . P B 1
H26B H 0.944109 0.220330 0.802528 0.088 Uiso 0.453(4) 1 calc R . P B 1
C19A C 0.6375(6) 0.4691(6) 0.5908(6) 0.064(2) Uani 0.308(5) 1 d . . P A 2
H19C H 0.617848 0.527111 0.633114 0.077 Uiso 0.308(5) 1 calc R . P A 2
H19D H 0.560117 0.416554 0.557493 0.077 Uiso 0.308(5) 1 calc R . P A 2
Cl Cl 0.6856(8) 0.5259(6) 0.4842(5) 0.095(2) Uani 0.308(5) 1 d . . P A 2
O1 O 0.7253(4) 0.5245(4) 0.9194(3) 0.0600(9) Uani 0.453(4) 1 d . . P B 1
O2 O 1.0476(4) 0.5265(4) 0.6650(3) 0.0676(11) Uani 0.453(4) 1 d . . P B 1
O3 O 0.9403(4) 0.7142(3) 0.7057(3) 0.0600(9) Uani 0.453(4) 1 d . . P B 1
O6 O 1.0426(4) 0.3660(3) 0.8156(4) 0.0590(10) Uani 0.453(4) 1 d . . P B 1
C8 C 0.6236(6) 0.5888(6) 0.8781(5) 0.0761(18) Uani 0.453(4) 1 d . . P B 1
H8A H 0.578512 0.592361 0.930541 0.091 Uiso 0.453(4) 1 calc R . P B 1
H8B H 0.562356 0.556416 0.806130 0.091 Uiso 0.453(4) 1 calc R . P B 1
C4 C 1.1434(7) 0.4548(7) 0.7024(6) 0.0813(19) Uani 0.453(4) 1 d . . P B 1
H4A H 1.140670 0.413689 0.635254 0.098 Uiso 0.453(4) 1 calc R . P B 1
H4B H 1.225703 0.501963 0.729685 0.098 Uiso 0.453(4) 1 calc R . P B 1
C1 C 0.9935(7) 0.7046(5) 0.6222(6) 0.0737(18) Uani 0.453(4) 1 d . . P B 1
H1A H 1.028968 0.777153 0.609358 0.088 Uiso 0.453(4) 1 calc R . P B 1
H1B H 0.926413 0.674130 0.552141 0.088 Uiso 0.453(4) 1 calc R . P B 1
O1A O 0.7097(3) 0.5843(3) 0.8834(3) 0.0612(8) Uani 0.547(4) 1 d . . P B 2
O23A O 0.7952(4) 0.3799(3) 0.9204(3) 0.0602(8) Uani 0.547(4) 1 d . . P B 2
C22A C 0.6406(6) 0.4965(5) 0.9162(4) 0.0753(13) Uani 0.547(4) 1 d . . P B 2
H22C H 0.579271 0.453510 0.850066 0.090 Uiso 0.547(4) 1 calc R . P B 2
H22D H 0.593088 0.524888 0.959262 0.090 Uiso 0.547(4) 1 calc R . P B 2
C27A C 0.8945(6) 0.3204(4) 0.9829(5) 0.0749(14) Uani 0.547(4) 1 d . . P B 2
H27C H 0.861122 0.265485 1.022852 0.090 Uiso 0.547(4) 1 calc R . P B 2
H27D H 0.962863 0.370181 1.038097 0.090 Uiso 0.547(4) 1 calc R . P B 2
C24A C 0.7362(9) 0.4253(9) 0.9870(6) 0.073(2) Uani 0.547(4) 1 d . . P B 2
H24C H 0.800537 0.469364 1.050580 0.087 Uiso 0.547(4) 1 calc R . P B 2
H24D H 0.692133 0.367092 1.015720 0.087 Uiso 0.547(4) 1 calc R . P B 2
C26A C 0.9461(8) 0.2665(5) 0.9083(7) 0.073(2) Uani 0.547(4) 1 d . . P B 2
H26C H 1.007938 0.218918 0.950484 0.087 Uiso 0.547(4) 1 calc R . P B 2
H26D H 0.876719 0.221264 0.849227 0.087 Uiso 0.547(4) 1 calc R . P B 2
C8A C 0.6332(5) 0.6620(5) 0.8244(5) 0.0626(12) Uani 0.547(4) 1 d . . P B 2
H8AA H 0.584421 0.688380 0.867342 0.075 Uiso 0.547(4) 1 calc R . P B 2
H8AB H 0.572521 0.628622 0.752538 0.075 Uiso 0.547(4) 1 calc R . P B 2
O6A O 1.0076(3) 0.3482(3) 0.8600(3) 0.0645(9) Uani 0.547(4) 1 d . . P B 2
C32A C 0.7182(4) 0.7542(4) 0.8060(4) 0.0605(11) Uani 0.547(4) 1 d . . P B 2
H32C H 0.668078 0.812824 0.772469 0.073 Uiso 0.547(4) 1 calc R . P B 2
H32D H 0.783203 0.783502 0.877680 0.073 Uiso 0.547(4) 1 calc R . P B 2
C40A C 1.0613(5) 0.3031(5) 0.7876(6) 0.0804(16) Uani 0.547(4) 1 d . . P B 2
H40C H 1.137618 0.272754 0.834989 0.097 Uiso 0.547(4) 1 calc R . P B 2
H40D H 0.999970 0.240893 0.744874 0.097 Uiso 0.547(4) 1 calc R . P B 2
O28A O 0.7785(3) 0.7176(2) 0.7345(3) 0.0537(7) Uani 0.547(4) 1 d . . P B 2
C4A C 1.0893(10) 0.3502(8) 0.7278(7) 0.094(2) Uani 0.547(4) 1 d . . P B 2
H4AA H 1.046735 0.308628 0.655648 0.113 Uiso 0.547(4) 1 calc R . P B 2
H4AB H 1.181098 0.346535 0.747735 0.113 Uiso 0.547(4) 1 calc R . P B 2
C31A C 0.8562(13) 0.8062(9) 0.7097(11) 0.071(3) Uani 0.547(4) 1 d . . P B 2
H31C H 0.923976 0.838651 0.778397 0.085 Uiso 0.547(4) 1 calc R . P B 2
H31D H 0.803795 0.862935 0.674460 0.085 Uiso 0.547(4) 1 calc R . P B 2
O2A O 1.0710(4) 0.4717(3) 0.7042(3) 0.0700(9) Uani 0.547(4) 1 d . . P B 2
C30A C 0.9133(5) 0.7607(3) 0.6319(4) 0.0688(12) Uani 0.547(4) 1 d . . P B 2
H30C H 0.844953 0.727432 0.563890 0.083 Uiso 0.547(4) 1 calc R . P B 2
H30D H 0.964370 0.819686 0.610814 0.083 Uiso 0.547(4) 1 calc R . P B 2
C37A C 1.1487(5) 0.5661(6) 0.6900(5) 0.0795(15) Uani 0.547(4) 1 d . . P B 2
H37C H 1.203046 0.544512 0.650198 0.095 Uiso 0.547(4) 1 calc R . P B 2
H37D H 1.204341 0.600585 0.763128 0.095 Uiso 0.547(4) 1 calc R . P B 2
O3A O 0.9927(3) 0.6803(3) 0.6851(3) 0.0615(8) Uani 0.547(4) 1 d . . P B 2
C1A C 1.0631(12) 0.6465(11) 0.6240(10) 0.070(3) Uani 0.547(4) 1 d . . P B 2
H1AA H 1.115187 0.709627 0.610196 0.084 Uiso 0.547(4) 1 calc R . P B 2
H1AB H 1.005322 0.611490 0.551809 0.084 Uiso 0.547(4) 1 calc R . P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S9 2.1590(5) . ?
Ni1 S7 2.1686(5) . ?
Ni1 S16 2.1597(5) . ?
Ni1 S15 2.1609(5) . ?
S6 C2 1.7426(16) . ?
S6 C5 1.7286(18) . ?
S9 C3 1.7174(16) . ?
S7 C2 1.7174(16) . ?
S16 C14 1.7120(17) . ?
S15 C10 1.7120(17) . ?
S4 C3 1.7370(16) . ?
S4 C5 1.7295(17) . ?
S13 C12 1.7250(19) . ?
S13 C14 1.7401(16) . ?
S11 C12 1.7299(19) . ?
S11 C10 1.7419(16) . ?
S8 C5 1.6488(17) . ?
S17 C12 1.6470(17) . ?
Cl18 C19 1.809(5) . ?
N21 H21A 0.9000 . ?
N21 H21B 0.9000 . ?
N21 H21C 0.9000 . ?
N21 C20 1.486(2) . ?
C3 C2 1.363(2) . ?
C10 C14 1.362(2) . ?
O23 C27 1.434(12) . ?
O23 C24 1.411(8) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C20 H20D 0.9800 . ?
C20 C19 1.493(4) . ?
C20 C19A 1.415(7) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 C31 1.508(16) . ?
C30 O3 1.357(14) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 O28 1.418(8) . ?
C32 C8 1.495(10) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 C24 1.511(14) . ?
C22 O1 1.405(13) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 O2 1.371(17) . ?
C37 C1 1.524(16) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
O28 C31 1.414(7) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 C26 1.477(13) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 O6 1.565(10) . ?
C40 C4 1.103(11) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 O6 1.413(8) . ?
C19A H19C 0.9800 . ?
C19A H19D 0.9800 . ?
C19A Cl 1.773(9) . ?
O1 C8 1.420(9) . ?
O2 C4 1.429(10) . ?
O3 C1 1.411(8) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
O1A C22A 1.423(7) . ?
O1A C8A 1.411(7) . ?
O23A C27A 1.417(7) . ?
O23A C24A 1.398(11) . ?
C22A H22C 0.9800 . ?
C22A H22D 0.9800 . ?
C22A C24A 1.520(12) . ?
C27A H27C 0.9800 . ?
C27A H27D 0.9800 . ?
C27A C26A 1.468(11) . ?
C24A H24C 0.9800 . ?
C24A H24D 0.9800 . ?
C26A H26C 0.9800 . ?
C26A H26D 0.9800 . ?
C26A O6A 1.434(10) . ?
C8A H8AA 0.9800 . ?
C8A H8AB 0.9800 . ?
C8A C32A 1.482(8) . ?
O6A C40A 1.413(7) . ?
C32A H32C 0.9800 . ?
C32A H32D 0.9800 . ?
C32A O28A 1.416(6) . ?
C40A H40C 0.9800 . ?
C40A H40D 0.9800 . ?
C40A C4A 1.086(9) . ?
O28A C31A 1.435(13) . ?
C4A H4AA 0.9800 . ?
C4A H4AB 0.9800 . ?
C4A O2A 1.558(9) . ?
C31A H31C 0.9800 . ?
C31A H31D 0.9800 . ?
C31A C30A 1.497(13) . ?
O2A C37A 1.432(7) . ?
C30A H30C 0.9800 . ?
C30A H30D 0.9800 . ?
C30A O3A 1.431(6) . ?
C37A H37C 0.9800 . ?
C37A H37D 0.9800 . ?
C37A C1A 1.518(11) . ?
O3A C1A 1.386(15) . ?
C1A H1AA 0.9800 . ?
C1A H1AB 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S9 Ni1 S7 93.087(17) . . ?
S9 Ni1 S16 86.049(17) . . ?
S9 Ni1 S15 178.12(2) . . ?
S16 Ni1 S7 176.68(2) . . ?
S16 Ni1 S15 93.002(18) . . ?
S15 Ni1 S7 87.950(17) . . ?
C5 S6 C2 97.50(8) . . ?
C3 S9 Ni1 102.34(6) . . ?
C2 S7 Ni1 102.02(6) . . ?
C14 S16 Ni1 102.30(6) . . ?
C10 S15 Ni1 102.36(6) . . ?
C5 S4 C3 97.37(8) . . ?
C12 S13 C14 97.58(8) . . ?
C12 S11 C10 97.46(8) . . ?
H21A N21 H21B 109.5 . . ?
H21A N21 H21C 109.5 . . ?
H21B N21 H21C 109.5 . . ?
C20 N21 H21A 109.5 . . ?
C20 N21 H21B 109.5 . . ?
C20 N21 H21C 109.5 . . ?
S9 C3 S4 122.58(10) . . ?
C2 C3 S9 121.12(12) . . ?
C2 C3 S4 116.30(12) . . ?
S7 C2 S6 123.10(9) . . ?
C3 C2 S6 115.64(12) . . ?
C3 C2 S7 121.26(12) . . ?
S13 C12 S11 113.12(10) . . ?
S17 C12 S13 123.21(12) . . ?
S17 C12 S11 123.67(12) . . ?
S15 C10 S11 123.12(10) . . ?
C14 C10 S15 121.06(13) . . ?
C14 C10 S11 115.82(13) . . ?
S6 C5 S4 113.16(9) . . ?
S8 C5 S6 123.46(10) . . ?
S8 C5 S4 123.38(11) . . ?
S16 C14 S13 122.79(10) . . ?
C10 C14 S16 121.25(13) . . ?
C10 C14 S13 115.96(13) . . ?
C24 O23 C27 111.4(7) . . ?
N21 C20 H20A 109.0 . . ?
N21 C20 H20B 109.0 . . ?
N21 C20 H20C 109.7 . . ?
N21 C20 H20D 109.7 . . ?
N21 C20 C19 112.77(19) . . ?
H20A C20 H20B 107.8 . . ?
H20C C20 H20D 108.2 . . ?
C19 C20 H20A 109.0 . . ?
C19 C20 H20B 109.0 . . ?
C19A C20 N21 109.9(3) . . ?
C19A C20 H20C 109.7 . . ?
C19A C20 H20D 109.7 . . ?
H30A C30 H30B 107.9 . . ?
C31 C30 H30A 109.2 . . ?
C31 C30 H30B 109.2 . . ?
O3 C30 H30A 109.2 . . ?
O3 C30 H30B 109.2 . . ?
O3 C30 C31 112.1(8) . . ?
H32A C32 H32B 108.3 . . ?
O28 C32 H32A 109.9 . . ?
O28 C32 H32B 109.9 . . ?
O28 C32 C8 109.0(5) . . ?
C8 C32 H32A 109.9 . . ?
C8 C32 H32B 109.9 . . ?
H22A C22 H22B 108.4 . . ?
C24 C22 H22A 110.0 . . ?
C24 C22 H22B 110.0 . . ?
O1 C22 H22A 110.0 . . ?
O1 C22 H22B 110.0 . . ?
O1 C22 C24 108.6(7) . . ?
H37A C37 H37B 108.2 . . ?
O2 C37 H37A 109.7 . . ?
O2 C37 H37B 109.7 . . ?
O2 C37 C1 109.9(12) . . ?
C1 C37 H37A 109.7 . . ?
C1 C37 H37B 109.7 . . ?
Cl18 C19 H19A 109.1 . . ?
Cl18 C19 H19B 109.1 . . ?
C20 C19 Cl18 112.3(2) . . ?
C20 C19 H19A 109.1 . . ?
C20 C19 H19B 109.1 . . ?
H19A C19 H19B 107.9 . . ?
C31 O28 C32 110.7(5) . . ?
O23 C27 H27A 109.7 . . ?
O23 C27 H27B 109.7 . . ?
O23 C27 C26 109.8(6) . . ?
H27A C27 H27B 108.2 . . ?
C26 C27 H27A 109.7 . . ?
C26 C27 H27B 109.7 . . ?
H40A C40 H40B 106.5 . . ?
O6 C40 H40A 106.4 . . ?
O6 C40 H40B 106.4 . . ?
C4 C40 H40A 106.4 . . ?
C4 C40 H40B 106.4 . . ?
C4 C40 O6 123.6(7) . . ?
O23 C24 C22 108.9(7) . . ?
O23 C24 H24A 109.9 . . ?
O23 C24 H24B 109.9 . . ?
C22 C24 H24A 109.9 . . ?
C22 C24 H24B 109.9 . . ?
H24A C24 H24B 108.3 . . ?
C30 C31 H31A 110.2 . . ?
C30 C31 H31B 110.2 . . ?
O28 C31 C30 107.6(6) . . ?
O28 C31 H31A 110.2 . . ?
O28 C31 H31B 110.2 . . ?
H31A C31 H31B 108.5 . . ?
C27 C26 H26A 109.9 . . ?
C27 C26 H26B 109.9 . . ?
H26A C26 H26B 108.3 . . ?
O6 C26 C27 108.9(6) . . ?
O6 C26 H26A 109.9 . . ?
O6 C26 H26B 109.9 . . ?
C20 C19A H19C 109.8 . . ?
C20 C19A H19D 109.8 . . ?
C20 C19A Cl 109.4(5) . . ?
H19C C19A H19D 108.2 . . ?
Cl C19A H19C 109.8 . . ?
Cl C19A H19D 109.8 . . ?
C22 O1 C8 113.6(7) . . ?
C37 O2 C4 112.1(8) . . ?
C30 O3 C1 112.9(7) . . ?
C26 O6 C40 128.5(5) . . ?
C32 C8 H8A 110.1 . . ?
C32 C8 H8B 110.1 . . ?
O1 C8 C32 108.0(6) . . ?
O1 C8 H8A 110.1 . . ?
O1 C8 H8B 110.1 . . ?
H8A C8 H8B 108.4 . . ?
C40 C4 O2 125.6(7) . . ?
C40 C4 H4A 105.9 . . ?
C40 C4 H4B 105.9 . . ?
O2 C4 H4A 105.9 . . ?
O2 C4 H4B 105.9 . . ?
H4A C4 H4B 106.2 . . ?
C37 C1 H1A 109.6 . . ?
C37 C1 H1B 109.6 . . ?
O3 C1 C37 110.4(9) . . ?
O3 C1 H1A 109.6 . . ?
O3 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
C8A O1A C22A 113.9(5) . . ?
C24A O23A C27A 112.0(6) . . ?
O1A C22A H22C 110.1 . . ?
O1A C22A H22D 110.1 . . ?
O1A C22A C24A 108.0(6) . . ?
H22C C22A H22D 108.4 . . ?
C24A C22A H22C 110.1 . . ?
C24A C22A H22D 110.1 . . ?
O23A C27A H27C 109.6 . . ?
O23A C27A H27D 109.6 . . ?
O23A C27A C26A 110.1(5) . . ?
H27C C27A H27D 108.1 . . ?
C26A C27A H27C 109.6 . . ?
C26A C27A H27D 109.6 . . ?
O23A C24A C22A 108.4(6) . . ?
O23A C24A H24C 110.0 . . ?
O23A C24A H24D 110.0 . . ?
C22A C24A H24C 110.0 . . ?
C22A C24A H24D 110.0 . . ?
H24C C24A H24D 108.4 . . ?
C27A C26A H26C 109.9 . . ?
C27A C26A H26D 109.9 . . ?
H26C C26A H26D 108.3 . . ?
O6A C26A C27A 109.0(5) . . ?
O6A C26A H26C 109.9 . . ?
O6A C26A H26D 109.9 . . ?
O1A C8A H8AA 110.0 . . ?
O1A C8A H8AB 110.0 . . ?
O1A C8A C32A 108.4(4) . . ?
H8AA C8A H8AB 108.4 . . ?
C32A C8A H8AA 110.0 . . ?
C32A C8A H8AB 110.0 . . ?
C40A O6A C26A 112.8(5) . . ?
C8A C32A H32C 109.7 . . ?
C8A C32A H32D 109.7 . . ?
H32C C32A H32D 108.2 . . ?
O28A C32A C8A 109.7(4) . . ?
O28A C32A H32C 109.7 . . ?
O28A C32A H32D 109.7 . . ?
O6A C40A H40C 106.6 . . ?
O6A C40A H40D 106.6 . . ?
H40C C40A H40D 106.6 . . ?
C4A C40A O6A 123.0(6) . . ?
C4A C40A H40C 106.6 . . ?
C4A C40A H40D 106.6 . . ?
C32A O28A C31A 111.2(6) . . ?
C40A C4A H4AA 105.7 . . ?
C40A C4A H4AB 105.7 . . ?
C40A C4A O2A 126.5(6) . . ?
H4AA C4A H4AB 106.1 . . ?
O2A C4A H4AA 105.7 . . ?
O2A C4A H4AB 105.7 . . ?
O28A C31A H31C 110.2 . . ?
O28A C31A H31D 110.2 . . ?
O28A C31A C30A 107.5(8) . . ?
H31C C31A H31D 108.5 . . ?
C30A C31A H31C 110.2 . . ?
C30A C31A H31D 110.2 . . ?
C37A O2A C4A 135.6(6) . . ?
C31A C30A H30C 109.7 . . ?
C31A C30A H30D 109.7 . . ?
H30C C30A H30D 108.2 . . ?
O3A C30A C31A 109.9(7) . . ?
O3A C30A H30C 109.7 . . ?
O3A C30A H30D 109.7 . . ?
O2A C37A H37C 109.8 . . ?
O2A C37A H37D 109.8 . . ?
O2A C37A C1A 109.3(7) . . ?
H37C C37A H37D 108.3 . . ?
C1A C37A H37C 109.8 . . ?
C1A C37A H37D 109.8 . . ?
C1A O3A C30A 112.6(7) . . ?
C37A C1A H1AA 110.0 . . ?
C37A C1A H1AB 110.0 . . ?
O3A C1A C37A 108.5(9) . . ?
O3A C1A H1AA 110.0 . . ?
O3A C1A H1AB 110.0 . . ?
H1AA C1A H1AB 108.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S9 C3 S4 -177.95(9) . . . . ?
Ni1 S9 C3 C2 2.31(16) . . . . ?
Ni1 S7 C2 S6 177.01(9) . . . . ?
Ni1 S7 C2 C3 -3.46(15) . . . . ?
Ni1 S16 C14 S13 -177.63(9) . . . . ?
Ni1 S16 C14 C10 2.02(16) . . . . ?
Ni1 S15 C10 S11 -179.50(9) . . . . ?
Ni1 S15 C10 C14 1.03(15) . . . . ?
S9 C3 C2 S6 -179.60(9) . . . . ?
S9 C3 C2 S7 0.8(2) . . . . ?
S15 C10 C14 S16 -2.2(2) . . . . ?
S15 C10 C14 S13 177.50(9) . . . . ?
S4 C3 C2 S6 0.64(19) . . . . ?
S4 C3 C2 S7 -178.92(9) . . . . ?
S11 C10 C14 S16 178.31(9) . . . . ?
S11 C10 C14 S13 -2.01(19) . . . . ?
N21 C20 C19 Cl18 -72.7(3) . . . . ?
N21 C20 C19A Cl 81.0(5) . . . . ?
C3 S4 C5 S6 -1.68(12) . . . . ?
C3 S4 C5 S8 177.84(12) . . . . ?
C2 S6 C5 S4 1.95(11) . . . . ?
C2 S6 C5 S8 -177.56(12) . . . . ?
C12 S13 C14 S16 -179.87(11) . . . . ?
C12 S13 C14 C10 0.46(15) . . . . ?
C12 S11 C10 S15 -177.00(11) . . . . ?
C12 S11 C10 C14 2.50(15) . . . . ?
C10 S11 C12 S13 -2.11(12) . . . . ?
C10 S11 C12 S17 177.87(12) . . . . ?
C5 S6 C2 S7 177.97(11) . . . . ?
C5 S6 C2 C3 -1.58(15) . . . . ?
C5 S4 C3 S9 -179.11(11) . . . . ?
C5 S4 C3 C2 0.64(15) . . . . ?
C14 S13 C12 S11 1.24(12) . . . . ?
C14 S13 C12 S17 -178.73(12) . . . . ?
O23 C27 C26 O6 63.6(7) . . . . ?
C30 O3 C1 C37 175.4(10) . . . . ?
C32 O28 C31 C30 -178.2(7) . . . . ?
C22 O1 C8 C32 173.0(6) . . . . ?
C37 O2 C4 C40 136.2(12) . . . . ?
O28 C32 C8 O1 64.6(6) . . . . ?
C27 O23 C24 C22 176.8(6) . . . . ?
C27 C26 O6 C40 146.0(7) . . . . ?
C24 O23 C27 C26 175.4(6) . . . . ?
C24 C22 O1 C8 -177.3(5) . . . . ?
C31 C30 O3 C1 -178.0(7) . . . . ?
O1 C22 C24 O23 -65.2(7) . . . . ?
O2 C37 C1 O3 64.9(12) . . . . ?
O3 C30 C31 O28 -63.4(11) . . . . ?
O6 C40 C4 O2 7.6(14) . . . . ?
C8 C32 O28 C31 -174.2(5) . . . . ?
C4 C40 O6 C26 153.4(8) . . . . ?
C1 C37 O2 C4 -177.4(8) . . . . ?
O1A C22A C24A O23A -64.0(6) . . . . ?
O1A C8A C32A O28A 65.6(5) . . . . ?
O23A C27A C26A O6A 65.8(6) . . . . ?
C22A O1A C8A C32A 174.1(4) . . . . ?
C27A O23A C24A C22A 174.5(5) . . . . ?
C27A C26A O6A C40A 179.4(5) . . . . ?
C24A O23A C27A C26A 175.1(6) . . . . ?
C26A O6A C40A C4A 163.7(9) . . . . ?
C8A O1A C22A C24A -175.2(5) . . . . ?
C8A C32A O28A C31A 176.7(7) . . . . ?
O6A C40A C4A O2A -3.4(15) . . . . ?
C32A O28A C31A C30A -178.7(6) . . . . ?
C40A C4A O2A C37A 134.8(10) . . . . ?
O28A C31A C30A O3A -61.6(9) . . . . ?
C4A O2A C37A C1A 157.1(7) . . . . ?
C31A C30A O3A C1A -171.2(8) . . . . ?
O2A C37A C1A O3A 62.8(9) . . . . ?
C30A O3A C1A C37A 177.1(6) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.675
_oxdiff_exptl_absorpt_empirical_full_min 0.778
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_93k-f
_database_code_depnum_ccdc_archive 'CCDC 2053390'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-18 downloaded from the CCDC.
;
_audit_creation_date             2020-11-10
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C2 H7 Cl N, C12 H24 O6'
_chemical_formula_sum            'C20 H31 Cl N Ni O6 S10'
_chemical_formula_weight         796.22
_chemical_melting_point          ?
_chemical_oxdiff_formula         ClCNNiSHO
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.2107(3)
_cell_length_b                   12.3150(2)
_cell_length_c                   12.7451(3)
_cell_angle_alpha                92.2792(18)
_cell_angle_beta                 112.126(2)
_cell_angle_gamma                96.0601(18)
_cell_volume                     1614.83(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    29610
_cell_measurement_temperature    93
_cell_measurement_theta_max      30.9190
_cell_measurement_theta_min      2.1280
_shelx_estimated_absorpt_T_max   0.791
_shelx_estimated_absorpt_T_min   0.452
_exptl_absorpt_coefficient_mu    1.366
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             822
_exptl_crystal_size_max          0.69
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0907
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.837
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            45358
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.837
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.014
_diffrn_reflns_theta_min         1.978
_diffrn_ambient_temperature      93
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.837
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -42.00  18.00   0.50    0.24    --    5.18 -30.00 -11.44  120
  2  ω    -67.00  18.00   0.50    0.24    --    5.18 -32.00 -57.00  170
  3  ω    -63.00  18.00   0.50    0.24    --    5.18 -29.00  28.00  162
  4  ω    -64.00  19.00   0.50    0.24    --    5.18 -33.00 132.51  166
  5  ω    -40.00  18.00   0.50    0.24    --    5.18 -31.00 173.49  116
  6  ω    -69.00  18.00   0.50    0.24    --    5.18 -19.00  60.00  174
  7  ω    -10.00  78.00   0.50    0.24    --    5.18  57.00 -30.00  176
  8  ω     43.00  80.00   0.50    0.24    --    5.18  29.00-170.00   74
  9  ω    -63.00  19.00   0.50    0.24    --    5.18 -28.00-113.26  164
 10  ω    -17.00  28.00   0.50    0.24    --   -4.95 -99.00 150.00   90
 11  ω    -80.00 -25.00   0.50    0.24    --   -4.95 -29.00  28.00  110
 12  ω     37.00  66.00   0.50    0.24    --   -4.95  29.00-170.00   58
 13  ω    -17.00  12.00   0.50    0.24    --   -4.95  29.00-170.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0061888000
_diffrn_orient_matrix_UB_12      -0.0073309000
_diffrn_orient_matrix_UB_13      -0.0531169000
_diffrn_orient_matrix_UB_21      0.0668493000
_diffrn_orient_matrix_UB_22      0.0208920000
_diffrn_orient_matrix_UB_23      0.0260276000
_diffrn_orient_matrix_UB_31      0.0154338000
_diffrn_orient_matrix_UB_32      -0.0537563000
_diffrn_orient_matrix_UB_33      0.0117284000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6983
_reflns_number_total             8651
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.083
_refine_diff_density_min         -1.368
_refine_diff_density_rms         0.118
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         8651
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0495
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0915P)²+0.2292P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1395
_refine_ls_wR_factor_ref         0.1478
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
2. Others
 Sof(H7BC)=Sof(H7BD)=Sof(O4A)=Sof(O1A)=Sof(O6A)=Sof(H9BC)=Sof(H9BD)=Sof(O2A)=
 Sof(H3BC)=Sof(H3BD)=Sof(O3A)=Sof(O5A)=Sof(C11A)=Sof(H11A)=Sof(H11B)=Sof(C7A)=
 Sof(H7AC)=Sof(H7AD)=Sof(C9A)=Sof(H9AC)=Sof(H9AD)=Sof(C12A)=Sof(H12C)=Sof(H12D)=
 Sof(C3A)=Sof(H3AC)=Sof(H3AD)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(C13A)=Sof(H13C)=
 Sof(H13D)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(C14A)=Sof(H14C)=Sof(H14D)=1-FVAR(1)
 Sof(H7AA)=Sof(H7AB)=Sof(O3)=Sof(O6)=Sof(O1)=Sof(H9AA)=Sof(H9AB)=Sof(O2)=
 Sof(H3AA)=Sof(H3AB)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C5)=Sof(H5A)=Sof(H5B)=
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(C4)=Sof(H4A)=
 Sof(H4B)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(O5)=
 Sof(O4)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C11)=Sof(H11C)=Sof(H11D)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C7(H7BC,H7BD), C7(H7AA,H7AB), C9(H9BC,H9BD), C9(H9AA,H9AB),
 C2(H2A,H2B), C3(H3AA,H3AB), C3(H3BC,H3BD), C13(H13A,H13B), C11A(H11A,H11B),
 C5(H5A,H5B), C7A(H7AC,H7AD), C12(H12A,H12B), C10(H10A,H10B), C9A(H9AC,H9AD),
 C12A(H12C,H12D), C4(H4A,H4B), C14(H14A,H14B), C8(H8A,H8B), C6(H6A,H6B),
 C3A(H3AC,H3AD), C5A(H5AA,H5AB), C13A(H13C,H13D), C11(H11C,H11D), C6A(H6AA,
 H6AB), C14A(H14C,H14D)
3.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.34548(3) 0.89101(2) 1.01186(2) 0.02019(10) Uani 1 1 d . . . . .
S1 S 0.50591(5) 0.81058(5) 1.00747(5) 0.02375(14) Uani 1 1 d . . . . .
S4 S 0.41293(6) 0.89460(5) 0.66564(5) 0.02523(14) Uani 1 1 d . . . . .
S9 S 0.11356(6) 1.02893(5) 1.22145(6) 0.02665(14) Uani 1 1 d . . . . .
S8 S 0.30080(6) 0.90040(5) 1.36740(5) 0.02393(14) Uani 1 1 d . . . . .
S6 S 0.39674(6) 0.84120(4) 1.18222(5) 0.02295(14) Uani 1 1 d . . . . .
S2 S 0.29582(6) 0.93836(5) 0.84065(5) 0.02454(14) Uani 1 1 d . . . . .
S3 S 0.60051(6) 0.76998(5) 0.81704(6) 0.02876(15) Uani 1 1 d . . . . .
S7 S 0.19190(6) 0.97894(5) 1.02199(5) 0.02682(14) Uani 1 1 d . . . . .
S5 S 0.59276(7) 0.78908(6) 0.58295(6) 0.03366(16) Uani 1 1 d . . . . .
S10 S 0.12498(7) 1.00324(5) 1.45656(6) 0.03159(16) Uani 1 1 d . . . . .
Cl1 Cl 0.34018(8) 0.45202(6) 1.01407(7) 0.0553(2) Uani 1 1 d . . . . .
N1 N 0.16862(18) 0.50265(14) 0.75522(17) 0.0210(4) Uani 1 1 d . . . . .
H1A H 0.162935 0.519449 0.684740 0.025 Uiso 1 1 calc R U . . .
H1B H 0.089500 0.502365 0.759750 0.025 Uiso 1 1 calc R U . . .
H1C H 0.194810 0.435232 0.767949 0.025 Uiso 1 1 calc R U . . .
C19 C 0.2087(2) 0.96714(17) 1.1612(2) 0.0227(5) Uani 1 1 d . . . . .
C16 C 0.4075(2) 0.88311(17) 0.8002(2) 0.0220(4) Uani 1 1 d . . . . .
C18 C 0.2963(2) 0.90710(17) 1.2297(2) 0.0207(4) Uani 1 1 d . . . . .
C17 C 0.5386(2) 0.8167(2) 0.6835(2) 0.0260(5) Uani 1 1 d . . . . .
C1 C 0.2643(2) 0.58569(19) 0.8420(2) 0.0280(5) Uani 1 1 d . . . . .
H1D H 0.241208 0.659744 0.822430 0.034 Uiso 1 1 calc R U . . .
H1E H 0.351517 0.581548 0.840969 0.034 Uiso 1 1 calc R U . . .
C15 C 0.4978(2) 0.82606(18) 0.8723(2) 0.0233(5) Uani 1 1 d . . . . .
C20 C 0.1773(2) 0.97922(18) 1.3539(2) 0.0247(5) Uani 1 1 d . . . . .
C7 C 0.1454(3) 0.2024(2) 0.7981(3) 0.0416(7) Uani 1 1 d . . . . .
H7BC H 0.215043 0.213068 0.875026 0.050 Uiso 0.495(2) 1 calc R U P A 2
H7BD H 0.095679 0.129100 0.790248 0.050 Uiso 0.495(2) 1 calc R U P A 2
H7AA H 0.203156 0.151312 0.843255 0.050 Uiso 0.505(2) 1 calc R U P A 1
H7AB H 0.082078 0.159566 0.728342 0.050 Uiso 0.505(2) 1 calc R U P A 1
O4A O 0.0599(3) 0.2846(3) 0.7874(3) 0.0263(8) Uani 0.495(2) 1 d . . P A 2
O1A O 0.1420(3) 0.6620(3) 0.5905(3) 0.0246(7) Uani 0.495(2) 1 d . . P A 2
O3 O 0.2204(3) 0.2807(2) 0.7658(3) 0.0250(7) Uani 0.505(2) 1 d . . P A 1
O6 O -0.0008(3) 0.6542(3) 0.6359(3) 0.0275(8) Uani 0.505(2) 1 d . . P A 1
O6A O -0.0452(3) 0.6350(3) 0.6898(3) 0.0240(7) Uani 0.495(2) 1 d . . P A 2
O1 O 0.2165(3) 0.6170(3) 0.5831(3) 0.0250(7) Uani 0.505(2) 1 d . . P A 1
C9 C -0.0833(3) 0.3624(2) 0.8544(3) 0.0457(8) Uani 1 1 d . . . . .
H9BC H -0.109290 0.364910 0.920505 0.055 Uiso 0.495(2) 1 calc R U P A 2
H9BD H -0.160923 0.331701 0.787041 0.055 Uiso 0.495(2) 1 calc R U P A 2
H9AA H -0.144494 0.300284 0.858692 0.055 Uiso 0.505(2) 1 calc R U P A 1
H9AB H -0.029611 0.392701 0.933377 0.055 Uiso 0.505(2) 1 calc R U P A 1
C2 C 0.2688(3) 0.5692(2) 0.9598(3) 0.0396(6) Uani 1 1 d . . . . .
H2A H 0.179273 0.562210 0.958120 0.048 Uiso 1 1 calc R U . . .
H2B H 0.318802 0.634612 1.011346 0.048 Uiso 1 1 calc R U . . .
O2A O 0.2742(3) 0.4830(3) 0.5774(3) 0.0240(8) Uani 0.495(2) 1 d . . P A 2
O2 O 0.2974(4) 0.4101(3) 0.6181(3) 0.0260(8) Uani 0.505(2) 1 d . . P A 1
C3 C 0.2945(4) 0.5792(3) 0.5348(4) 0.0578(10) Uani 1 1 d . . . . .
H3AA H 0.354320 0.642436 0.530351 0.069 Uiso 0.505(2) 1 calc R U P A 1
H3AB H 0.239505 0.549933 0.455801 0.069 Uiso 0.505(2) 1 calc R U P A 1
H3BC H 0.313713 0.562872 0.466504 0.069 Uiso 0.495(2) 1 calc R U P A 2
H3BD H 0.373011 0.623025 0.591789 0.069 Uiso 0.495(2) 1 calc R U P A 2
O3A O 0.2694(3) 0.3102(3) 0.7133(3) 0.0238(7) Uani 0.495(2) 1 d . . P A 2
O5A O -0.0438(3) 0.4726(3) 0.8366(3) 0.0258(8) Uani 0.495(2) 1 d . . P A 2
C13 C 0.0245(8) 0.7083(6) 0.5489(7) 0.0321(15) Uani 0.505(2) 1 d . . P A 1
H13A H -0.057320 0.698981 0.480670 0.038 Uiso 0.505(2) 1 calc R U P A 1
H13B H 0.046067 0.787561 0.573682 0.038 Uiso 0.505(2) 1 calc R U P A 1
C11A C -0.1409(5) 0.5454(4) 0.8049(5) 0.0281(11) Uani 0.495(2) 1 d . . P A 2
H11A H -0.172080 0.556688 0.867124 0.034 Uiso 0.495(2) 1 calc R U P A 2
H11B H -0.215832 0.512860 0.736165 0.034 Uiso 0.495(2) 1 calc R U P A 2
C5 C 0.3219(6) 0.3065(4) 0.6284(6) 0.0285(11) Uani 0.505(2) 1 d . . P A 1
H5A H 0.417140 0.308264 0.653515 0.034 Uiso 0.505(2) 1 calc R U P A 1
H5B H 0.283134 0.268423 0.550914 0.034 Uiso 0.505(2) 1 calc R U P A 1
C7A C 0.2022(5) 0.2050(4) 0.7173(4) 0.0249(10) Uani 0.495(2) 1 d . . P A 2
H7AC H 0.133467 0.182445 0.641316 0.030 Uiso 0.495(2) 1 calc R U P A 2
H7AD H 0.264384 0.150533 0.733696 0.030 Uiso 0.495(2) 1 calc R U P A 2
C12 C -0.0568(5) 0.7015(4) 0.7067(5) 0.0300(11) Uani 0.505(2) 1 d . . P A 1
H12A H -0.105825 0.760871 0.669292 0.036 Uiso 0.505(2) 1 calc R U P A 1
H12B H 0.012124 0.733073 0.779713 0.036 Uiso 0.505(2) 1 calc R U P A 1
C10 C -0.1533(5) 0.4404(4) 0.8004(5) 0.0304(11) Uani 0.505(2) 1 d . . P A 1
H10A H -0.203749 0.465114 0.843952 0.036 Uiso 0.505(2) 1 calc R U P A 1
H10B H -0.215527 0.408974 0.724325 0.036 Uiso 0.505(2) 1 calc R U P A 1
C9A C 0.0096(5) 0.2919(4) 0.8733(5) 0.0281(11) Uani 0.495(2) 1 d . . P A 2
H9AC H -0.029122 0.217862 0.880302 0.034 Uiso 0.495(2) 1 calc R U P A 2
H9AD H 0.082169 0.316604 0.946599 0.034 Uiso 0.495(2) 1 calc R U P A 2
C12A C -0.0839(6) 0.6540(4) 0.7814(5) 0.0296(11) Uani 0.495(2) 1 d . . P A 2
H12C H -0.149514 0.705621 0.761798 0.035 Uiso 0.495(2) 1 calc R U P A 2
H12D H -0.008274 0.686444 0.849557 0.035 Uiso 0.495(2) 1 calc R U P A 2
C4 C 0.3703(5) 0.4972(4) 0.5886(5) 0.0299(11) Uani 0.505(2) 1 d . . P A 1
H4A H 0.442787 0.531160 0.658343 0.036 Uiso 0.505(2) 1 calc R U P A 1
H4B H 0.408340 0.466547 0.537079 0.036 Uiso 0.505(2) 1 calc R U P A 1
C14 C 0.1170(5) 0.6789(4) 0.5171(5) 0.0301(11) Uani 0.505(2) 1 d . . P A 1
H14A H 0.162208 0.747294 0.503979 0.036 Uiso 0.505(2) 1 calc R U P A 1
H14B H 0.072348 0.636834 0.441992 0.036 Uiso 0.505(2) 1 calc R U P A 1
C8 C 0.0771(5) 0.2398(4) 0.8608(5) 0.0332(12) Uani 0.505(2) 1 d . . P A 1
H8A H 0.139276 0.270891 0.936958 0.040 Uiso 0.505(2) 1 calc R U P A 1
H8B H 0.020524 0.177233 0.871085 0.040 Uiso 0.505(2) 1 calc R U P A 1
O5 O -0.0723(3) 0.5316(3) 0.7882(3) 0.0273(8) Uani 0.505(2) 1 d . . P A 1
O4 O 0.0004(4) 0.3202(3) 0.8065(3) 0.0282(8) Uani 0.505(2) 1 d . . P A 1
C6 C 0.2844(5) 0.2416(4) 0.6964(4) 0.0260(10) Uani 0.505(2) 1 d . . P A 1
H6A H 0.363185 0.213244 0.747931 0.031 Uiso 0.505(2) 1 calc R U P A 1
H6B H 0.226518 0.177810 0.647043 0.031 Uiso 0.505(2) 1 calc R U P A 1
C3A C 0.1932(5) 0.6445(4) 0.5047(5) 0.0280(11) Uani 0.495(2) 1 d . . P A 2
H3AC H 0.121875 0.609463 0.434756 0.034 Uiso 0.495(2) 1 calc R U P A 2
H3AD H 0.225270 0.716605 0.486747 0.034 Uiso 0.495(2) 1 calc R U P A 2
C5A C 0.3783(5) 0.4205(4) 0.6200(5) 0.0278(11) Uani 0.495(2) 1 d . . P A 2
H5AA H 0.394128 0.391132 0.553603 0.033 Uiso 0.495(2) 1 calc R U P A 2
H5AB H 0.456117 0.472453 0.665778 0.033 Uiso 0.495(2) 1 calc R U P A 2
C13A C -0.0163(5) 0.7350(4) 0.6455(5) 0.0272(10) Uani 0.495(2) 1 d . . P A 2
H13C H -0.099156 0.755808 0.591912 0.033 Uiso 0.495(2) 1 calc R U P A 2
H13D H 0.019785 0.793011 0.709332 0.033 Uiso 0.495(2) 1 calc R U P A 2
C11 C -0.1464(6) 0.6134(5) 0.7279(6) 0.0341(12) Uani 0.505(2) 1 d . . P A 1
H11C H -0.191071 0.645424 0.773170 0.041 Uiso 0.505(2) 1 calc R U P A 1
H11D H -0.213137 0.579844 0.654630 0.041 Uiso 0.505(2) 1 calc R U P A 1
C6A C 0.3749(5) 0.3350(4) 0.6839(6) 0.0263(11) Uani 0.495(2) 1 d . . P A 2
H6AA H 0.453033 0.348901 0.755319 0.032 Uiso 0.495(2) 1 calc R U P A 2
H6AB H 0.383844 0.268532 0.642585 0.032 Uiso 0.495(2) 1 calc R U P A 2
C14A C 0.0652(8) 0.7353(5) 0.5924(7) 0.0310(16) Uani 0.495(2) 1 d . . P A 2
H14C H 0.011526 0.741898 0.511582 0.037 Uiso 0.495(2) 1 calc R U P A 2
H14D H 0.123275 0.805522 0.620092 0.037 Uiso 0.495(2) 1 calc R U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S1 2.1601(6) . ?
Ni1 S6 2.1590(6) . ?
Ni1 S2 2.1602(6) . ?
Ni1 S7 2.1688(6) . ?
S1 C15 1.709(2) . ?
S4 C16 1.749(2) . ?
S4 C17 1.738(2) . ?
S9 C19 1.746(2) . ?
S9 C20 1.733(3) . ?
S8 C18 1.742(2) . ?
S8 C20 1.734(2) . ?
S6 C18 1.720(2) . ?
S2 C16 1.713(2) . ?
S3 C17 1.727(3) . ?
S3 C15 1.744(2) . ?
S7 C19 1.726(2) . ?
S5 C17 1.650(2) . ?
S10 C20 1.651(2) . ?
Cl1 C2 1.763(3) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N1 C1 1.485(3) . ?
C19 C18 1.354(3) . ?
C16 C15 1.365(3) . ?
C1 H1D 0.9900 . ?
C1 H1E 0.9900 . ?
C1 C2 1.505(4) . ?
C7 H7BC 0.9900 . ?
C7 H7BD 0.9900 . ?
C7 H7AA 0.9900 . ?
C7 H7AB 0.9900 . ?
C7 O4A 1.443(4) . ?
C7 O3 1.388(4) . ?
C7 C7A 1.399(6) . ?
C7 C8 1.394(6) . ?
O4A C9A 1.412(6) . ?
O1A C3A 1.433(6) . ?
O1A C14A 1.317(8) . ?
O3 C6 1.431(5) . ?
O6 C13 1.418(9) . ?
O6 C12 1.417(6) . ?
O6A C12A 1.410(6) . ?
O6A C13A 1.432(5) . ?
O1 C3 1.354(4) . ?
O1 C14 1.434(6) . ?
C9 H9BC 0.9900 . ?
C9 H9BD 0.9900 . ?
C9 H9AA 0.9900 . ?
C9 H9AB 0.9900 . ?
C9 O5A 1.436(4) . ?
C9 C10 1.348(6) . ?
C9 C9A 1.383(6) . ?
C9 O4 1.425(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
O2A C3 1.356(4) . ?
O2A C5A 1.413(6) . ?
O2 C5 1.335(6) . ?
O2 C4 1.428(6) . ?
C3 H3AA 0.9900 . ?
C3 H3AB 0.9900 . ?
C3 H3BC 0.9900 . ?
C3 H3BD 0.9900 . ?
C3 C4 1.418(6) . ?
C3 C3A 1.404(6) . ?
O3A C7A 1.440(5) . ?
O3A C6A 1.378(6) . ?
O5A C11A 1.434(6) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.324(10) . ?
C11A H11A 0.9900 . ?
C11A H11B 0.9900 . ?
C11A C12A 1.511(7) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.351(7) . ?
C7A H7AC 0.9900 . ?
C7A H7AD 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C11 1.502(8) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 O5 1.420(6) . ?
C9A H9AC 0.9900 . ?
C9A H9AD 0.9900 . ?
C12A H12C 0.9900 . ?
C12A H12D 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 O4 1.409(6) . ?
O5 C11 1.433(6) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C3A H3AC 0.9900 . ?
C3A H3AD 0.9900 . ?
C5A H5AA 0.9900 . ?
C5A H5AB 0.9900 . ?
C5A C6A 1.362(7) . ?
C13A H13C 0.9900 . ?
C13A H13D 0.9900 . ?
C13A C14A 1.326(9) . ?
C11 H11C 0.9900 . ?
C11 H11D 0.9900 . ?
C6A H6AA 0.9900 . ?
C6A H6AB 0.9900 . ?
C14A H14C 0.9900 . ?
C14A H14D 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S1 Ni1 S2 93.00(2) . . ?
S1 Ni1 S7 176.93(3) . . ?
S6 Ni1 S1 86.05(2) . . ?
S6 Ni1 S2 178.95(2) . . ?
S6 Ni1 S7 93.19(2) . . ?
S2 Ni1 S7 87.78(2) . . ?
C15 S1 Ni1 102.43(8) . . ?
C17 S4 C16 97.23(11) . . ?
C20 S9 C19 97.23(11) . . ?
C20 S8 C18 97.26(11) . . ?
C18 S6 Ni1 102.15(8) . . ?
C16 S2 Ni1 102.28(8) . . ?
C17 S3 C15 97.75(12) . . ?
C19 S7 Ni1 101.80(8) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
S7 C19 S9 122.71(14) . . ?
C18 C19 S9 116.10(18) . . ?
C18 C19 S7 121.19(17) . . ?
S2 C16 S4 122.85(14) . . ?
C15 C16 S4 115.99(17) . . ?
C15 C16 S2 121.15(18) . . ?
S6 C18 S8 122.32(14) . . ?
C19 C18 S8 116.27(17) . . ?
C19 C18 S6 121.41(18) . . ?
S3 C17 S4 113.16(13) . . ?
S5 C17 S4 123.57(16) . . ?
S5 C17 S3 123.28(15) . . ?
N1 C1 H1D 109.2 . . ?
N1 C1 H1E 109.2 . . ?
N1 C1 C2 112.23(19) . . ?
H1D C1 H1E 107.9 . . ?
C2 C1 H1D 109.2 . . ?
C2 C1 H1E 109.2 . . ?
S1 C15 S3 123.10(14) . . ?
C16 C15 S1 121.07(17) . . ?
C16 C15 S3 115.82(18) . . ?
S9 C20 S8 113.10(13) . . ?
S10 C20 S9 123.55(13) . . ?
S10 C20 S8 123.34(15) . . ?
H7BC C7 H7BD 107.7 . . ?
H7AA C7 H7AB 107.2 . . ?
O4A C7 H7BC 108.9 . . ?
O4A C7 H7BD 108.9 . . ?
O3 C7 H7AA 108.0 . . ?
O3 C7 H7AB 108.0 . . ?
O3 C7 C8 117.2(3) . . ?
C7A C7 H7BC 108.9 . . ?
C7A C7 H7BD 108.9 . . ?
C7A C7 O4A 113.3(3) . . ?
C8 C7 H7AA 108.0 . . ?
C8 C7 H7AB 108.0 . . ?
C9A O4A C7 115.5(4) . . ?
C14A O1A C3A 126.0(5) . . ?
C7 O3 C6 116.6(3) . . ?
C12 O6 C13 124.0(4) . . ?
C12A O6A C13A 111.8(4) . . ?
C3 O1 C14 118.1(4) . . ?
H9BC C9 H9BD 107.5 . . ?
H9AA C9 H9AB 107.2 . . ?
O5A C9 H9BC 108.4 . . ?
O5A C9 H9BD 108.4 . . ?
C10 C9 H9AA 108.0 . . ?
C10 C9 H9AB 108.0 . . ?
C10 C9 O4 117.3(3) . . ?
C9A C9 H9BC 108.4 . . ?
C9A C9 H9BD 108.4 . . ?
C9A C9 O5A 115.4(3) . . ?
O4 C9 H9AA 108.0 . . ?
O4 C9 H9AB 108.0 . . ?
Cl1 C2 H2A 109.1 . . ?
Cl1 C2 H2B 109.1 . . ?
C1 C2 Cl1 112.7(2) . . ?
C1 C2 H2A 109.1 . . ?
C1 C2 H2B 109.1 . . ?
H2A C2 H2B 107.8 . . ?
C3 O2A C5A 118.7(4) . . ?
C5 O2 C4 126.8(4) . . ?
O1 C3 H3AA 107.9 . . ?
O1 C3 H3AB 107.9 . . ?
O1 C3 C4 117.5(3) . . ?
O2A C3 H3BC 108.1 . . ?
O2A C3 H3BD 108.1 . . ?
O2A C3 C3A 116.9(3) . . ?
H3AA C3 H3AB 107.2 . . ?
H3BC C3 H3BD 107.3 . . ?
C4 C3 H3AA 107.9 . . ?
C4 C3 H3AB 107.9 . . ?
C3A C3 H3BC 108.1 . . ?
C3A C3 H3BD 108.1 . . ?
C6A O3A C7A 129.7(4) . . ?
C11A O5A C9 117.3(3) . . ?
O6 C13 H13A 107.5 . . ?
O6 C13 H13B 107.5 . . ?
H13A C13 H13B 107.0 . . ?
C14 C13 O6 119.1(6) . . ?
C14 C13 H13A 107.5 . . ?
C14 C13 H13B 107.5 . . ?
O5A C11A H11A 109.8 . . ?
O5A C11A H11B 109.8 . . ?
O5A C11A C12A 109.5(4) . . ?
H11A C11A H11B 108.2 . . ?
C12A C11A H11A 109.8 . . ?
C12A C11A H11B 109.8 . . ?
O2 C5 H5A 106.8 . . ?
O2 C5 H5B 106.8 . . ?
O2 C5 C6 122.3(4) . . ?
H5A C5 H5B 106.6 . . ?
C6 C5 H5A 106.8 . . ?
C6 C5 H5B 106.8 . . ?
C7 C7A O3A 114.7(4) . . ?
C7 C7A H7AC 108.6 . . ?
C7 C7A H7AD 108.6 . . ?
O3A C7A H7AC 108.6 . . ?
O3A C7A H7AD 108.6 . . ?
H7AC C7A H7AD 107.6 . . ?
O6 C12 H12A 110.0 . . ?
O6 C12 H12B 110.0 . . ?
O6 C12 C11 108.4(4) . . ?
H12A C12 H12B 108.4 . . ?
C11 C12 H12A 110.0 . . ?
C11 C12 H12B 110.0 . . ?
C9 C10 H10A 109.3 . . ?
C9 C10 H10B 109.3 . . ?
C9 C10 O5 111.4(4) . . ?
H10A C10 H10B 108.0 . . ?
O5 C10 H10A 109.3 . . ?
O5 C10 H10B 109.3 . . ?
O4A C9A H9AC 108.7 . . ?
O4A C9A H9AD 108.7 . . ?
C9 C9A O4A 114.3(5) . . ?
C9 C9A H9AC 108.7 . . ?
C9 C9A H9AD 108.7 . . ?
H9AC C9A H9AD 107.6 . . ?
O6A C12A C11A 108.0(4) . . ?
O6A C12A H12C 110.1 . . ?
O6A C12A H12D 110.1 . . ?
C11A C12A H12C 110.1 . . ?
C11A C12A H12D 110.1 . . ?
H12C C12A H12D 108.4 . . ?
O2 C4 H4A 109.0 . . ?
O2 C4 H4B 109.0 . . ?
C3 C4 O2 113.0(4) . . ?
C3 C4 H4A 109.0 . . ?
C3 C4 H4B 109.0 . . ?
H4A C4 H4B 107.8 . . ?
O1 C14 H14A 106.4 . . ?
O1 C14 H14B 106.4 . . ?
C13 C14 O1 123.9(6) . . ?
C13 C14 H14A 106.4 . . ?
C13 C14 H14B 106.4 . . ?
H14A C14 H14B 106.4 . . ?
C7 C8 H8A 109.3 . . ?
C7 C8 H8B 109.3 . . ?
C7 C8 O4 111.7(4) . . ?
H8A C8 H8B 108.0 . . ?
O4 C8 H8A 109.3 . . ?
O4 C8 H8B 109.3 . . ?
C10 O5 C11 111.7(4) . . ?
C8 O4 C9 119.5(4) . . ?
O3 C6 H6A 106.8 . . ?
O3 C6 H6B 106.8 . . ?
C5 C6 O3 122.2(4) . . ?
C5 C6 H6A 106.8 . . ?
C5 C6 H6B 106.8 . . ?
H6A C6 H6B 106.6 . . ?
O1A C3A H3AC 108.6 . . ?
O1A C3A H3AD 108.6 . . ?
C3 C3A O1A 114.5(4) . . ?
C3 C3A H3AC 108.6 . . ?
C3 C3A H3AD 108.6 . . ?
H3AC C3A H3AD 107.6 . . ?
O2A C5A H5AA 106.7 . . ?
O2A C5A H5AB 106.7 . . ?
H5AA C5A H5AB 106.6 . . ?
C6A C5A O2A 122.4(5) . . ?
C6A C5A H5AA 106.7 . . ?
C6A C5A H5AB 106.7 . . ?
O6A C13A H13C 108.0 . . ?
O6A C13A H13D 108.0 . . ?
H13C C13A H13D 107.2 . . ?
C14A C13A O6A 117.3(5) . . ?
C14A C13A H13C 108.0 . . ?
C14A C13A H13D 108.0 . . ?
C12 C11 H11C 109.9 . . ?
C12 C11 H11D 109.9 . . ?
O5 C11 C12 109.1(4) . . ?
O5 C11 H11C 109.9 . . ?
O5 C11 H11D 109.9 . . ?
H11C C11 H11D 108.3 . . ?
O3A C6A H6AA 107.4 . . ?
O3A C6A H6AB 107.4 . . ?
C5A C6A O3A 119.8(4) . . ?
C5A C6A H6AA 107.4 . . ?
C5A C6A H6AB 107.4 . . ?
H6AA C6A H6AB 106.9 . . ?
O1A C14A C13A 128.7(6) . . ?
O1A C14A H14C 105.1 . . ?
O1A C14A H14D 105.1 . . ?
C13A C14A H14C 105.1 . . ?
C13A C14A H14D 105.1 . . ?
H14C C14A H14D 105.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S1 C15 S3 -176.58(12) . . . . ?
Ni1 S1 C15 C16 2.6(2) . . . . ?
Ni1 S6 C18 S8 -177.34(12) . . . . ?
Ni1 S6 C18 C19 2.8(2) . . . . ?
Ni1 S2 C16 S4 179.33(12) . . . . ?
Ni1 S2 C16 C15 -0.1(2) . . . . ?
Ni1 S7 C19 S9 176.97(12) . . . . ?
Ni1 S7 C19 C18 -4.1(2) . . . . ?
S4 C16 C15 S1 178.72(12) . . . . ?
S4 C16 C15 S3 -2.0(2) . . . . ?
S9 C19 C18 S8 0.1(3) . . . . ?
S9 C19 C18 S6 179.91(12) . . . . ?
S2 C16 C15 S1 -1.8(3) . . . . ?
S2 C16 C15 S3 177.45(12) . . . . ?
S7 C19 C18 S8 -178.91(12) . . . . ?
S7 C19 C18 S6 0.9(3) . . . . ?
N1 C1 C2 Cl1 70.8(3) . . . . ?
C19 S9 C20 S8 1.85(15) . . . . ?
C19 S9 C20 S10 -177.56(16) . . . . ?
C16 S4 C17 S3 -1.75(15) . . . . ?
C16 S4 C17 S5 177.75(16) . . . . ?
C18 S8 C20 S9 -1.82(15) . . . . ?
C18 S8 C20 S10 177.60(16) . . . . ?
C17 S4 C16 S2 -177.17(15) . . . . ?
C17 S4 C16 C15 2.3(2) . . . . ?
C17 S3 C15 S1 179.92(15) . . . . ?
C17 S3 C15 C16 0.7(2) . . . . ?
C15 S3 C17 S4 0.89(15) . . . . ?
C15 S3 C17 S5 -178.61(16) . . . . ?
C20 S9 C19 S7 177.79(15) . . . . ?
C20 S9 C19 C18 -1.2(2) . . . . ?
C20 S8 C18 S6 -178.76(15) . . . . ?
C20 S8 C18 C19 1.1(2) . . . . ?
C7 O4A C9A C9 -173.0(3) . . . . ?
C7 O3 C6 C5 156.9(5) . . . . ?
C7 C8 O4 C9 175.7(3) . . . . ?
O4A C7 C7A O3A 54.0(5) . . . . ?
O3 C7 C8 O4 52.9(5) . . . . ?
O6 C13 C14 O1 -17.1(10) . . . . ?
O6 C12 C11 O5 63.1(6) . . . . ?
O6A C13A C14A O1A -12.9(11) . . . . ?
O1 C3 C4 O2 47.3(6) . . . . ?
C9 O5A C11A C12A -175.7(4) . . . . ?
C9 C10 O5 C11 178.3(4) . . . . ?
O2A C3 C3A O1A 49.4(6) . . . . ?
O2A C5A C6A O3A -2.9(9) . . . . ?
O2 C5 C6 O3 -2.6(9) . . . . ?
C3 O1 C14 C13 171.1(5) . . . . ?
C3 O2A C5A C6A 166.8(5) . . . . ?
O5A C9 C9A O4A -55.4(5) . . . . ?
O5A C11A C12A O6A 61.5(6) . . . . ?
C13 O6 C12 C11 142.6(6) . . . . ?
C5 O2 C4 C3 152.8(5) . . . . ?
C7A C7 O4A C9A -174.4(4) . . . . ?
C7A O3A C6A C5A 139.6(5) . . . . ?
C12 O6 C13 C14 154.8(6) . . . . ?
C10 C9 O4 C8 179.1(4) . . . . ?
C10 O5 C11 C12 -173.9(4) . . . . ?
C9A C9 O5A C11A 173.6(4) . . . . ?
C12A O6A C13A C14A 154.9(6) . . . . ?
C4 O2 C5 C6 153.5(6) . . . . ?
C14 O1 C3 C4 -165.0(4) . . . . ?
C8 C7 O3 C6 -176.8(4) . . . . ?
O4 C9 C10 O5 -56.3(5) . . . . ?
C3A O1A C14A C13A 156.9(7) . . . . ?
C5A O2A C3 C3A -173.3(4) . . . . ?
C13A O6A C12A C11A 167.3(4) . . . . ?
C6A O3A C7A C7 150.3(5) . . . . ?
C14A O1A C3A C3 166.5(5) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.420
_oxdiff_exptl_absorpt_empirical_full_min 0.405
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_353k-f
_database_code_depnum_ccdc_archive 'CCDC 2053403'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-18 downloaded from the CCDC.
;
_audit_creation_date             2020-11-24
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C2 H7 Cl N, C12 H24 O6'
_chemical_formula_sum            'C20 H31 Cl N Ni O6 S10'
_chemical_formula_weight         796.22
_chemical_melting_point          ?
_chemical_oxdiff_formula         C20H30NO6NiS10Cl
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.3244(5)
_cell_length_b                   12.3495(4)
_cell_length_c                   12.9385(6)
_cell_angle_alpha                90.918(3)
_cell_angle_beta                 110.128(4)
_cell_angle_gamma                96.018(3)
_cell_volume                     1686.95(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    13011
_cell_measurement_temperature    353
_cell_measurement_theta_max      28.7530
_cell_measurement_theta_min      1.7150
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.308
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45184
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             822
_exptl_crystal_size_max          0.69
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0904
_diffrn_reflns_av_unetI/netI     0.0637
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.879
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30129
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.879
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.212
_diffrn_reflns_theta_min         1.929
_diffrn_ambient_temperature      353
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.879
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -40.00 101.00   0.50    0.53    --   21.85  37.00-150.00  282
  2  ω    -24.00 103.00   0.50    0.53    --   21.85  19.00 -30.00  254
  3  ω    -21.00 104.00   0.50    0.53    --   21.85  57.00  30.00  250
  4  ω    -26.00 103.00   0.50    0.53    --   21.85  77.00 150.00  258
  5  ω    -25.00  52.00   0.50    0.53    --  -21.77  19.00 120.00  154
  6  ω     35.00  60.00   0.50    0.53    --  -21.77  19.00-180.00   50
  7  ω    -13.00  29.00   0.50    0.53    --  -21.77  19.00-180.00   84
  8  ω    -51.00 -13.00   0.50    0.53    --  -21.77 111.00-128.00   76
  9  ω    -68.00  44.00   0.50    0.53    --   21.85 -37.00-180.00  224
 10  ω     32.00  74.00   0.50    0.53    --   21.85-111.00 137.00   84
 11  ω     46.00 104.00   0.50    0.53    --   21.85 178.00  60.00  116
 12  ω     49.00  86.00   0.50    0.53    --   21.85 178.00  90.00   74
 13  ω     67.00 104.00   0.50    0.53    --   21.85-178.00-180.00   74
 14  ω    -16.00  37.00   0.50    0.53    --  -21.77 -99.00-180.00  106
 15  ω    -18.00  29.00   0.50    0.53    --  -21.77 -99.00 -60.00   94
 16  ω   -125.00 -90.00   0.50    0.53    --  -21.77-178.00 150.00   70
 17  ω    -70.00 -43.00   0.50    0.53    --  -21.77-178.00 150.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0195204000
_diffrn_orient_matrix_UB_12      -0.0564985000
_diffrn_orient_matrix_UB_13      -0.0001067000
_diffrn_orient_matrix_UB_21      -0.0161082000
_diffrn_orient_matrix_UB_22      -0.0045170000
_diffrn_orient_matrix_UB_23      -0.0580707000
_diffrn_orient_matrix_UB_31      0.0622248000
_diffrn_orient_matrix_UB_32      -0.0115525000
_diffrn_orient_matrix_UB_33      0.0068877000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4632
_reflns_number_total             8054
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT n/a (Sheldrick, 2015)'
_refine_diff_density_max         0.779
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.916
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         8054
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_gt           0.0559
_refine_ls_restrained_S_all      0.916
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1221P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1553
_refine_ls_wR_factor_ref         0.1910
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
2. Rigid body (RIGU) restrains
 O3, C9, C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11, C10A, O4A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(Cl1A)=Sof(H1d)=Sof(H1e)=Sof(C2A)=Sof(H2Aa)=Sof(H2Ab)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(Cl1)=FVAR(1)
 Sof(H3a)=Sof(H3b)=Sof(O5A)=Sof(O4A)=Sof(C10A)=Sof(H10c)=Sof(H10d)=Sof(C9A)=
 Sof(H9Aa)=Sof(H9Ab)=Sof(H11c)=Sof(H11d)=Sof(C8A)=Sof(H8Aa)=Sof(H8Ab)=Sof(O3A)=
 Sof(C12A)=Sof(H12c)=Sof(H12d)=Sof(C13A)=Sof(H13c)=Sof(H13d)=Sof(C6A)=Sof(H6Aa)=
 Sof(H6Ab)=Sof(O6A)=Sof(O2A)=Sof(C14A)=Sof(H14c)=Sof(H14d)=Sof(C4A)=Sof(H4Aa)=
 Sof(H4Ab)=Sof(C5A)=Sof(H5Aa)=Sof(H5Ab)=Sof(O1A)=Sof(C7A)=Sof(H7Aa)=Sof(H7Ab)=1-
 FVAR(2)
 Sof(O4)=Sof(O1)=Sof(O3)=Sof(O6)=Sof(H3AA)=Sof(H3AB)=Sof(O5)=Sof(O2)=Sof(C9)=
 Sof(H9A)=Sof(H9B)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C13)=Sof(H13A)=Sof(H13B)=
 Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C7)=Sof(H7A)=
 Sof(H7B)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C8)=
 Sof(H8A)=Sof(H8B)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H11A)=Sof(H11B)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1AA,H1AB), C1(H1d,H1e), C3(H3AA,H3AB), C3(H3a,H3b), C9(H9A,H9B), C5(H5A,
 H5B), C13(H13A,H13B), C14(H14A,H14B), C4(H4A,H4B), C7(H7A,H7B), C2(H2A,H2B),
 C12(H12A,H12B), C6(H6A,H6B), C2A(H2Aa,H2Ab), C8(H8A,H8B), C10(H10A,H10B),
 C10A(H10c,H10d), C9A(H9Aa,H9Ab), C11(H11A,H11B), C11(H11c,H11d), C8A(H8Aa,
 H8Ab), C12A(H12c,H12d), C13A(H13c,H13d), C6A(H6Aa,H6Ab), C14A(H14c,H14d),
 C4A(H4Aa,H4Ab), C5A(H5Aa,H5Ab), C7A(H7Aa,H7Ab)
4.b Idealised Me refined as rotating group:
 N1(H1a,H1b,H1c)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.84510(3) 0.88980(3) 0.51194(4) 0.06033(18) Uani 1 1 d . . . . .
S6 S 0.69191(8) 0.97485(8) 0.52333(8) 0.0728(3) Uani 1 1 d . . . . .
S2 S 1.00509(8) 0.81276(8) 0.50579(9) 0.0740(3) Uani 1 1 d . . . . .
S1 S 0.78907(9) 0.92743(8) 0.34046(9) 0.0744(3) Uani 1 1 d . . . . .
S7 S 0.89929(9) 0.84571(9) 0.68135(9) 0.0770(3) Uani 1 1 d . . . . .
S8 S 0.61310(8) 1.02438(8) 0.71984(9) 0.0732(3) Uani 1 1 d . . . . .
S9 S 0.80114(9) 0.90250(9) 0.86309(9) 0.0802(3) Uani 1 1 d . . . . .
S4 S 1.09874(9) 0.77236(9) 0.31758(10) 0.0804(3) Uani 1 1 d . . . . .
S3 S 0.90608(10) 0.88462(9) 0.16707(9) 0.0815(3) Uani 1 1 d . . . . .
S10 S 0.62539(11) 1.00236(10) 0.95148(10) 0.0936(4) Uani 1 1 d . . . . .
S5 S 1.08868(11) 0.78591(12) 0.08622(11) 0.1005(4) Uani 1 1 d . . . . .
Cl1A Cl 0.8267(12) 0.4517(8) 0.5251(9) 0.103(2) Uani 0.348(11) 1 d . . P A 2
N1 N 0.6669(3) 0.5024(2) 0.2575(3) 0.0713(8) Uani 1 1 d . . . . .
H1A H 0.660872 0.517406 0.188962 0.086 Uiso 1 1 calc R U . . .
H1B H 0.592505 0.506456 0.265619 0.086 Uiso 1 1 calc R U . . .
H1C H 0.688622 0.435418 0.270603 0.086 Uiso 1 1 calc R U . . .
C18 C 0.7081(3) 0.9647(3) 0.6589(3) 0.0624(8) Uani 1 1 d . . . . .
C19 C 0.7985(3) 0.9080(3) 0.7288(3) 0.0644(8) Uani 1 1 d . . . . .
C15 C 0.9019(3) 0.8752(3) 0.2992(3) 0.0652(8) Uani 1 1 d . . . . .
C17 C 1.0336(3) 0.8127(3) 0.1842(3) 0.0734(9) Uani 1 1 d . . . . .
C20 C 0.6768(3) 0.9780(3) 0.8502(3) 0.0706(9) Uani 1 1 d . . . . .
C16 C 0.9949(3) 0.8242(3) 0.3726(3) 0.0667(9) Uani 1 1 d . . . . .
O4 O 0.7044(9) 0.6183(7) 0.0781(8) 0.091(2) Uani 0.516(9) 1 d . . P B 1
O1 O 0.5104(8) 0.3200(7) 0.3183(10) 0.096(3) Uani 0.516(9) 1 d . . P B 1
O3 O 0.4941(8) 0.6520(7) 0.1426(9) 0.094(2) Uani 0.516(9) 1 d . . P B 1
O6 O 0.7210(6) 0.2822(6) 0.2645(7) 0.081(2) Uani 0.516(9) 1 d . . P B 1
C1 C 0.7643(5) 0.5820(4) 0.3362(4) 0.1009(15) Uani 1 1 d . . . . .
H1AA H 0.846796 0.571257 0.333526 0.121 Uiso 0.652(11) 1 calc R U P A 1
H1AB H 0.747637 0.655284 0.314370 0.121 Uiso 0.652(11) 1 calc R U P A 1
H1D H 0.802935 0.630844 0.295805 0.121 Uiso 0.348(11) 1 calc R U P A 2
H1E H 0.724118 0.625478 0.374709 0.121 Uiso 0.348(11) 1 calc R U P A 2
C3 C 0.6471(5) 0.2044(4) 0.3033(7) 0.124(2) Uani 1 1 d . . . . .
H3AA H 0.583918 0.164328 0.239716 0.149 Uiso 0.516(9) 1 calc R U P B 1
H3AB H 0.702004 0.152705 0.344182 0.149 Uiso 0.516(9) 1 calc R U P B 1
H3A H 0.713587 0.213537 0.375151 0.149 Uiso 0.484(9) 1 calc R U P B 2
H3B H 0.599574 0.133355 0.299088 0.149 Uiso 0.484(9) 1 calc R U P B 2
O5 O 0.7878(9) 0.4148(8) 0.1173(7) 0.099(2) Uani 0.516(9) 1 d . . P B 1
O2 O 0.4318(10) 0.5278(9) 0.2999(10) 0.110(3) Uani 0.516(9) 1 d . . P B 1
C9 C 0.552(2) 0.7334(14) 0.0961(17) 0.098(5) Uani 0.516(9) 1 d . . P B 1
H9A H 0.620671 0.776612 0.153343 0.117 Uiso 0.516(9) 1 calc R U P B 1
H9B H 0.491118 0.781432 0.056622 0.117 Uiso 0.516(9) 1 calc R U P B 1
C5 C 0.429(3) 0.359(3) 0.363(2) 0.148(14) Uani 0.516(9) 1 d . . P B 1
H5A H 0.375617 0.296046 0.372926 0.177 Uiso 0.516(9) 1 calc R U P B 1
H5B H 0.479788 0.389991 0.436027 0.177 Uiso 0.516(9) 1 calc R U P B 1
C13 C 0.8654(13) 0.3403(12) 0.1731(16) 0.093(4) Uani 0.516(9) 1 d . . P B 1
H13A H 0.925668 0.373420 0.242176 0.111 Uiso 0.516(9) 1 calc R U P B 1
H13B H 0.911831 0.314123 0.129148 0.111 Uiso 0.516(9) 1 calc R U P B 1
C14 C 0.7784(10) 0.2460(11) 0.1947(10) 0.083(3) Uani 0.516(9) 1 d . . P B 1
H14A H 0.714456 0.217327 0.125541 0.100 Uiso 0.516(9) 1 calc R U P B 1
H14B H 0.827748 0.187698 0.227477 0.100 Uiso 0.516(9) 1 calc R U P B 1
C4 C 0.5887(11) 0.2406(8) 0.3659(14) 0.105(4) Uani 0.516(9) 1 d . . P B 1
H4A H 0.651399 0.270953 0.434974 0.126 Uiso 0.516(9) 1 calc R U P B 1
H4B H 0.537942 0.179714 0.382421 0.126 Uiso 0.516(9) 1 calc R U P B 1
C7 C 0.356(2) 0.605(2) 0.242(2) 0.121(6) Uani 0.516(9) 1 d . . P B 1
H7A H 0.312890 0.634847 0.287288 0.145 Uiso 0.516(9) 1 calc R U P B 1
H7B H 0.292106 0.570235 0.175541 0.145 Uiso 0.516(9) 1 calc R U P B 1
C2 C 0.7662(9) 0.5713(6) 0.4490(7) 0.109(3) Uani 0.652(11) 1 d . . P A 1
H2A H 0.679863 0.566662 0.448335 0.131 Uiso 0.652(11) 1 calc R U P A 1
H2B H 0.812425 0.636732 0.492846 0.131 Uiso 0.652(11) 1 calc R U P A 1
C12 C 0.8557(15) 0.5036(13) 0.0829(11) 0.116(4) Uani 0.516(9) 1 d . . P B 1
H12A H 0.921062 0.540003 0.147481 0.140 Uiso 0.516(9) 1 calc R U P B 1
H12B H 0.897153 0.474391 0.036154 0.140 Uiso 0.516(9) 1 calc R U P B 1
C6 C 0.3544(11) 0.4304(14) 0.3138(13) 0.108(4) Uani 0.516(9) 1 d . . P B 1
H6A H 0.304569 0.449258 0.357750 0.130 Uiso 0.516(9) 1 calc R U P B 1
H6B H 0.296931 0.400108 0.242432 0.130 Uiso 0.516(9) 1 calc R U P B 1
C2A C 0.8589(12) 0.5307(13) 0.4137(13) 0.109(6) Uani 0.348(11) 1 d . . P A 2
H2AA H 0.928550 0.586797 0.449721 0.131 Uiso 0.348(11) 1 calc R U P A 2
H2AB H 0.889821 0.481432 0.372423 0.131 Uiso 0.348(11) 1 calc R U P A 2
C8 C 0.4391(13) 0.6961(12) 0.2125(16) 0.110(5) Uani 0.516(9) 1 d . . P B 1
H8A H 0.388098 0.752114 0.176030 0.132 Uiso 0.516(9) 1 calc R U P B 1
H8B H 0.504531 0.729067 0.278862 0.132 Uiso 0.516(9) 1 calc R U P B 1
C10 C 0.6019(16) 0.6782(10) 0.0188(14) 0.108(4) Uani 0.516(9) 1 d . . P B 1
H10A H 0.534309 0.628761 -0.032728 0.129 Uiso 0.516(9) 1 calc R U P B 1
H10B H 0.631322 0.732364 -0.023021 0.129 Uiso 0.516(9) 1 calc R U P B 1
O5A O 0.7751(8) 0.4730(9) 0.0812(8) 0.101(3) Uani 0.484(9) 1 d . . P B 2
O4A O 0.6472(11) 0.6517(8) 0.0881(9) 0.096(3) Uani 0.484(9) 1 d . . P B 2
C10A C 0.695(2) 0.6331(13) 0.0042(15) 0.130(5) Uani 0.484(9) 1 d . . P B 2
H10C H 0.626375 0.598030 -0.059227 0.156 Uiso 0.484(9) 1 calc R U P B 2
H10D H 0.723595 0.702917 -0.017558 0.156 Uiso 0.484(9) 1 calc R U P B 2
C9A C 0.533(2) 0.7040(16) 0.0483(14) 0.095(5) Uani 0.484(9) 1 d . . P B 2
H9AA H 0.467437 0.655894 -0.006447 0.114 Uiso 0.484(9) 1 calc R U P B 2
H9AB H 0.549274 0.770229 0.013578 0.114 Uiso 0.484(9) 1 calc R U P B 2
C11 C 0.7848(9) 0.5750(6) 0.0298(7) 0.156(3) Uani 1 1 d . . . . .
H11A H 0.732432 0.541742 -0.042069 0.187 Uiso 0.516(9) 1 calc R U P B 1
H11B H 0.839648 0.635308 0.017549 0.187 Uiso 0.516(9) 1 calc R U P B 1
H11C H 0.859133 0.619808 0.078694 0.187 Uiso 0.484(9) 1 calc R U P B 2
H11D H 0.801633 0.558768 -0.037096 0.187 Uiso 0.484(9) 1 calc R U P B 2
C8A C 0.4912(15) 0.7303(13) 0.1400(15) 0.117(5) Uani 0.484(9) 1 d . . P B 2
H8AA H 0.558675 0.774996 0.196824 0.140 Uiso 0.484(9) 1 calc R U P B 2
H8AB H 0.418809 0.771129 0.114115 0.140 Uiso 0.484(9) 1 calc R U P B 2
O3A O 0.4579(10) 0.6333(8) 0.1833(9) 0.092(2) Uani 0.484(9) 1 d . . P B 2
C12A C 0.8738(14) 0.4098(15) 0.1215(12) 0.120(5) Uani 0.484(9) 1 d . . P B 2
H12C H 0.934085 0.443291 0.190292 0.144 Uiso 0.484(9) 1 calc R U P B 2
H12D H 0.917324 0.405010 0.069124 0.144 Uiso 0.484(9) 1 calc R U P B 2
C13A C 0.8215(15) 0.2954(13) 0.1405(16) 0.092(4) Uani 0.484(9) 1 d . . P B 2
H13C H 0.760461 0.261731 0.072103 0.111 Uiso 0.484(9) 1 calc R U P B 2
H13D H 0.889679 0.250052 0.166653 0.111 Uiso 0.484(9) 1 calc R U P B 2
C6A C 0.3583(17) 0.542(2) 0.2978(14) 0.130(7) Uani 0.484(9) 1 d . . P B 2
H6AA H 0.324008 0.553444 0.355816 0.156 Uiso 0.484(9) 1 calc R U P B 2
H6AB H 0.289833 0.509265 0.233357 0.156 Uiso 0.484(9) 1 calc R U P B 2
O6A O 0.7642(9) 0.3051(7) 0.2181(8) 0.091(2) Uani 0.484(9) 1 d . . P B 2
O2A O 0.4517(10) 0.4722(10) 0.3323(9) 0.108(3) Uani 0.484(9) 1 d . . P B 2
C14A C 0.7004(12) 0.2040(10) 0.2283(11) 0.098(3) Uani 0.484(9) 1 d . . P B 2
H14C H 0.635609 0.181000 0.157634 0.118 Uiso 0.484(9) 1 calc R U P B 2
H14D H 0.760198 0.150496 0.245689 0.118 Uiso 0.484(9) 1 calc R U P B 2
C4A C 0.508(2) 0.2960(16) 0.3820(18) 0.133(10) Uani 0.484(9) 1 d . . P B 2
H4AA H 0.474544 0.223529 0.393986 0.160 Uiso 0.484(9) 1 calc R U P B 2
H4AB H 0.574029 0.324450 0.450040 0.160 Uiso 0.484(9) 1 calc R U P B 2
C5A C 0.418(2) 0.359(2) 0.357(3) 0.189(16) Uani 0.484(9) 1 d . . P B 2
H5AA H 0.386473 0.361463 0.417916 0.227 Uiso 0.484(9) 1 calc R U P B 2
H5AB H 0.348644 0.324955 0.293414 0.227 Uiso 0.484(9) 1 calc R U P B 2
O1A O 0.5602(9) 0.2894(9) 0.2966(8) 0.095(3) Uani 0.484(9) 1 d . . P B 2
C7A C 0.412(2) 0.653(2) 0.270(2) 0.119(7) Uani 0.484(9) 1 d . . P B 2
H7AA H 0.346565 0.701438 0.246651 0.142 Uiso 0.484(9) 1 calc R U P B 2
H7AB H 0.480339 0.687522 0.333691 0.142 Uiso 0.484(9) 1 calc R U P B 2
Cl1 Cl 0.8287(7) 0.4679(6) 0.5071(6) 0.153(2) Uani 0.652(11) 1 d . . P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S6 2.1651(9) . ?
Ni1 S2 2.1570(9) . ?
Ni1 S1 2.1603(11) . ?
Ni1 S7 2.1588(11) . ?
S6 C18 1.708(4) . ?
S2 C16 1.696(4) . ?
S1 C15 1.722(3) . ?
S7 C19 1.710(3) . ?
S8 C18 1.747(3) . ?
S8 C20 1.725(4) . ?
S9 C19 1.730(4) . ?
S9 C20 1.732(3) . ?
S4 C17 1.732(4) . ?
S4 C16 1.738(3) . ?
S3 C15 1.732(4) . ?
S3 C17 1.725(4) . ?
S10 C20 1.642(4) . ?
S5 C17 1.637(4) . ?
Cl1A C2A 1.869(17) . ?
N1 C1 1.479(5) . ?
C18 C19 1.374(5) . ?
C15 C16 1.370(5) . ?
O4 C10 1.44(2) . ?
O4 C11 1.411(13) . ?
O1 C5 1.36(4) . ?
O1 C4 1.397(17) . ?
O3 C9 1.40(2) . ?
O3 C8 1.39(2) . ?
O6 C3 1.419(9) . ?
O6 C14 1.374(15) . ?
C1 C2 1.460(9) . ?
C1 C2A 1.407(14) . ?
C3 C4 1.308(16) . ?
C3 C14A 1.307(15) . ?
C3 O1A 1.496(13) . ?
O5 C13 1.375(18) . ?
O5 C12 1.438(17) . ?
O2 C7 1.40(3) . ?
O2 C6 1.46(2) . ?
C9 C10 1.49(3) . ?
C5 C6 1.31(3) . ?
C13 C14 1.538(17) . ?
C7 C8 1.53(3) . ?
C2 Cl1 1.597(10) . ?
C12 C11 1.297(16) . ?
O5A C11 1.445(13) . ?
O5A C12A 1.39(2) . ?
O4A C10A 1.393(19) . ?
O4A C9A 1.44(2) . ?
C10A C11 1.26(2) . ?
C9A C8A 1.47(3) . ?
C8A O3A 1.401(19) . ?
O3A C7A 1.41(3) . ?
C12A C13A 1.53(2) . ?
C13A O6A 1.38(2) . ?
C6A O2A 1.40(3) . ?
C6A C7A 1.54(3) . ?
O6A C14A 1.407(17) . ?
O2A C5A 1.48(3) . ?
C4A C5A 1.30(4) . ?
C4A O1A 1.43(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S2 Ni1 S6 176.77(4) . . ?
S2 Ni1 S1 92.88(4) . . ?
S2 Ni1 S7 86.27(4) . . ?
S1 Ni1 S6 88.04(3) . . ?
S7 Ni1 S6 92.92(4) . . ?
S7 Ni1 S1 177.83(4) . . ?
C18 S6 Ni1 102.08(11) . . ?
C16 S2 Ni1 102.63(12) . . ?
C15 S1 Ni1 102.57(13) . . ?
C19 S7 Ni1 102.84(12) . . ?
C20 S8 C18 98.14(16) . . ?
C19 S9 C20 97.86(17) . . ?
C17 S4 C16 98.33(18) . . ?
C17 S3 C15 97.57(18) . . ?
S6 C18 S8 123.44(19) . . ?
C19 C18 S6 121.7(3) . . ?
C19 C18 S8 114.8(3) . . ?
S7 C19 S9 123.31(19) . . ?
C18 C19 S7 120.3(3) . . ?
C18 C19 S9 116.4(3) . . ?
S1 C15 S3 123.1(2) . . ?
C16 C15 S1 120.0(3) . . ?
C16 C15 S3 116.9(3) . . ?
S3 C17 S4 112.6(2) . . ?
S5 C17 S4 123.2(2) . . ?
S5 C17 S3 124.2(2) . . ?
S8 C20 S9 112.7(2) . . ?
S10 C20 S8 123.8(2) . . ?
S10 C20 S9 123.4(2) . . ?
S2 C16 S4 123.5(2) . . ?
C15 C16 S2 121.9(3) . . ?
C15 C16 S4 114.6(3) . . ?
C11 O4 C10 123.4(11) . . ?
C5 O1 C4 123.3(19) . . ?
C8 O3 C9 111.7(13) . . ?
C14 O6 C3 118.3(9) . . ?
C2 C1 N1 112.0(4) . . ?
C2A C1 N1 112.0(7) . . ?
C4 C3 O6 117.6(7) . . ?
C14A C3 O1A 116.5(7) . . ?
C13 O5 C12 112.5(12) . . ?
C7 O2 C6 111.0(15) . . ?
O3 C9 C10 107.4(13) . . ?
C6 C5 O1 121(2) . . ?
O5 C13 C14 106.4(10) . . ?
O6 C14 C13 109.9(12) . . ?
C3 C4 O1 113.7(16) . . ?
O2 C7 C8 109.2(16) . . ?
C1 C2 Cl1 114.4(7) . . ?
C11 C12 O5 113.9(14) . . ?
C5 C6 O2 108.8(15) . . ?
C1 C2A Cl1A 121.7(10) . . ?
O3 C8 C7 108.9(13) . . ?
O4 C10 C9 110.9(16) . . ?
C12A O5A C11 124.3(13) . . ?
C10A O4A C9A 111.2(16) . . ?
C11 C10A O4A 114.4(18) . . ?
O4A C9A C8A 110.0(13) . . ?
C12 C11 O4 117.9(8) . . ?
C10A C11 O5A 120.7(9) . . ?
O3A C8A C9A 109.1(15) . . ?
C8A O3A C7A 111.8(17) . . ?
O5A C12A C13A 109.6(14) . . ?
O6A C13A C12A 108.0(12) . . ?
O2A C6A C7A 111.1(15) . . ?
C13A O6A C14A 110.3(14) . . ?
C6A O2A C5A 119.8(15) . . ?
C3 C14A O6A 114.7(13) . . ?
C5A C4A O1A 111(2) . . ?
C4A C5A O2A 116.4(14) . . ?
C4A O1A C3 117.5(12) . . ?
O3A C7A C6A 107.4(16) . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.183
_oxdiff_exptl_absorpt_empirical_full_min 0.343
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_333k
_database_code_depnum_ccdc_archive 'CCDC 2053310'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-18 downloaded from the CCDC.
;
_audit_creation_date             2020-11-10
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C2 H7 Br N, C12 H24 O6'
_chemical_formula_sum            'C20 H31 Br N Ni O6 S10'
_chemical_formula_weight         840.68
_chemical_melting_point          ?
_chemical_oxdiff_formula         BrCHNONiS
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.1865(5)
_cell_length_b                   12.1459(5)
_cell_length_c                   13.7395(6)
_cell_angle_alpha                65.630(4)
_cell_angle_beta                 81.204(4)
_cell_angle_gamma                78.269(4)
_cell_volume                     1659.95(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    13915
_cell_measurement_temperature    333
_cell_measurement_theta_max      28.5810
_cell_measurement_theta_min      1.8750
_shelx_estimated_absorpt_T_max   0.847
_shelx_estimated_absorpt_T_min   0.440
_exptl_absorpt_coefficient_mu    2.452
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36099
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             858
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0896
_diffrn_reflns_av_unetI/netI     0.0734
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.887
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            34340
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.887
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.036
_diffrn_reflns_theta_min         1.865
_diffrn_ambient_temperature      333
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.887
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -25.00 103.00   0.50    1.27    --   21.69  19.00  30.00  256
  2  ω     46.00  91.00   0.50    1.27    --   21.69 178.00 150.00   90
  3  ω     69.00 102.00   0.50    1.27    --   21.69 160.00-118.00   66
  4  ω    -40.00 103.00   0.50    1.27    --   21.69  37.00-120.00  286
  5  ω    -25.00  55.00   0.50    1.27    --  -21.62  19.00-120.00  160
  6  ω    -72.00  -9.00   0.50    1.27    --  -21.62 117.00  90.00  126
  7  ω   -116.00 -59.00   0.50    1.27    --  -21.62 160.00-118.00  114
  8  ω    -24.00  60.00   0.50    1.27    --  -21.62  19.00 -30.00  168
  9  ω    -33.00  40.00   0.50    1.27    --   21.69 -37.00-180.00  146
 10  ω    -17.00  37.00   0.50    1.27    --  -21.62 -99.00-180.00  108
 11  ω     61.00  87.00   0.50    1.27    --   21.69-160.00-148.00   52
 12  ω     18.00  72.00   0.50    1.27    --   21.69-117.00   2.00  108
 13  ω   -105.00  18.00   0.50    1.27    --  -21.62 -57.00  90.00  246
 14  ω    -18.00  38.00   0.50    1.27    --  -21.62 -99.00 -30.00  112
 15  ω   -109.00  44.00   0.50    1.27    --  -21.62 -37.00-150.00  306
 16  ω    -88.00 -62.00   0.50    1.27    --  -21.62-160.00-148.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0294740000
_diffrn_orient_matrix_UB_12      0.0065210000
_diffrn_orient_matrix_UB_13      0.0390777000
_diffrn_orient_matrix_UB_21      -0.0246049000
_diffrn_orient_matrix_UB_22      -0.0506875000
_diffrn_orient_matrix_UB_23      0.0404065000
_diffrn_orient_matrix_UB_31      0.0523921000
_diffrn_orient_matrix_UB_32      -0.0400075000
_diffrn_orient_matrix_UB_33      -0.0084612000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4844
_reflns_number_total             7868
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT n/a (Sheldrick, 2015)'
_refine_diff_density_max         0.512
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         7868
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0450
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0466P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1248
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C1A \\sim N1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
C1 \\sim C2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
3. Others
 1*[Sof(Br1)]+1*[Sof(Br1B)]+1*[Sof(Br1A)]=1 with esd of 0.0001
 Sof(H1BD)=Sof(H1BE)=Sof(H1BF)=Sof(C1A)=Sof(H1AD)=Sof(H1AE)=Sof(C2A)=Sof(H2AA)=
 Sof(H2AB)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=
 Sof(H2B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C8(H8A,H8B), C11(H11A,H11B), C12(H12A,H12B), C9(H9A,H9B),
 C14(H14A,H14B), C3(H3A,H3B), C13(H13A,H13B), C7(H7A,H7B), C4(H4A,H4B), C6(H6A,
 H6B), C5(H5A,H5B), C1A(H1AD,H1AE), C1(H1A,H1B), C2(H2A,H2B), C2A(H2AA,H2AB)
4.b Idealised Me refined as rotating group:
 N1(H1BD,H1BE,H1BF), N1(H1AA,H1AB,H1AC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.13341(3) 0.46400(3) 0.88309(3) 0.04421(13) Uani 1 1 d . . . . .
S1 S 0.09996(7) 0.33940(7) 0.81746(6) 0.0494(2) Uani 1 1 d . . . . .
S3 S 0.20733(7) 0.07281(7) 0.86682(7) 0.0519(2) Uani 1 1 d . . . . .
S9 S 0.05427(7) 0.84293(7) 0.92129(7) 0.0533(2) Uani 1 1 d . . . . .
S4 S 0.35659(7) 0.06315(7) 1.02448(7) 0.0515(2) Uani 1 1 d . . . . .
S2 S 0.26451(7) 0.32811(7) 0.98869(7) 0.0544(2) Uani 1 1 d . . . . .
S7 S 0.15999(8) 0.58078(7) 0.95830(7) 0.0560(2) Uani 1 1 d . . . . .
S6 S 0.01182(8) 0.60754(7) 0.77162(7) 0.0579(2) Uani 1 1 d . . . . .
S8 S -0.07949(8) 0.87085(8) 0.74700(8) 0.0654(3) Uani 1 1 d . . . . .
S5 S 0.36374(9) -0.16204(7) 0.98824(8) 0.0679(3) Uani 1 1 d . . . . .
S10 S -0.09579(9) 1.08215(8) 0.80843(9) 0.0746(3) Uani 1 1 d . . . . .
Br1A Br 0.07788(9) 0.14509(11) 0.54001(13) 0.0916(4) Uani 0.562(2) 1 d . . P A
3
O5 O 0.3594(2) 0.3937(2) 0.61845(18) 0.0659(6) Uani 1 1 d . . . . .
O6 O 0.5665(2) 0.2209(2) 0.62428(19) 0.0707(7) Uani 1 1 d . . . . .
O4 O 0.2565(2) 0.5349(2) 0.4213(2) 0.0736(7) Uani 1 1 d . . . . .
O1 O 0.6415(2) 0.1420(2) 0.4568(2) 0.0779(7) Uani 1 1 d . . . . .
N1 N 0.3984(2) 0.2929(3) 0.4591(2) 0.0597(7) Uani 1 1 d . U . . .
H1BD H 0.417022 0.287650 0.395611 0.072 Uiso 0.391(13) 1 calc R U P B 2
H1BE H 0.467055 0.283371 0.488922 0.072 Uiso 0.391(13) 1 calc R U P B 2
H1BF H 0.354927 0.365871 0.450348 0.072 Uiso 0.391(13) 1 calc R U P B 2
H1AA H 0.373560 0.362731 0.405346 0.072 Uiso 0.609(13) 1 calc R U P B 1
H1AB H 0.476812 0.266701 0.445101 0.072 Uiso 0.609(13) 1 calc R U P B 1
H1AC H 0.389903 0.305108 0.519480 0.072 Uiso 0.609(13) 1 calc R U P B 1
O3 O 0.3224(2) 0.4669(3) 0.2533(2) 0.0853(8) Uani 1 1 d . . . . .
O2 O 0.5423(3) 0.3061(3) 0.2632(2) 0.1017(11) Uani 1 1 d . . . . .
C19 C 0.0701(2) 0.7150(2) 0.8898(2) 0.0440(7) Uani 1 1 d . . . . .
C15 C 0.1969(2) 0.2087(2) 0.8850(2) 0.0419(7) Uani 1 1 d . . . . .
C16 C 0.2673(2) 0.2031(2) 0.9596(2) 0.0435(7) Uani 1 1 d . . . . .
C18 C 0.0063(3) 0.7269(3) 0.8089(3) 0.0509(8) Uani 1 1 d . . . . .
C20 C -0.0432(3) 0.9394(3) 0.8248(3) 0.0537(8) Uani 1 1 d . . . . .
C17 C 0.3116(3) -0.0158(3) 0.9613(2) 0.0480(7) Uani 1 1 d . . . . .
C10 C 0.3029(4) 0.5177(3) 0.5880(3) 0.0737(11) Uani 1 1 d . . . . .
H10A H 0.363168 0.571174 0.549690 0.088 Uiso 1 1 calc R U . . .
H10B H 0.270155 0.533270 0.651479 0.088 Uiso 1 1 calc R U . . .
C8 C 0.1768(3) 0.5718(4) 0.3416(3) 0.0812(12) Uani 1 1 d . . . . .
H8A H 0.130665 0.651795 0.332523 0.097 Uiso 1 1 calc R U . . .
H8B H 0.119236 0.514587 0.362538 0.097 Uiso 1 1 calc R U . . .
C11 C 0.4477(3) 0.3593(4) 0.6940(3) 0.0730(11) Uani 1 1 d . . . . .
H11A H 0.408786 0.368321 0.759003 0.088 Uiso 1 1 calc R U . . .
H11B H 0.510226 0.411824 0.664799 0.088 Uiso 1 1 calc R U . . .
C12 C 0.5042(4) 0.2303(4) 0.7188(3) 0.0765(11) Uani 1 1 d . . . . .
H12A H 0.561322 0.204106 0.773551 0.092 Uiso 1 1 calc R U . . .
H12B H 0.441459 0.178074 0.745703 0.092 Uiso 1 1 calc R U . . .
C9 C 0.2031(3) 0.5437(4) 0.5188(3) 0.0811(12) Uani 1 1 d . . . . .
H9A H 0.146787 0.485096 0.553830 0.097 Uiso 1 1 calc R U . . .
H9B H 0.157928 0.625124 0.504933 0.097 Uiso 1 1 calc R U . . .
C14 C 0.7166(4) 0.1163(4) 0.5400(4) 0.0865(13) Uani 1 1 d . . . . .
H14A H 0.764888 0.181277 0.520360 0.104 Uiso 1 1 calc R U . . .
H14B H 0.772246 0.040295 0.551385 0.104 Uiso 1 1 calc R U . . .
C3 C 0.7078(4) 0.1714(4) 0.3552(4) 0.0917(14) Uani 1 1 d . . . . .
H3A H 0.769675 0.102293 0.356104 0.110 Uiso 1 1 calc R U . . .
H3B H 0.748995 0.240396 0.339843 0.110 Uiso 1 1 calc R U . . .
C13 C 0.6378(4) 0.1059(4) 0.6403(3) 0.0917(14) Uani 1 1 d . . . . .
H13A H 0.585071 0.045015 0.657387 0.110 Uiso 1 1 calc R U . . .
H13B H 0.688318 0.080796 0.699567 0.110 Uiso 1 1 calc R U . . .
C7 C 0.2451(4) 0.5774(4) 0.2400(3) 0.0782(11) Uani 1 1 d . . . . .
H7A H 0.188000 0.594730 0.187135 0.094 Uiso 1 1 calc R U . . .
H7B H 0.293416 0.643307 0.213726 0.094 Uiso 1 1 calc R U . . .
C4 C 0.6274(4) 0.2012(5) 0.2729(4) 0.1009(16) Uani 1 1 d . . . . .
H4A H 0.675366 0.214382 0.205103 0.121 Uiso 1 1 calc R U . . .
H4B H 0.584374 0.133065 0.289706 0.121 Uiso 1 1 calc R U . . .
C6 C 0.4011(4) 0.4710(5) 0.1623(3) 0.1019(17) Uani 1 1 d . . . . .
H6A H 0.456173 0.529100 0.147663 0.122 Uiso 1 1 calc R U . . .
H6B H 0.353038 0.499297 0.101000 0.122 Uiso 1 1 calc R U . . .
C5 C 0.4720(5) 0.3526(6) 0.1763(4) 0.134(2) Uani 1 1 d . . . . .
H5A H 0.416975 0.295940 0.186188 0.161 Uiso 1 1 calc R U . . .
H5B H 0.525227 0.359751 0.111960 0.161 Uiso 1 1 calc R U . . .
C1A C 0.321(2) 0.189(2) 0.5341(16) 0.105(6) Uani 0.391(13) 1 d . U P B 2
H1AD H 0.325515 0.137272 0.495562 0.126 Uiso 0.391(13) 1 calc R U P B 2
H1AE H 0.368877 0.141645 0.595334 0.126 Uiso 0.391(13) 1 calc R U P B 2
C1 C 0.3260(15) 0.2027(13) 0.4708(17) 0.139(5) Uani 0.609(13) 1 d . U P B 1
H1A H 0.366717 0.162672 0.423753 0.167 Uiso 0.609(13) 1 calc R U P B 1
H1B H 0.333138 0.141758 0.543378 0.167 Uiso 0.609(13) 1 calc R U P B 1
Br1B Br 0.1051(2) 0.2297(3) 0.4744(3) 0.0858(12) Uani 0.207(2) 1 d . . P B 2
Br1 Br 0.1222(4) 0.2047(4) 0.5679(4) 0.1414(19) Uani 0.232(2) 1 d . . P B 1
C2 C 0.2094(10) 0.2266(9) 0.4545(9) 0.160(6) Uani 0.609(13) 1 d . U P B 1
H2A H 0.192269 0.174156 0.422582 0.192 Uiso 0.609(13) 1 calc R U P B 1
H2B H 0.189646 0.310829 0.404695 0.192 Uiso 0.609(13) 1 calc R U P B 1
C2A C 0.2178(15) 0.1966(16) 0.5714(13) 0.115(6) Uani 0.391(13) 1 d . . P B 2
H2AA H 0.202082 0.260641 0.598663 0.138 Uiso 0.391(13) 1 calc R U P B 2
H2AB H 0.207084 0.120067 0.631431 0.138 Uiso 0.391(13) 1 calc R U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S1 2.1687(8) . ?
Ni1 S2 2.1611(8) . ?
Ni1 S7 2.1548(8) . ?
Ni1 S6 2.1690(8) . ?
S1 C15 1.717(3) . ?
S3 C15 1.747(3) . ?
S3 C17 1.733(3) . ?
S9 C19 1.747(3) . ?
S9 C20 1.720(3) . ?
S4 C16 1.736(3) . ?
S4 C17 1.716(3) . ?
S2 C16 1.716(3) . ?
S7 C19 1.707(3) . ?
S6 C18 1.713(3) . ?
S8 C18 1.744(3) . ?
S8 C20 1.733(3) . ?
S5 C17 1.653(3) . ?
S10 C20 1.646(3) . ?
O5 C10 1.420(4) . ?
O5 C11 1.420(4) . ?
O6 C12 1.414(4) . ?
O6 C13 1.408(4) . ?
O4 C8 1.387(4) . ?
O4 C9 1.418(4) . ?
O1 C14 1.416(4) . ?
O1 C3 1.416(5) . ?
N1 H1BD 0.8900 . ?
N1 H1BE 0.8900 . ?
N1 H1BF 0.8900 . ?
N1 H1AA 0.8900 . ?
N1 H1AB 0.8900 . ?
N1 H1AC 0.8900 . ?
N1 C1A 1.58(2) . ?
N1 C1 1.434(14) . ?
O3 C7 1.399(4) . ?
O3 C6 1.403(5) . ?
O2 C4 1.397(4) . ?
O2 C5 1.382(4) . ?
C19 C18 1.354(4) . ?
C15 C16 1.359(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C9 1.478(5) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C7 1.468(5) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.481(5) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C13 1.491(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.434(6) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C5 1.445(6) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C1A H1AD 0.9700 . ?
C1A H1AE 0.9700 . ?
C1A C2A 1.19(2) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.310(17) . ?
Br1B C2A 1.842(13) . ?
Br1 C2 1.658(13) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S1 Ni1 S6 88.53(3) . . ?
S2 Ni1 S1 93.20(3) . . ?
S2 Ni1 S6 176.11(4) . . ?
S7 Ni1 S1 176.10(4) . . ?
S7 Ni1 S2 85.56(3) . . ?
S7 Ni1 S6 92.93(3) . . ?
C15 S1 Ni1 101.75(10) . . ?
C17 S3 C15 97.17(13) . . ?
C20 S9 C19 97.16(14) . . ?
C17 S4 C16 97.49(13) . . ?
C16 S2 Ni1 102.30(10) . . ?
C19 S7 Ni1 102.43(10) . . ?
C18 S6 Ni1 101.87(10) . . ?
C20 S8 C18 97.76(14) . . ?
C10 O5 C11 112.7(3) . . ?
C13 O6 C12 114.2(3) . . ?
C8 O4 C9 115.4(3) . . ?
C14 O1 C3 112.6(3) . . ?
H1BD N1 H1BE 109.5 . . ?
H1BD N1 H1BF 109.5 . . ?
H1BE N1 H1BF 109.5 . . ?
H1AA N1 H1AB 109.5 . . ?
H1AA N1 H1AC 109.5 . . ?
H1AB N1 H1AC 109.5 . . ?
C1A N1 H1BD 109.5 . . ?
C1A N1 H1BE 109.5 . . ?
C1A N1 H1BF 109.5 . . ?
C1 N1 H1AA 109.5 . . ?
C1 N1 H1AB 109.5 . . ?
C1 N1 H1AC 109.5 . . ?
C7 O3 C6 113.7(3) . . ?
C5 O2 C4 116.0(3) . . ?
S7 C19 S9 121.86(17) . . ?
C18 C19 S9 116.8(2) . . ?
C18 C19 S7 121.4(2) . . ?
S1 C15 S3 122.74(16) . . ?
C16 C15 S1 121.7(2) . . ?
C16 C15 S3 115.5(2) . . ?
S2 C16 S4 122.55(17) . . ?
C15 C16 S4 116.4(2) . . ?
C15 C16 S2 121.0(2) . . ?
S6 C18 S8 123.48(18) . . ?
C19 C18 S6 121.4(2) . . ?
C19 C18 S8 115.1(2) . . ?
S9 C20 S8 113.16(16) . . ?
S10 C20 S9 123.1(2) . . ?
S10 C20 S8 123.76(18) . . ?
S4 C17 S3 113.42(15) . . ?
S5 C17 S3 123.69(18) . . ?
S5 C17 S4 122.89(17) . . ?
O5 C10 H10A 109.7 . . ?
O5 C10 H10B 109.7 . . ?
O5 C10 C9 109.9(3) . . ?
H10A C10 H10B 108.2 . . ?
C9 C10 H10A 109.7 . . ?
C9 C10 H10B 109.7 . . ?
O4 C8 H8A 109.6 . . ?
O4 C8 H8B 109.6 . . ?
O4 C8 C7 110.4(3) . . ?
H8A C8 H8B 108.1 . . ?
C7 C8 H8A 109.6 . . ?
C7 C8 H8B 109.6 . . ?
O5 C11 H11A 109.9 . . ?
O5 C11 H11B 109.9 . . ?
O5 C11 C12 109.1(3) . . ?
H11A C11 H11B 108.3 . . ?
C12 C11 H11A 109.9 . . ?
C12 C11 H11B 109.9 . . ?
O6 C12 C11 108.8(3) . . ?
O6 C12 H12A 109.9 . . ?
O6 C12 H12B 109.9 . . ?
C11 C12 H12A 109.9 . . ?
C11 C12 H12B 109.9 . . ?
H12A C12 H12B 108.3 . . ?
O4 C9 C10 107.9(3) . . ?
O4 C9 H9A 110.1 . . ?
O4 C9 H9B 110.1 . . ?
C10 C9 H9A 110.1 . . ?
C10 C9 H9B 110.1 . . ?
H9A C9 H9B 108.4 . . ?
O1 C14 H14A 109.8 . . ?
O1 C14 H14B 109.8 . . ?
O1 C14 C13 109.2(3) . . ?
H14A C14 H14B 108.3 . . ?
C13 C14 H14A 109.8 . . ?
C13 C14 H14B 109.8 . . ?
O1 C3 H3A 109.5 . . ?
O1 C3 H3B 109.5 . . ?
O1 C3 C4 110.7(4) . . ?
H3A C3 H3B 108.1 . . ?
C4 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
O6 C13 C14 108.3(3) . . ?
O6 C13 H13A 110.0 . . ?
O6 C13 H13B 110.0 . . ?
C14 C13 H13A 110.0 . . ?
C14 C13 H13B 110.0 . . ?
H13A C13 H13B 108.4 . . ?
O3 C7 C8 110.9(3) . . ?
O3 C7 H7A 109.5 . . ?
O3 C7 H7B 109.5 . . ?
C8 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 108.0 . . ?
O2 C4 C3 111.5(4) . . ?
O2 C4 H4A 109.3 . . ?
O2 C4 H4B 109.3 . . ?
C3 C4 H4A 109.3 . . ?
C3 C4 H4B 109.3 . . ?
H4A C4 H4B 108.0 . . ?
O3 C6 H6A 109.2 . . ?
O3 C6 H6B 109.2 . . ?
O3 C6 C5 111.9(4) . . ?
H6A C6 H6B 107.9 . . ?
C5 C6 H6A 109.2 . . ?
C5 C6 H6B 109.2 . . ?
O2 C5 C6 112.4(4) . . ?
O2 C5 H5A 109.1 . . ?
O2 C5 H5B 109.1 . . ?
C6 C5 H5A 109.1 . . ?
C6 C5 H5B 109.1 . . ?
H5A C5 H5B 107.9 . . ?
N1 C1A H1AD 104.6 . . ?
N1 C1A H1AE 104.6 . . ?
H1AD C1A H1AE 105.7 . . ?
C2A C1A N1 131(2) . . ?
C2A C1A H1AD 104.6 . . ?
C2A C1A H1AE 104.6 . . ?
N1 C1 H1A 106.2 . . ?
N1 C1 H1B 106.2 . . ?
H1A C1 H1B 106.4 . . ?
C2 C1 N1 124.4(12) . . ?
C2 C1 H1A 106.2 . . ?
C2 C1 H1B 106.2 . . ?
C1 C2 Br1 111.4(11) . . ?
C1 C2 H2A 109.3 . . ?
C1 C2 H2B 109.3 . . ?
Br1 C2 H2A 109.3 . . ?
Br1 C2 H2B 109.3 . . ?
H2A C2 H2B 108.0 . . ?
C1A C2A Br1B 113.2(12) . . ?
C1A C2A H2AA 108.9 . . ?
C1A C2A H2AB 108.9 . . ?
Br1B C2A H2AA 108.9 . . ?
Br1B C2A H2AB 108.9 . . ?
H2AA C2A H2AB 107.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S1 C15 S3 178.56(16) . . . . ?
Ni1 S1 C15 C16 1.2(3) . . . . ?
Ni1 S2 C16 S4 -178.51(16) . . . . ?
Ni1 S2 C16 C15 0.2(3) . . . . ?
Ni1 S7 C19 S9 178.28(16) . . . . ?
Ni1 S7 C19 C18 -1.0(3) . . . . ?
Ni1 S6 C18 S8 -179.82(18) . . . . ?
Ni1 S6 C18 C19 0.4(3) . . . . ?
S1 C15 C16 S4 177.78(16) . . . . ?
S1 C15 C16 S2 -1.0(4) . . . . ?
S3 C15 C16 S4 0.2(3) . . . . ?
S3 C15 C16 S2 -178.54(16) . . . . ?
S9 C19 C18 S6 -178.90(18) . . . . ?
S9 C19 C18 S8 1.3(3) . . . . ?
S7 C19 C18 S6 0.4(4) . . . . ?
S7 C19 C18 S8 -179.37(17) . . . . ?
O5 C10 C9 O4 -66.6(4) . . . . ?
O5 C11 C12 O6 62.9(4) . . . . ?
O4 C8 C7 O3 53.1(5) . . . . ?
O1 C14 C13 O6 -64.9(5) . . . . ?
O1 C3 C4 O2 63.7(5) . . . . ?
N1 C1A C2A Br1B 77.5(19) . . . . ?
N1 C1 C2 Br1 -95.1(18) . . . . ?
O3 C6 C5 O2 -58.5(6) . . . . ?
C19 S9 C20 S8 0.4(2) . . . . ?
C19 S9 C20 S10 -179.4(2) . . . . ?
C15 S3 C17 S4 -0.8(2) . . . . ?
C15 S3 C17 S5 179.4(2) . . . . ?
C16 S4 C17 S3 0.9(2) . . . . ?
C16 S4 C17 S5 -179.3(2) . . . . ?
C18 S8 C20 S9 0.1(2) . . . . ?
C18 S8 C20 S10 180.0(2) . . . . ?
C20 S9 C19 S7 179.6(2) . . . . ?
C20 S9 C19 C18 -1.1(3) . . . . ?
C20 S8 C18 S6 179.4(2) . . . . ?
C20 S8 C18 C19 -0.9(3) . . . . ?
C17 S3 C15 S1 -177.2(2) . . . . ?
C17 S3 C15 C16 0.3(3) . . . . ?
C17 S4 C16 S2 178.1(2) . . . . ?
C17 S4 C16 C15 -0.7(3) . . . . ?
C10 O5 C11 C12 -178.4(3) . . . . ?
C8 O4 C9 C10 -172.2(3) . . . . ?
C11 O5 C10 C9 -173.9(3) . . . . ?
C12 O6 C13 C14 -168.8(3) . . . . ?
C9 O4 C8 C7 171.0(4) . . . . ?
C14 O1 C3 C4 -177.8(4) . . . . ?
C3 O1 C14 C13 171.1(4) . . . . ?
C13 O6 C12 C11 171.9(3) . . . . ?
C7 O3 C6 C5 -175.2(4) . . . . ?
C4 O2 C5 C6 -170.6(4) . . . . ?
C6 O3 C7 C8 -172.8(4) . . . . ?
C5 O2 C4 C3 171.1(5) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.201
_oxdiff_exptl_absorpt_empirical_full_min 0.269
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_313k-f2
_database_code_depnum_ccdc_archive 'CCDC 2053401'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-18 downloaded from the CCDC.
;
_audit_creation_date             2020-11-24
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C2 H7 Cl N, C12 H24 O6'
_chemical_formula_sum            'C20 H31 Cl N Ni O6 S10'
_chemical_formula_weight         796.22
_chemical_melting_point          ?
_chemical_oxdiff_formula         C20H30NO6NiS10Cl
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.3149(3)
_cell_length_b                   12.3589(3)
_cell_length_c                   12.9090(3)
_cell_angle_alpha                90.9686(19)
_cell_angle_beta                 110.340(2)
_cell_angle_gamma                96.269(2)
_cell_volume                     1679.59(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    14036
_cell_measurement_temperature    313
_cell_measurement_theta_max      28.3050
_cell_measurement_theta_min      1.6660
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.314
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56992
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             822
_exptl_crystal_size_max          0.961
_exptl_crystal_size_mid          0.624
_exptl_crystal_size_min          0.371
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.893
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            32926
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.893
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.016
_diffrn_reflns_theta_min         1.934
_diffrn_ambient_temperature      313
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      7.00  96.00   0.50    0.15    --   21.85  35.00 -63.00  178
  2  ω     79.00 104.00   0.50    0.15    --   21.85  57.00  90.00   50
  3  ω    -21.00  60.00   0.50    0.15    --   21.85  57.00  90.00  162
  4  ω    -25.00  91.00   0.50    0.15    --   21.85  19.00  90.00  232
  5  ω    -22.00  56.00   0.50    0.15    --  -21.77  35.00 -63.00  156
  6  ω    -16.00  44.00   0.50    0.15    --   21.85 -37.00  60.00  120
  7  ω    -61.00  14.00   0.50    0.15    --   21.85 -35.00 138.00  150
  8  ω    -64.00 -39.00   0.50    0.15    --   21.85 -37.00  60.00   50
  9  ω    -74.00  26.00   0.50    0.15    --   21.85 -19.00  30.00  200
 10  ω     22.00  81.00   0.50    0.15    --   21.85 -99.00 -60.00  118
 11  ω     54.00 104.00   0.50    0.15    --   21.85-178.00 120.00  100
 12  ω    -98.00  -6.00   0.50    0.15    --  -21.77 -35.00 138.00  184
 13  ω    -98.00  20.00   0.50    0.15    --  -21.77 -57.00 120.00  236
 14  ω    -18.00  37.00   0.50    0.15    --  -21.77 -99.00 -60.00  110
 15  ω    -10.00  26.00   0.50    0.15    --  -21.77 -99.00-120.00   72
 16  ω   -125.00 -51.00   0.50    0.15    --  -21.77-178.00 120.00  148
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0541026000
_diffrn_orient_matrix_UB_12      0.0204528000
_diffrn_orient_matrix_UB_13      0.0049411000
_diffrn_orient_matrix_UB_21      0.0347841000
_diffrn_orient_matrix_UB_22      0.0157651000
_diffrn_orient_matrix_UB_23      0.0564600000
_diffrn_orient_matrix_UB_31      0.0200264000
_diffrn_orient_matrix_UB_32      0.0517523000
_diffrn_orient_matrix_UB_33      -0.0152903000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5758
_reflns_number_total             7989
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS n/a (Sheldrick, 2008)'
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         7989
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0389
_refine_ls_restrained_S_all      0.996
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0791P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1150
_refine_ls_wR_factor_ref         0.1287
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
2. Others
 Sof(Cl1A)=Sof(H1BC)=Sof(H1BD)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(Cl1)=FVAR(1)
 Sof(H3BC)=Sof(H3BD)=Sof(O5A)=Sof(O4A)=Sof(C10A)=Sof(H10C)=Sof(H10D)=Sof(C9A)=
 Sof(H9AA)=Sof(H9AB)=Sof(H11C)=Sof(H11D)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(O3A)=
 Sof(C12A)=Sof(H12C)=Sof(H12D)=Sof(C13A)=Sof(H13C)=Sof(H13D)=Sof(C6A)=Sof(H6AA)=
 Sof(H6AB)=Sof(O6A)=Sof(O2A)=Sof(C14A)=Sof(H14C)=Sof(H14D)=Sof(C4A)=Sof(H4AA)=
 Sof(H4AB)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(O1A)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=1-
 FVAR(2)
 Sof(O4)=Sof(O1)=Sof(O3)=Sof(O6)=Sof(H3AA)=Sof(H3AB)=Sof(O5)=Sof(O2)=Sof(C9)=
 Sof(H9A)=Sof(H9B)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C13)=Sof(H13A)=Sof(H13B)=
 Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C7)=Sof(H7A)=
 Sof(H7B)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C8)=
 Sof(H8A)=Sof(H8B)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H11A)=Sof(H11B)=FVAR(2)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1AA,H1AB), C1(H1BC,H1BD), C3(H3AA,H3AB), C3(H3BC,H3BD), C9(H9A,H9B),
 C5(H5A,H5B), C13(H13A,H13B), C14(H14A,H14B), C4(H4A,H4B), C7(H7A,H7B), C2(H2A,
 H2B), C12(H12A,H12B), C6(H6A,H6B), C2A(H2AA,H2AB), C8(H8A,H8B), C10(H10A,H10B),
  C10A(H10C,H10D), C9A(H9AA,H9AB), C11(H11C,H11D), C11(H11A,H11B), C8A(H8AA,
 H8AB), C12A(H12C,H12D), C13A(H13C,H13D), C6A(H6AA,H6AB), C14A(H14C,H14D),
 C4A(H4AA,H4AB), C5A(H5AA,H5AB), C7A(H7AA,H7AB)
3.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.84527(2) 0.88970(2) 0.51222(2) 0.05150(11) Uani 1 1 d . . . . .
S6 S 0.69208(6) 0.97509(5) 0.52331(5) 0.06270(16) Uani 1 1 d . . . . .
S2 S 1.00551(6) 0.81255(5) 0.50666(5) 0.06356(16) Uani 1 1 d . . . . .
S1 S 0.78956(6) 0.92782(5) 0.34022(5) 0.06369(17) Uani 1 1 d . . . . .
S7 S 0.89933(6) 0.84534(5) 0.68205(5) 0.06560(17) Uani 1 1 d . . . . .
S8 S 0.61370(6) 1.02494(5) 0.72022(5) 0.06294(16) Uani 1 1 d . . . . .
S9 S 0.80172(6) 0.90284(5) 0.86448(5) 0.06873(18) Uani 1 1 d . . . . .
S4 S 1.09921(6) 0.77187(6) 0.31782(6) 0.06936(18) Uani 1 1 d . . . . .
S3 S 0.90673(7) 0.88498(6) 0.16673(5) 0.06996(18) Uani 1 1 d . . . . .
S10 S 0.62593(8) 1.00273(6) 0.95277(6) 0.0797(2) Uani 1 1 d . . . . .
S5 S 1.08910(8) 0.78578(7) 0.08556(6) 0.0864(2) Uani 1 1 d . . . . .
Cl1A Cl 0.8241(8) 0.4504(5) 0.5234(6) 0.0863(12) Uani 0.339(7) 1 d . . P A 2
N1 N 0.66583(18) 0.50194(13) 0.25596(15) 0.0608(5) Uani 1 1 d . . . . .
H1A H 0.656996 0.519323 0.187265 0.073 Uiso 1 1 calc R U . . .
H1B H 0.592071 0.502830 0.266141 0.073 Uiso 1 1 calc R U . . .
H1C H 0.689856 0.435570 0.266540 0.073 Uiso 1 1 calc R U . . .
C18 C 0.7085(2) 0.96498(16) 0.66033(18) 0.0525(5) Uani 1 1 d . . . . .
C19 C 0.7979(2) 0.90786(17) 0.72847(18) 0.0547(5) Uani 1 1 d . . . . .
C15 C 0.9023(2) 0.87675(16) 0.30028(18) 0.0547(5) Uani 1 1 d . . . . .
C17 C 1.0339(2) 0.81274(19) 0.1851(2) 0.0632(6) Uani 1 1 d . . . . .
C20 C 0.6780(2) 0.97833(17) 0.8514(2) 0.0598(5) Uani 1 1 d . . . . .
C16 C 0.9948(2) 0.82438(17) 0.37163(19) 0.0559(5) Uani 1 1 d . . . . .
O4 O 0.7042(6) 0.6197(4) 0.0798(4) 0.0764(13) Uani 0.537(6) 1 d . . P B 1
O1 O 0.5092(5) 0.3199(4) 0.3174(5) 0.0827(14) Uani 0.537(6) 1 d . . P B 1
O3 O 0.4922(5) 0.6516(4) 0.1426(5) 0.0784(13) Uani 0.537(6) 1 d . . P B 1
O6 O 0.7216(4) 0.2816(3) 0.2645(4) 0.0687(12) Uani 0.537(6) 1 d . . P B 1
C1 C 0.7636(3) 0.5822(2) 0.3360(2) 0.0856(8) Uani 1 1 d . . . . .
H1AA H 0.746713 0.655240 0.313795 0.103 Uiso 0.661(7) 1 calc R U P A 1
H1AB H 0.846281 0.572018 0.333272 0.103 Uiso 0.661(7) 1 calc R U P A 1
H1BC H 0.800226 0.633300 0.295899 0.103 Uiso 0.339(7) 1 calc R U P A 2
H1BD H 0.723797 0.623135 0.376778 0.103 Uiso 0.339(7) 1 calc R U P A 2
C3 C 0.6465(3) 0.2033(2) 0.3032(4) 0.1071(12) Uani 1 1 d . . . . .
H3AA H 0.582373 0.163760 0.239089 0.128 Uiso 0.537(6) 1 calc R U P B 1
H3AB H 0.700934 0.151241 0.343656 0.128 Uiso 0.537(6) 1 calc R U P B 1
H3BC H 0.713599 0.213342 0.375164 0.128 Uiso 0.463(6) 1 calc R U P B 2
H3BD H 0.598890 0.132285 0.299646 0.128 Uiso 0.463(6) 1 calc R U P B 2
O5 O 0.7877(5) 0.4167(5) 0.1160(4) 0.0809(13) Uani 0.537(6) 1 d . . P B 1
O2 O 0.4315(6) 0.5260(5) 0.2990(5) 0.0925(16) Uani 0.537(6) 1 d . . P B 1
C9 C 0.5526(13) 0.7316(9) 0.0931(9) 0.084(3) Uani 0.537(6) 1 d . . P B 1
H9A H 0.621077 0.775793 0.150291 0.101 Uiso 0.537(6) 1 calc R U P B 1
H9B H 0.491815 0.779082 0.052416 0.101 Uiso 0.537(6) 1 calc R U P B 1
C5 C 0.4407(16) 0.3515(16) 0.3782(14) 0.090(4) Uani 0.537(6) 1 d . . P B 1
H5A H 0.497207 0.385831 0.448767 0.108 Uiso 0.537(6) 1 calc R U P B 1
H5B H 0.390280 0.288673 0.392265 0.108 Uiso 0.537(6) 1 calc R U P B 1
C13 C 0.8654(9) 0.3387(8) 0.1730(9) 0.083(2) Uani 0.537(6) 1 d . . P B 1
H13A H 0.926473 0.371304 0.242569 0.100 Uiso 0.537(6) 1 calc R U P B 1
H13B H 0.911540 0.312442 0.128825 0.100 Uiso 0.537(6) 1 calc R U P B 1
C14 C 0.7794(6) 0.2452(6) 0.1942(6) 0.0767(19) Uani 0.537(6) 1 d . . P B 1
H14A H 0.715144 0.216197 0.124648 0.092 Uiso 0.537(6) 1 calc R U P B 1
H14B H 0.828898 0.187211 0.227174 0.092 Uiso 0.537(6) 1 calc R U P B 1
C4 C 0.5890(7) 0.2399(5) 0.3665(7) 0.089(2) Uani 0.537(6) 1 d . . P B 1
H4A H 0.652515 0.271005 0.435528 0.107 Uiso 0.537(6) 1 calc R U P B 1
H4B H 0.538434 0.179185 0.383795 0.107 Uiso 0.537(6) 1 calc R U P B 1
C7 C 0.3555(10) 0.6071(11) 0.2425(10) 0.103(3) Uani 0.537(6) 1 d . . P B 1
H7A H 0.315203 0.637454 0.289654 0.124 Uiso 0.537(6) 1 calc R U P B 1
H7B H 0.289436 0.574280 0.175727 0.124 Uiso 0.537(6) 1 calc R U P B 1
C2 C 0.7674(5) 0.5729(3) 0.4517(4) 0.0924(18) Uani 0.661(7) 1 d . . P A 1
H2A H 0.681479 0.567813 0.452330 0.111 Uiso 0.661(7) 1 calc R U P A 1
H2B H 0.814826 0.638294 0.495579 0.111 Uiso 0.661(7) 1 calc R U P A 1
C12 C 0.8568(9) 0.5053(7) 0.0834(7) 0.104(3) Uani 0.537(6) 1 d . . P B 1
H12A H 0.921446 0.542169 0.148784 0.125 Uiso 0.537(6) 1 calc R U P B 1
H12B H 0.899269 0.476759 0.037130 0.125 Uiso 0.537(6) 1 calc R U P B 1
C6 C 0.3537(9) 0.4326(9) 0.3121(8) 0.102(3) Uani 0.537(6) 1 d . . P B 1
H6A H 0.299996 0.399206 0.240177 0.123 Uiso 0.537(6) 1 calc R U P B 1
H6B H 0.299633 0.453494 0.351179 0.123 Uiso 0.537(6) 1 calc R U P B 1
C2A C 0.8597(8) 0.5312(7) 0.4102(7) 0.083(3) Uani 0.339(7) 1 d . . P A 2
H2AA H 0.930473 0.586904 0.446336 0.099 Uiso 0.339(7) 1 calc R U P A 2
H2AB H 0.888540 0.481943 0.367318 0.099 Uiso 0.339(7) 1 calc R U P A 2
C8 C 0.4384(8) 0.6963(7) 0.2133(9) 0.102(3) Uani 0.537(6) 1 d . . P B 1
H8A H 0.388122 0.752718 0.177099 0.123 Uiso 0.537(6) 1 calc R U P B 1
H8B H 0.504903 0.728965 0.279945 0.123 Uiso 0.537(6) 1 calc R U P B 1
C10 C 0.6027(10) 0.6795(6) 0.0188(9) 0.095(2) Uani 0.537(6) 1 d . . P B 1
H10A H 0.535595 0.630305 -0.034503 0.114 Uiso 0.537(6) 1 calc R U P B 1
H10B H 0.633755 0.734367 -0.021527 0.114 Uiso 0.537(6) 1 calc R U P B 1
O5A O 0.7761(6) 0.4749(6) 0.0804(5) 0.0818(15) Uani 0.463(6) 1 d . . P B 2
O4A O 0.6460(8) 0.6532(6) 0.0884(5) 0.0824(16) Uani 0.463(6) 1 d . . P B 2
C10A C 0.6955(12) 0.6341(7) 0.0040(9) 0.110(4) Uani 0.463(6) 1 d . . P B 2
H10C H 0.626906 0.599918 -0.060467 0.132 Uiso 0.463(6) 1 calc R U P B 2
H10D H 0.725995 0.703879 -0.016674 0.132 Uiso 0.463(6) 1 calc R U P B 2
C9A C 0.5318(17) 0.7050(12) 0.0460(11) 0.095(4) Uani 0.463(6) 1 d . . P B 2
H9AA H 0.465805 0.656557 -0.009148 0.114 Uiso 0.463(6) 1 calc R U P B 2
H9AB H 0.548189 0.771237 0.011341 0.114 Uiso 0.463(6) 1 calc R U P B 2
C11 C 0.7830(6) 0.5761(4) 0.0288(5) 0.1379(19) Uani 1 1 d . . . . .
H11C H 0.858356 0.621203 0.077066 0.165 Uiso 0.463(6) 1 calc R U P B 2
H11D H 0.798429 0.559772 -0.038868 0.165 Uiso 0.463(6) 1 calc R U P B 2
H11A H 0.728814 0.541394 -0.042357 0.165 Uiso 0.537(6) 1 calc R U P B 1
H11B H 0.836514 0.636461 0.014388 0.165 Uiso 0.537(6) 1 calc R U P B 1
C8A C 0.4904(10) 0.7310(7) 0.1389(8) 0.095(3) Uani 0.463(6) 1 d . . P B 2
H8AA H 0.558345 0.776300 0.195617 0.114 Uiso 0.463(6) 1 calc R U P B 2
H8AB H 0.417629 0.771308 0.113208 0.114 Uiso 0.463(6) 1 calc R U P B 2
O3A O 0.4572(6) 0.6327(5) 0.1843(5) 0.0759(15) Uani 0.463(6) 1 d . . P B 2
C12A C 0.8727(10) 0.4088(9) 0.1220(8) 0.099(3) Uani 0.463(6) 1 d . . P B 2
H12C H 0.932079 0.440795 0.192557 0.119 Uiso 0.463(6) 1 calc R U P B 2
H12D H 0.918624 0.404806 0.071364 0.119 Uiso 0.463(6) 1 calc R U P B 2
C13A C 0.8198(10) 0.2972(10) 0.1370(10) 0.084(3) Uani 0.463(6) 1 d . . P B 2
H13C H 0.756946 0.265866 0.067752 0.101 Uiso 0.463(6) 1 calc R U P B 2
H13D H 0.886910 0.250601 0.160580 0.101 Uiso 0.463(6) 1 calc R U P B 2
C6A C 0.3586(12) 0.5428(11) 0.2988(9) 0.105(3) Uani 0.463(6) 1 d . . P B 2
H6AA H 0.323489 0.553369 0.356404 0.126 Uiso 0.463(6) 1 calc R U P B 2
H6AB H 0.290305 0.510699 0.233099 0.126 Uiso 0.463(6) 1 calc R U P B 2
O6A O 0.7642(6) 0.3050(4) 0.2169(4) 0.0761(15) Uani 0.463(6) 1 d . . P B 2
O2A O 0.4522(7) 0.4715(6) 0.3337(5) 0.0916(19) Uani 0.463(6) 1 d . . P B 2
C14A C 0.6988(8) 0.2021(6) 0.2282(7) 0.087(2) Uani 0.463(6) 1 d . . P B 2
H14C H 0.633469 0.178388 0.157416 0.104 Uiso 0.463(6) 1 calc R U P B 2
H14D H 0.758671 0.148702 0.245950 0.104 Uiso 0.463(6) 1 calc R U P B 2
C4A C 0.5065(10) 0.2947(8) 0.3779(10) 0.097(3) Uani 0.463(6) 1 d . . P B 2
H4AA H 0.571067 0.324380 0.446950 0.116 Uiso 0.463(6) 1 calc R U P B 2
H4AB H 0.471538 0.222761 0.389837 0.116 Uiso 0.463(6) 1 calc R U P B 2
C5A C 0.4015(19) 0.3686(18) 0.3413(16) 0.100(6) Uani 0.463(6) 1 d . . P B 2
H5AA H 0.339677 0.341298 0.269978 0.120 Uiso 0.463(6) 1 calc R U P B 2
H5AB H 0.358364 0.368863 0.394384 0.120 Uiso 0.463(6) 1 calc R U P B 2
O1A O 0.5604(7) 0.2872(5) 0.2959(5) 0.0795(16) Uani 0.463(6) 1 d . . P B 2
C7A C 0.4145(14) 0.6520(12) 0.2737(11) 0.101(4) Uani 0.463(6) 1 d . . P B 2
H7AA H 0.350673 0.701806 0.253378 0.122 Uiso 0.463(6) 1 calc R U P B 2
H7AB H 0.484868 0.683766 0.338173 0.122 Uiso 0.463(6) 1 calc R U P B 2
Cl1 Cl 0.8323(5) 0.4672(4) 0.5082(4) 0.1345(15) Uani 0.661(7) 1 d . . P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S6 2.1692(6) . ?
Ni1 S2 2.1605(6) . ?
Ni1 S1 2.1626(6) . ?
Ni1 S7 2.1593(6) . ?
S6 C18 1.721(2) . ?
S2 C16 1.715(2) . ?
S1 C15 1.707(2) . ?
S7 C19 1.711(2) . ?
S8 C18 1.740(2) . ?
S8 C20 1.731(2) . ?
S9 C19 1.744(2) . ?
S9 C20 1.728(2) . ?
S4 C17 1.723(3) . ?
S4 C16 1.738(2) . ?
S3 C15 1.746(2) . ?
S3 C17 1.725(3) . ?
S10 C20 1.647(2) . ?
S5 C17 1.655(2) . ?
Cl1A C2A 1.916(11) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.486(3) . ?
C18 C19 1.362(3) . ?
C15 C16 1.364(3) . ?
O4 C10 1.437(11) . ?
O4 C11 1.421(8) . ?
O1 C5 1.36(2) . ?
O1 C4 1.419(10) . ?
O3 C9 1.424(14) . ?
O3 C8 1.396(12) . ?
O6 C3 1.428(6) . ?
O6 C14 1.386(9) . ?
C1 H1AA 0.9700 . ?
C1 H1AB 0.9700 . ?
C1 H1BC 0.9700 . ?
C1 H1BD 0.9700 . ?
C1 C2 1.487(5) . ?
C1 C2A 1.394(8) . ?
C3 H3AA 0.9700 . ?
C3 H3AB 0.9700 . ?
C3 H3BC 0.9700 . ?
C3 H3BD 0.9700 . ?
C3 C4 1.311(9) . ?
C3 C14A 1.299(10) . ?
C3 O1A 1.481(8) . ?
O5 C13 1.415(12) . ?
O5 C12 1.430(10) . ?
O2 C7 1.433(13) . ?
O2 C6 1.423(12) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.446(18) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.538(16) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.519(12) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.508(15) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 Cl1 1.627(7) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C11 1.316(10) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
O5A C11 1.435(8) . ?
O5A C12A 1.397(13) . ?
O4A C10A 1.415(13) . ?
O4A C9A 1.442(19) . ?
C10A H10C 0.9700 . ?
C10A H10D 0.9700 . ?
C10A C11 1.241(13) . ?
C9A H9AA 0.9700 . ?
C9A H9AB 0.9700 . ?
C9A C8A 1.474(19) . ?
C11 H11C 0.9700 . ?
C11 H11D 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C8A H8AA 0.9700 . ?
C8A H8AB 0.9700 . ?
C8A O3A 1.428(11) . ?
O3A C7A 1.424(13) . ?
C12A H12C 0.9700 . ?
C12A H12D 0.9700 . ?
C12A C13A 1.486(15) . ?
C13A H13C 0.9700 . ?
C13A H13D 0.9700 . ?
C13A O6A 1.390(13) . ?
C6A H6AA 0.9700 . ?
C6A H6AB 0.9700 . ?
C6A O2A 1.409(15) . ?
C6A C7A 1.515(18) . ?
O6A C14A 1.436(10) . ?
O2A C5A 1.36(2) . ?
C14A H14C 0.9700 . ?
C14A H14D 0.9700 . ?
C4A H4AA 0.9700 . ?
C4A H4AB 0.9700 . ?
C4A C5A 1.53(2) . ?
C4A O1A 1.399(13) . ?
C5A H5AA 0.9700 . ?
C5A H5AB 0.9700 . ?
C7A H7AA 0.9700 . ?
C7A H7AB 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S2 Ni1 S6 176.67(3) . . ?
S2 Ni1 S1 92.98(2) . . ?
S1 Ni1 S6 87.97(2) . . ?
S7 Ni1 S6 93.02(2) . . ?
S7 Ni1 S2 86.13(2) . . ?
S7 Ni1 S1 177.89(2) . . ?
C18 S6 Ni1 102.05(8) . . ?
C16 S2 Ni1 102.36(8) . . ?
C15 S1 Ni1 102.30(8) . . ?
C19 S7 Ni1 102.38(8) . . ?
C20 S8 C18 97.60(11) . . ?
C20 S9 C19 97.64(11) . . ?
C17 S4 C16 97.37(11) . . ?
C17 S3 C15 97.51(12) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
S6 C18 S8 123.08(13) . . ?
C19 C18 S6 120.91(17) . . ?
C19 C18 S8 116.01(17) . . ?
S7 C19 S9 122.72(13) . . ?
C18 C19 S7 121.50(17) . . ?
C18 C19 S9 115.78(17) . . ?
S1 C15 S3 123.23(14) . . ?
C16 C15 S1 121.45(17) . . ?
C16 C15 S3 115.31(18) . . ?
S4 C17 S3 113.43(13) . . ?
S5 C17 S4 122.99(15) . . ?
S5 C17 S3 123.58(16) . . ?
S9 C20 S8 112.94(13) . . ?
S10 C20 S8 123.50(14) . . ?
S10 C20 S9 123.56(15) . . ?
S2 C16 S4 122.81(14) . . ?
C15 C16 S2 120.87(18) . . ?
C15 C16 S4 116.32(18) . . ?
C11 O4 C10 121.3(7) . . ?
C5 O1 C4 113.7(10) . . ?
C8 O3 C9 113.4(7) . . ?
C14 O6 C3 118.3(5) . . ?
N1 C1 H1AA 108.9 . . ?
N1 C1 H1AB 108.9 . . ?
N1 C1 H1BC 109.3 . . ?
N1 C1 H1BD 109.3 . . ?
N1 C1 C2 113.3(3) . . ?
H1AA C1 H1AB 107.7 . . ?
H1BC C1 H1BD 108.0 . . ?
C2 C1 H1AA 108.9 . . ?
C2 C1 H1AB 108.9 . . ?
C2A C1 N1 111.6(4) . . ?
C2A C1 H1BC 109.3 . . ?
C2A C1 H1BD 109.3 . . ?
O6 C3 H3AA 108.0 . . ?
O6 C3 H3AB 108.0 . . ?
H3AA C3 H3AB 107.2 . . ?
H3BC C3 H3BD 107.3 . . ?
C4 C3 O6 117.3(4) . . ?
C4 C3 H3AA 108.0 . . ?
C4 C3 H3AB 108.0 . . ?
C14A C3 H3BC 108.1 . . ?
C14A C3 H3BD 108.1 . . ?
C14A C3 O1A 116.6(5) . . ?
O1A C3 H3BC 108.1 . . ?
O1A C3 H3BD 108.1 . . ?
C13 O5 C12 113.0(8) . . ?
C6 O2 C7 110.8(9) . . ?
O3 C9 H9A 109.6 . . ?
O3 C9 H9B 109.6 . . ?
O3 C9 C10 110.3(8) . . ?
H9A C9 H9B 108.1 . . ?
C10 C9 H9A 109.6 . . ?
C10 C9 H9B 109.6 . . ?
O1 C5 H5A 110.1 . . ?
O1 C5 H5B 110.1 . . ?
O1 C5 C6 107.9(13) . . ?
H5A C5 H5B 108.4 . . ?
C6 C5 H5A 110.1 . . ?
C6 C5 H5B 110.1 . . ?
O5 C13 H13A 110.2 . . ?
O5 C13 H13B 110.2 . . ?
O5 C13 C14 107.6(7) . . ?
H13A C13 H13B 108.5 . . ?
C14 C13 H13A 110.2 . . ?
C14 C13 H13B 110.2 . . ?
O6 C14 C13 109.8(7) . . ?
O6 C14 H14A 109.7 . . ?
O6 C14 H14B 109.7 . . ?
C13 C14 H14A 109.7 . . ?
C13 C14 H14B 109.7 . . ?
H14A C14 H14B 108.2 . . ?
O1 C4 H4A 108.9 . . ?
O1 C4 H4B 108.9 . . ?
C3 C4 O1 113.3(8) . . ?
C3 C4 H4A 108.9 . . ?
C3 C4 H4B 108.9 . . ?
H4A C4 H4B 107.7 . . ?
O2 C7 H7A 109.8 . . ?
O2 C7 H7B 109.8 . . ?
O2 C7 C8 109.4(8) . . ?
H7A C7 H7B 108.2 . . ?
C8 C7 H7A 109.8 . . ?
C8 C7 H7B 109.8 . . ?
C1 C2 H2A 109.1 . . ?
C1 C2 H2B 109.1 . . ?
C1 C2 Cl1 112.6(4) . . ?
H2A C2 H2B 107.8 . . ?
Cl1 C2 H2A 109.1 . . ?
Cl1 C2 H2B 109.1 . . ?
O5 C12 H12A 109.1 . . ?
O5 C12 H12B 109.1 . . ?
H12A C12 H12B 107.9 . . ?
C11 C12 O5 112.4(8) . . ?
C11 C12 H12A 109.1 . . ?
C11 C12 H12B 109.1 . . ?
O2 C6 C5 108.3(12) . . ?
O2 C6 H6A 110.0 . . ?
O2 C6 H6B 110.0 . . ?
C5 C6 H6A 110.0 . . ?
C5 C6 H6B 110.0 . . ?
H6A C6 H6B 108.4 . . ?
Cl1A C2A H2AA 107.6 . . ?
Cl1A C2A H2AB 107.6 . . ?
C1 C2A Cl1A 119.0(6) . . ?
C1 C2A H2AA 107.6 . . ?
C1 C2A H2AB 107.6 . . ?
H2AA C2A H2AB 107.0 . . ?
O3 C8 C7 108.9(7) . . ?
O3 C8 H8A 109.9 . . ?
O3 C8 H8B 109.9 . . ?
C7 C8 H8A 109.9 . . ?
C7 C8 H8B 109.9 . . ?
H8A C8 H8B 108.3 . . ?
O4 C10 C9 110.3(9) . . ?
O4 C10 H10A 109.6 . . ?
O4 C10 H10B 109.6 . . ?
C9 C10 H10A 109.6 . . ?
C9 C10 H10B 109.6 . . ?
H10A C10 H10B 108.1 . . ?
C12A O5A C11 127.5(8) . . ?
C10A O4A C9A 110.8(11) . . ?
O4A C10A H10C 108.5 . . ?
O4A C10A H10D 108.5 . . ?
H10C C10A H10D 107.5 . . ?
C11 C10A O4A 115.2(11) . . ?
C11 C10A H10C 108.5 . . ?
C11 C10A H10D 108.5 . . ?
O4A C9A H9AA 110.0 . . ?
O4A C9A H9AB 110.0 . . ?
O4A C9A C8A 108.4(9) . . ?
H9AA C9A H9AB 108.4 . . ?
C8A C9A H9AA 110.0 . . ?
C8A C9A H9AB 110.0 . . ?
O4 C11 H11A 108.0 . . ?
O4 C11 H11B 108.0 . . ?
C12 C11 O4 117.2(5) . . ?
C12 C11 H11A 108.0 . . ?
C12 C11 H11B 108.0 . . ?
O5A C11 H11C 106.7 . . ?
O5A C11 H11D 106.7 . . ?
C10A C11 O5A 122.5(6) . . ?
C10A C11 H11C 106.7 . . ?
C10A C11 H11D 106.7 . . ?
H11C C11 H11D 106.6 . . ?
H11A C11 H11B 107.2 . . ?
C9A C8A H8AA 109.7 . . ?
C9A C8A H8AB 109.7 . . ?
H8AA C8A H8AB 108.2 . . ?
O3A C8A C9A 109.8(9) . . ?
O3A C8A H8AA 109.7 . . ?
O3A C8A H8AB 109.7 . . ?
C7A O3A C8A 112.7(10) . . ?
O5A C12A H12C 109.5 . . ?
O5A C12A H12D 109.5 . . ?
O5A C12A C13A 110.9(10) . . ?
H12C C12A H12D 108.0 . . ?
C13A C12A H12C 109.5 . . ?
C13A C12A H12D 109.5 . . ?
C12A C13A H13C 110.1 . . ?
C12A C13A H13D 110.1 . . ?
H13C C13A H13D 108.4 . . ?
O6A C13A C12A 107.9(8) . . ?
O6A C13A H13C 110.1 . . ?
O6A C13A H13D 110.1 . . ?
H6AA C6A H6AB 108.1 . . ?
O2A C6A H6AA 109.5 . . ?
O2A C6A H6AB 109.5 . . ?
O2A C6A C7A 110.7(10) . . ?
C7A C6A H6AA 109.5 . . ?
C7A C6A H6AB 109.5 . . ?
C13A O6A C14A 111.5(8) . . ?
C5A O2A C6A 111.9(11) . . ?
C3 C14A O6A 114.6(7) . . ?
C3 C14A H14C 108.6 . . ?
C3 C14A H14D 108.6 . . ?
O6A C14A H14C 108.6 . . ?
O6A C14A H14D 108.6 . . ?
H14C C14A H14D 107.6 . . ?
H4AA C4A H4AB 108.3 . . ?
C5A C4A H4AA 109.8 . . ?
C5A C4A H4AB 109.8 . . ?
O1A C4A H4AA 109.8 . . ?
O1A C4A H4AB 109.8 . . ?
O1A C4A C5A 109.2(12) . . ?
O2A C5A C4A 109.7(14) . . ?
O2A C5A H5AA 109.7 . . ?
O2A C5A H5AB 109.7 . . ?
C4A C5A H5AA 109.7 . . ?
C4A C5A H5AB 109.7 . . ?
H5AA C5A H5AB 108.2 . . ?
C4A O1A C3 118.6(7) . . ?
O3A C7A C6A 107.2(9) . . ?
O3A C7A H7AA 110.3 . . ?
O3A C7A H7AB 110.3 . . ?
C6A C7A H7AA 110.3 . . ?
C6A C7A H7AB 110.3 . . ?
H7AA C7A H7AB 108.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S6 C18 S8 177.14(11) . . . . ?
Ni1 S6 C18 C19 -3.2(2) . . . . ?
Ni1 S2 C16 S4 -178.13(11) . . . . ?
Ni1 S2 C16 C15 2.0(2) . . . . ?
Ni1 S1 C15 S3 -179.46(11) . . . . ?
Ni1 S1 C15 C16 1.7(2) . . . . ?
Ni1 S7 C19 S9 -178.16(12) . . . . ?
Ni1 S7 C19 C18 1.9(2) . . . . ?
S6 C18 C19 S7 0.9(3) . . . . ?
S6 C18 C19 S9 -178.98(11) . . . . ?
S1 C15 C16 S2 -2.7(3) . . . . ?
S1 C15 C16 S4 177.47(11) . . . . ?
S8 C18 C19 S7 -179.38(11) . . . . ?
S8 C18 C19 S9 0.7(2) . . . . ?
S3 C15 C16 S2 178.41(11) . . . . ?
S3 C15 C16 S4 -1.4(2) . . . . ?
N1 C1 C2 Cl1 74.4(5) . . . . ?
N1 C1 C2A Cl1A -72.5(7) . . . . ?
C18 S8 C20 S9 1.97(14) . . . . ?
C18 S8 C20 S10 -177.66(15) . . . . ?
C19 S9 C20 S8 -1.67(15) . . . . ?
C19 S9 C20 S10 177.95(15) . . . . ?
C15 S3 C17 S4 -2.13(15) . . . . ?
C15 S3 C17 S5 178.33(16) . . . . ?
C17 S4 C16 S2 -179.89(14) . . . . ?
C17 S4 C16 C15 0.0(2) . . . . ?
C17 S3 C15 S1 -176.73(14) . . . . ?
C17 S3 C15 C16 2.16(19) . . . . ?
C20 S8 C18 S6 178.04(14) . . . . ?
C20 S8 C18 C19 -1.62(19) . . . . ?
C20 S9 C19 S7 -179.31(14) . . . . ?
C20 S9 C19 C18 0.6(2) . . . . ?
C16 S4 C17 S3 1.51(15) . . . . ?
C16 S4 C17 S5 -178.95(16) . . . . ?
O1 C5 C6 O2 -63.1(14) . . . . ?
O3 C9 C10 O4 -66.5(9) . . . . ?
O6 C3 C4 O1 55.9(7) . . . . ?
C3 O6 C14 C13 -173.9(5) . . . . ?
O5 C13 C14 O6 -64.6(7) . . . . ?
O5 C12 C11 O4 53.5(8) . . . . ?
O2 C7 C8 O3 61.4(10) . . . . ?
C9 O3 C8 C7 168.7(7) . . . . ?
C5 O1 C4 C3 174.6(10) . . . . ?
C13 O5 C12 C11 178.9(6) . . . . ?
C14 O6 C3 C4 -177.7(5) . . . . ?
C4 O1 C5 C6 -176.8(9) . . . . ?
C7 O2 C6 C5 -177.1(10) . . . . ?
C12 O5 C13 C14 -175.4(6) . . . . ?
C6 O2 C7 C8 -170.7(8) . . . . ?
C8 O3 C9 C10 -178.3(7) . . . . ?
C10 O4 C11 C12 -167.1(7) . . . . ?
O5A C12A C13A O6A -64.1(9) . . . . ?
O4A C10A C11 O5A 47.7(11) . . . . ?
O4A C9A C8A O3A -64.0(11) . . . . ?
C10A O4A C9A C8A -175.4(8) . . . . ?
C9A O4A C10A C11 -170.2(9) . . . . ?
C9A C8A O3A C7A -179.2(10) . . . . ?
C11 O4 C10 C9 -169.6(7) . . . . ?
C11 O5A C12A C13A -162.6(7) . . . . ?
C8A O3A C7A C6A 169.1(9) . . . . ?
C12A O5A C11 C10A -172.9(8) . . . . ?
C12A C13A O6A C14A 173.9(8) . . . . ?
C13A O6A C14A C3 178.8(7) . . . . ?
C6A O2A C5A C4A 179.3(11) . . . . ?
O2A C6A C7A O3A 62.8(11) . . . . ?
C14A C3 O1A C4A -177.1(6) . . . . ?
C5A C4A O1A C3 -168.2(10) . . . . ?
O1A C3 C14A O6A 53.0(7) . . . . ?
O1A C4A C5A O2A -64.6(15) . . . . ?
C7A C6A O2A C5A -171.0(12) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.805
_oxdiff_exptl_absorpt_empirical_full_min 0.506
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_173k-f
_database_code_depnum_ccdc_archive 'CCDC 2053395'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-18 downloaded from the CCDC.
;
_audit_creation_date             2020-11-25
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C2 H7 Cl N, C12 H24 O6'
_chemical_formula_sum            'C20 H31 Cl N Ni O6 S10'
_chemical_formula_weight         796.22
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHNONiSCl
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.2452(2)
_cell_length_b                   12.3442(2)
_cell_length_c                   12.8113(2)
_cell_angle_alpha                91.8320(10)
_cell_angle_beta                 111.4310(10)
_cell_angle_gamma                96.2430(10)
_cell_volume                     1640.65(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    29080
_cell_measurement_temperature    173
_cell_measurement_theta_max      72.0580
_cell_measurement_theta_min      3.6060
_shelx_estimated_absorpt_T_max   0.371
_shelx_estimated_absorpt_T_min   0.208
_exptl_absorpt_coefficient_mu    7.865
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             822
_exptl_crystal_size_max          0.291
_exptl_crystal_size_mid          0.249
_exptl_crystal_size_min          0.157
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0930
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            39675
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.485
_diffrn_reflns_theta_min         3.613
_diffrn_ambient_temperature      173
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -106.00   0.00   0.50    0.50    --  -18.00  54.00 173.51  212
  2  ω     11.00  71.00   0.50    0.50    --  -18.00  54.00 173.51  120
  3  ω     16.00  55.00   0.50    0.50    --  -34.00  54.00 -62.82   78
  4  ω    -90.00 -52.00   0.50    0.50    --  -42.00  54.00  61.65   76
  5  ω     18.00  44.00   0.50    0.50    --  -42.00  54.00  61.65   52
  6  ω    -71.00 -12.00   0.50    0.50    --  -42.00  55.00 113.27  118
  7  ω   -126.00 -77.00   0.50    0.50    --  -42.00  55.00 113.27   98
  8  ω      1.00  46.00   0.50    0.50    --  -42.00  55.00 113.27   90
  9  ω     19.00  45.00   0.50    0.50    --  -42.00  55.00-168.97   52
 10  ω     11.00  40.00   0.50    0.50    --  -46.00  55.00 -92.15   58
 11  ω    -57.00 -30.00   0.50    0.50    --  -46.00  55.00 -92.15   54
 12  ω    -90.00 -63.00   0.50    0.50    --  -46.00  55.00 -92.15   54
 13  ω     -1.00  29.00   0.50    0.50    --  -58.00  55.00  -7.06   60
 14  ω    -94.00 -68.00   0.50    0.50    --  -58.00  55.00  -7.06   52
 15  ω    -14.00  30.00   0.50    0.50    --  -58.00  52.00-103.43   88
 16  ω     -5.00  30.00   0.50    0.50    --  -58.00  55.00  72.15   70
 17  ω     -3.00  27.00   0.50    0.50    --  -62.00  54.00-173.21   60
 18  ω     -8.00  27.00   0.50    0.50    --  -62.00  55.00  49.22   70
 19  ω     -4.00  27.00   0.50    0.50    --  -62.00  54.00  19.35   62
 20  ω     -9.00  26.00   0.50    0.50    --  -62.00  55.00 175.69   70
 21  ω     -2.00  27.00   0.50    0.50    --  -62.00  55.00 -31.81   58
 22  ω     -9.00  22.00   0.50    0.50    --  -66.00  54.00 136.19   62
 23  ω    -38.00  18.00   0.50    0.50    --  -70.00  55.00 -53.49  112
 24  ω    -15.00  19.00   0.50    0.50    --  -70.00  55.00 -97.79   68
 25  ω     -9.00  19.00   0.50    0.50    --  -70.00  55.00 163.61   56
 26  ω    -12.00  19.00   0.50    0.50    --  -70.00  55.00 115.56   62
 27  ω    -12.00  14.00   0.50    0.50    --  -74.00  55.00   1.40   52
 28  ω    -99.00  15.00   0.50    0.50    --  -74.00  55.00-118.39  228
 29  ω    -14.00  11.00   0.50    0.50    --  -78.00  55.00 104.38   50
 30  ω    -26.00   5.00   0.50    0.50    --  -82.00  51.00 -64.52   62
 31  ω    -44.00   3.00   0.50    0.50    --  -86.00  53.00 154.54   94
 32  ω    -91.00 -65.00   0.50    0.50    --  -86.00  53.00 154.54   52
 33  ω    -24.00   1.00   0.50    0.50    --  -86.00  53.00  41.86   50
 34  ω    -24.00   2.00   0.50    0.50    --  -86.00  54.00 -10.03   52
 35  ω    -28.00   3.00   0.50    0.50    --  -86.00  54.00  82.53   62
 36  ω   -173.00 -40.00   0.50    0.50    --  -86.00  54.00  82.53  266
 37  ω   -137.00  -1.00   0.50    0.50    --  -90.00  54.00-179.33  272
 38  ω    -37.00  -1.00   0.50    0.50    --  -90.00  52.00-110.37   72
 39  ω   -144.00  -4.00   0.50    0.50    --  -90.00  55.00 133.70  280
 40  ω    -87.00  -5.00   0.50    0.50    --  -94.00  49.00-159.14  164
 41  ω    -92.00 -62.00   0.50    0.50    --  -95.40  55.00-116.86   60
 42  ω   -117.00  -8.00   0.50    0.50    --  -95.40  55.00 -14.52  218
 43  ω   -164.00-138.00   0.50    0.50    --  -95.40  55.00 -14.52   52
 44  ω   -131.00-101.00   0.50    0.50    --  -95.40  55.00-116.86   60
 45  ω    -68.00  -8.00   0.50    0.50    --  -95.40  55.00 159.09  120
 46  ω   -101.00 -73.00   0.50    0.50    --  -95.40  55.00 159.09   56
 47  ω    -98.00  -6.00   0.50    0.50    --  -95.40  53.00  19.94  184
 48  ω   -115.00 -13.00   0.50    0.50    --  -95.40  55.00 114.58  204
 49  ω   -180.00  -7.00   0.50    0.50    --  -95.40  55.00 -79.54  346
 50  ω   -165.00-134.00   0.50    0.50    --  -95.40  55.00 114.58   62
 51  ω   -179.00-138.00   0.50    0.50    --  -95.40  55.00 159.09   82
 52  ω   -183.00  -6.00   0.50    0.50    --  -95.40  55.00-134.94  354
 53  ω   -161.00  -7.00   0.50    0.50    --  -95.40  55.00 -66.26  308
 54  ω   -105.00  -6.00   0.50    0.50    --  -95.40  55.00  72.31  198
 55  ω    -31.00  -6.00   0.50    0.50    --  -95.40  53.00  35.64   50
 56  ω   -184.00-146.00   0.50    0.50    --  -95.40  55.00  72.31   76
 57  ω   -128.00 -41.00   0.50    0.50    --  -95.40  53.00  35.64  174
 58  ω   -137.00  -7.00   0.50    0.50    --  -95.40  54.00 -29.55  260
 59  ω    -59.00  -6.00   0.50    0.50    --  -95.40  55.00-116.86  106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0782058000
_diffrn_orient_matrix_UB_12      -0.0641238000
_diffrn_orient_matrix_UB_13      -0.0513367000
_diffrn_orient_matrix_UB_21      0.1048803000
_diffrn_orient_matrix_UB_22      -0.0015381000
_diffrn_orient_matrix_UB_23      0.1177421000
_diffrn_orient_matrix_UB_31      -0.0700921000
_diffrn_orient_matrix_UB_32      -0.1083629000
_diffrn_orient_matrix_UB_33      0.0170393000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5869
_reflns_number_total             6266
_reflns_odcompleteness_completeness 98.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       0.0034(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         6266
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0354
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0662P)²+0.4591P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1011
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
2. Others
 Sof(Cl1A)=Sof(H1BC)=Sof(H1BD)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(Cl1)=FVAR(1)
 Sof(H3BC)=Sof(H3BD)=Sof(O5A)=Sof(O4A)=Sof(C10A)=Sof(H10C)=Sof(H10D)=Sof(C9A)=
 Sof(H9AA)=Sof(H9AB)=Sof(H11C)=Sof(H11D)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(O3A)=
 Sof(C12A)=Sof(H12C)=Sof(H12D)=Sof(C13A)=Sof(H13C)=Sof(H13D)=Sof(C6A)=Sof(H6AA)=
 Sof(H6AB)=Sof(O6A)=Sof(O2A)=Sof(C14A)=Sof(H14C)=Sof(H14D)=Sof(C4A)=Sof(H4AA)=
 Sof(H4AB)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(O1A)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=1-
 FVAR(2)
 Sof(O4)=Sof(O1)=Sof(O3)=Sof(O6)=Sof(H3AA)=Sof(H3AB)=Sof(O5)=Sof(O2)=Sof(C9)=
 Sof(H9A)=Sof(H9B)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C13)=Sof(H13A)=Sof(H13B)=
 Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C7)=Sof(H7A)=
 Sof(H7B)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C8)=
 Sof(H8A)=Sof(H8B)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H11A)=Sof(H11B)=FVAR(2)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1BC,H1BD), C1(H1AA,H1AB), C3(H3AA,H3AB), C3(H3BC,H3BD), C9(H9A,H9B),
 C5(H5A,H5B), C13(H13A,H13B), C14(H14A,H14B), C4(H4A,H4B), C7(H7A,H7B), C2(H2A,
 H2B), C12(H12A,H12B), C6(H6A,H6B), C2A(H2AA,H2AB), C8(H8A,H8B), C10(H10A,H10B),
  C10A(H10C,H10D), C9A(H9AA,H9AB), C11(H11A,H11B), C11(H11C,H11D), C8A(H8AA,
 H8AB), C12A(H12C,H12D), C13A(H13C,H13D), C6A(H6AA,H6AB), C14A(H14C,H14D),
 C4A(H4AA,H4AB), C5A(H5AA,H5AB), C7A(H7AA,H7AB)
3.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.84528(3) 0.89037(2) 0.51225(2) 0.03103(11) Uani 1 1 d . . . . .
S6 S 0.69180(5) 0.97708(4) 0.52277(4) 0.03901(13) Uani 1 1 d . . . . .
S2 S 1.00588(4) 0.81153(4) 0.50750(4) 0.03755(13) Uani 1 1 d . . . . .
S1 S 0.79317(5) 0.93387(4) 0.34059(4) 0.03866(13) Uani 1 1 d . . . . .
S7 S 0.89779(5) 0.84288(4) 0.68247(4) 0.03802(13) Uani 1 1 d . . . . .
S8 S 0.61356(4) 1.02728(4) 0.72123(4) 0.03814(13) Uani 1 1 d . . . . .
S9 S 0.80138(5) 0.90157(4) 0.86663(4) 0.03941(13) Uani 1 1 d . . . . .
S4 S 1.10013(5) 0.77093(4) 0.31783(4) 0.04284(13) Uani 1 1 d . . . . .
S3 S 0.91040(5) 0.89057(4) 0.16619(4) 0.04138(13) Uani 1 1 d . . . . .
S10 S 0.62575(5) 1.00341(4) 0.95546(4) 0.04701(14) Uani 1 1 d . . . . .
S5 S 1.09113(5) 0.78769(5) 0.08421(4) 0.05219(15) Uani 1 1 d . . . . .
Cl1A Cl 0.8067(7) 0.4725(6) 0.5123(4) 0.0661(16) Uani 0.220(6) 1 d . . P A 2
N1 N 0.66686(15) 0.50258(12) 0.25506(12) 0.0357(3) Uani 1 1 d . . . . .
H1A H 0.663305 0.517381 0.184927 0.043 Uiso 1 1 calc R U . . .
H1B H 0.588226 0.505787 0.259202 0.043 Uiso 1 1 calc R U . . .
H1C H 0.689598 0.434477 0.269383 0.043 Uiso 1 1 calc R U . . .
C18 C 0.70829(17) 0.96592(14) 0.66080(15) 0.0321(4) Uani 1 1 d . . . . .
C19 C 0.79685(17) 0.90740(14) 0.72953(14) 0.0324(4) Uani 1 1 d . . . . .
C15 C 0.90529(18) 0.88018(15) 0.30017(15) 0.0342(4) Uani 1 1 d . . . . .
C17 C 1.03671(19) 0.81517(17) 0.18418(16) 0.0395(4) Uani 1 1 d . . . . .
C20 C 0.67769(18) 0.97918(15) 0.85333(15) 0.0364(4) Uani 1 1 d . . . . .
C16 C 0.99631(17) 0.82582(15) 0.37223(15) 0.0342(4) Uani 1 1 d . . . . .
O4 O 0.7107(3) 0.6179(3) 0.0808(3) 0.0445(7) Uani 0.506(3) 1 d . . P B 1
O1 O 0.5027(3) 0.3219(3) 0.3102(3) 0.0472(8) Uani 0.506(3) 1 d . . P B 1
O3 O 0.4952(3) 0.6538(3) 0.1359(3) 0.0479(8) Uani 0.506(3) 1 d . . P B 1
O6 O 0.7200(3) 0.2824(2) 0.2650(3) 0.0409(7) Uani 0.506(3) 1 d . . P B 1
C1 C 0.7639(2) 0.58434(18) 0.33938(17) 0.0495(5) Uani 1 1 d . . . . .
H1BC H 0.797647 0.640879 0.300619 0.059 Uiso 0.220(6) 1 calc R U P A 2
H1BD H 0.723253 0.620675 0.385286 0.059 Uiso 0.220(6) 1 calc R U P A 2
H1AA H 0.743402 0.658619 0.318871 0.059 Uiso 0.780(6) 1 calc R U P A 1
H1AB H 0.849930 0.577634 0.337251 0.059 Uiso 0.780(6) 1 calc R U P A 1
C3 C 0.6457(3) 0.2038(2) 0.3019(3) 0.0668(7) Uani 1 1 d . . . . .
H3AA H 0.582069 0.160028 0.234806 0.080 Uiso 0.506(3) 1 calc R U P B 1
H3AB H 0.703821 0.153581 0.347073 0.080 Uiso 0.506(3) 1 calc R U P B 1
H3BC H 0.715299 0.215664 0.377315 0.080 Uiso 0.494(3) 1 calc R U P B 2
H3BD H 0.597026 0.130804 0.297185 0.080 Uiso 0.494(3) 1 calc R U P B 2
O5 O 0.7932(3) 0.4139(3) 0.1167(3) 0.0448(7) Uani 0.506(3) 1 d . . P B 1
O2 O 0.4280(4) 0.5317(3) 0.2906(3) 0.0512(8) Uani 0.506(3) 1 d . . P B 1
C9 C 0.5586(8) 0.7337(6) 0.0906(6) 0.0528(18) Uani 0.506(3) 1 d . . P B 1
H9A H 0.629129 0.778678 0.152317 0.063 Uiso 0.506(3) 1 calc R U P B 1
H9B H 0.497008 0.782590 0.047593 0.063 Uiso 0.506(3) 1 calc R U P B 1
C5 C 0.4354(9) 0.3614(13) 0.3706(10) 0.050(2) Uani 0.506(3) 1 d . . P B 1
H5A H 0.496408 0.399596 0.442417 0.060 Uiso 0.506(3) 1 calc R U P B 1
H5B H 0.383471 0.299840 0.388337 0.060 Uiso 0.506(3) 1 calc R U P B 1
C13 C 0.8212(6) 0.3015(5) 0.1339(5) 0.0544(13) Uani 0.506(3) 1 d . . P B 1
H13A H 0.788810 0.261639 0.058584 0.065 Uiso 0.506(3) 1 calc R U P B 1
H13B H 0.916111 0.304310 0.163661 0.065 Uiso 0.506(3) 1 calc R U P B 1
C14 C 0.7818(4) 0.2440(4) 0.1943(4) 0.0457(11) Uani 0.506(3) 1 d . . P B 1
H14A H 0.856804 0.211044 0.243903 0.055 Uiso 0.506(3) 1 calc R U P B 1
H14B H 0.721173 0.183128 0.144061 0.055 Uiso 0.506(3) 1 calc R U P B 1
C4 C 0.5809(5) 0.2418(4) 0.3642(4) 0.0537(12) Uani 0.506(3) 1 d . . P B 1
H4A H 0.643857 0.273972 0.438081 0.064 Uiso 0.506(3) 1 calc R U P B 1
H4B H 0.526016 0.179908 0.377684 0.064 Uiso 0.506(3) 1 calc R U P B 1
C7 C 0.3532(6) 0.6127(5) 0.2308(6) 0.0605(14) Uani 0.506(3) 1 d . . P B 1
H7A H 0.309465 0.644608 0.276712 0.073 Uiso 0.506(3) 1 calc R U P B 1
H7B H 0.286426 0.578662 0.159556 0.073 Uiso 0.506(3) 1 calc R U P B 1
C2 C 0.7687(3) 0.5708(2) 0.4571(2) 0.0544(9) Uani 0.780(6) 1 d . . P A 1
H2A H 0.680058 0.564224 0.456776 0.065 Uiso 0.780(6) 1 calc R U P A 1
H2B H 0.818290 0.636796 0.506006 0.065 Uiso 0.780(6) 1 calc R U P A 1
C12 C 0.8653(5) 0.5004(4) 0.0867(4) 0.0547(12) Uani 0.506(3) 1 d . . P B 1
H12A H 0.935386 0.535503 0.155568 0.066 Uiso 0.506(3) 1 calc R U P B 1
H12B H 0.905397 0.469952 0.037094 0.066 Uiso 0.506(3) 1 calc R U P B 1
C6 C 0.3484(5) 0.4389(5) 0.3038(4) 0.0584(13) Uani 0.506(3) 1 d . . P B 1
H6A H 0.291773 0.403044 0.229313 0.070 Uiso 0.506(3) 1 calc R U P B 1
H6B H 0.293598 0.461831 0.343698 0.070 Uiso 0.506(3) 1 calc R U P B 1
C2A C 0.8647(9) 0.5321(9) 0.4087(8) 0.051(3) Uani 0.220(6) 1 d . . P A 2
H2AA H 0.942997 0.585241 0.445940 0.062 Uiso 0.220(6) 1 calc R U P A 2
H2AB H 0.885171 0.474649 0.364680 0.062 Uiso 0.220(6) 1 calc R U P A 2
C8 C 0.4398(5) 0.7004(5) 0.2065(5) 0.0577(13) Uani 0.506(3) 1 d . . P B 1
H8A H 0.389879 0.758836 0.168976 0.069 Uiso 0.506(3) 1 calc R U P B 1
H8B H 0.508295 0.732928 0.277529 0.069 Uiso 0.506(3) 1 calc R U P B 1
C10 C 0.6118(5) 0.6795(4) 0.0157(5) 0.0552(12) Uani 0.506(3) 1 d . . P B 1
H10A H 0.542358 0.630252 -0.042687 0.066 Uiso 0.506(3) 1 calc R U P B 1
H10B H 0.648016 0.735155 -0.022283 0.066 Uiso 0.506(3) 1 calc R U P B 1
O5A O 0.7757(3) 0.4783(3) 0.0801(3) 0.0450(8) Uani 0.494(3) 1 d . . P B 2
O4A O 0.6462(4) 0.6583(3) 0.0906(3) 0.0476(8) Uani 0.494(3) 1 d . . P B 2
C10A C 0.6969(6) 0.6386(4) 0.0061(5) 0.0571(13) Uani 0.494(3) 1 d . . P B 2
H10C H 0.625872 0.603039 -0.061920 0.068 Uiso 0.494(3) 1 calc R U P B 2
H10D H 0.728487 0.709895 -0.013999 0.068 Uiso 0.494(3) 1 calc R U P B 2
C9A C 0.5309(9) 0.7064(7) 0.0486(6) 0.0564(19) Uani 0.494(3) 1 d . . P B 2
H9AA H 0.463100 0.655081 -0.008883 0.068 Uiso 0.494(3) 1 calc R U P B 2
H9AB H 0.545441 0.773794 0.012790 0.068 Uiso 0.494(3) 1 calc R U P B 2
C11 C 0.7924(4) 0.5767(2) 0.0336(3) 0.0892(11) Uani 1 1 d . . . . .
H11A H 0.738638 0.545304 -0.043572 0.107 Uiso 0.506(3) 1 calc R U P B 1
H11B H 0.851186 0.639260 0.026393 0.107 Uiso 0.506(3) 1 calc R U P B 1
H11C H 0.870547 0.621240 0.087594 0.107 Uiso 0.494(3) 1 calc R U P B 2
H11D H 0.809985 0.559866 -0.035072 0.107 Uiso 0.494(3) 1 calc R U P B 2
C8A C 0.4882(5) 0.7332(4) 0.1428(5) 0.0571(13) Uani 0.494(3) 1 d . . P B 2
H8AA H 0.557681 0.781290 0.202417 0.069 Uiso 0.494(3) 1 calc R U P B 2
H8AB H 0.411411 0.772116 0.115037 0.069 Uiso 0.494(3) 1 calc R U P B 2
O3A O 0.4580(3) 0.6339(3) 0.1870(3) 0.0450(8) Uani 0.494(3) 1 d . . P B 2
C12A C 0.8779(6) 0.4129(5) 0.1229(4) 0.0552(13) Uani 0.494(3) 1 d . . P B 2
H12C H 0.893462 0.382299 0.057360 0.066 Uiso 0.494(3) 1 calc R U P B 2
H12D H 0.956165 0.463271 0.167703 0.066 Uiso 0.494(3) 1 calc R U P B 2
C13A C 0.8712(5) 0.3378(5) 0.1798(5) 0.0477(12) Uani 0.494(3) 1 d . . P B 2
H13C H 0.949735 0.351385 0.248967 0.057 Uiso 0.494(3) 1 calc R U P B 2
H13D H 0.880337 0.271978 0.138628 0.057 Uiso 0.494(3) 1 calc R U P B 2
C6A C 0.3592(6) 0.5458(5) 0.3016(4) 0.0573(13) Uani 0.494(3) 1 d . . P B 2
H6AA H 0.325694 0.557535 0.362073 0.069 Uiso 0.494(3) 1 calc R U P B 2
H6AB H 0.286416 0.512745 0.233503 0.069 Uiso 0.494(3) 1 calc R U P B 2
O6A O 0.7663(3) 0.3059(3) 0.2169(3) 0.0454(8) Uani 0.494(3) 1 d . . P B 2
O2A O 0.4550(3) 0.4735(3) 0.3357(3) 0.0491(8) Uani 0.494(3) 1 d . . P B 2
C14A C 0.7005(5) 0.2034(3) 0.2229(4) 0.0501(11) Uani 0.494(3) 1 d . . P B 2
H14C H 0.632271 0.180284 0.148459 0.060 Uiso 0.494(3) 1 calc R U P B 2
H14D H 0.761817 0.148672 0.240078 0.060 Uiso 0.494(3) 1 calc R U P B 2
C4A C 0.5075(5) 0.2937(4) 0.3766(5) 0.0527(13) Uani 0.494(3) 1 d . . P B 2
H4AA H 0.575566 0.326733 0.447637 0.063 Uiso 0.494(3) 1 calc R U P B 2
H4AB H 0.474863 0.219810 0.390135 0.063 Uiso 0.494(3) 1 calc R U P B 2
C5A C 0.3973(11) 0.3642(12) 0.3406(11) 0.056(3) Uani 0.494(3) 1 d . . P B 2
H5AA H 0.332415 0.336080 0.265971 0.067 Uiso 0.494(3) 1 calc R U P B 2
H5AB H 0.354477 0.363877 0.395749 0.067 Uiso 0.494(3) 1 calc R U P B 2
O1A O 0.5600(3) 0.2854(3) 0.2919(3) 0.0454(8) Uani 0.494(3) 1 d . . P B 2
C7A C 0.4156(7) 0.6534(5) 0.2771(5) 0.0577(13) Uani 0.494(3) 1 d . . P B 2
H7AA H 0.349889 0.704304 0.255883 0.069 Uiso 0.494(3) 1 calc R U P B 2
H7AB H 0.489030 0.686583 0.344667 0.069 Uiso 0.494(3) 1 calc R U P B 2
Cl1 Cl 0.8419(2) 0.45223(15) 0.51479(16) 0.0673(5) Uani 0.780(6) 1 d . . P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S6 2.1692(5) . ?
Ni1 S2 2.1613(5) . ?
Ni1 S1 2.1610(5) . ?
Ni1 S7 2.1597(5) . ?
S6 C18 1.7211(18) . ?
S2 C16 1.7127(18) . ?
S1 C15 1.7128(18) . ?
S7 C19 1.7182(17) . ?
S8 C18 1.7459(18) . ?
S8 C20 1.7327(19) . ?
S9 C19 1.7425(17) . ?
S9 C20 1.7345(19) . ?
S4 C17 1.729(2) . ?
S4 C16 1.7449(18) . ?
S3 C15 1.7467(18) . ?
S3 C17 1.732(2) . ?
S10 C20 1.6475(18) . ?
S5 C17 1.6492(19) . ?
Cl1A C2A 1.822(12) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N1 C1 1.485(2) . ?
C18 C19 1.358(3) . ?
C15 C16 1.360(3) . ?
O4 C10 1.435(6) . ?
O4 C11 1.398(5) . ?
O1 C5 1.376(15) . ?
O1 C4 1.420(6) . ?
O3 C9 1.416(10) . ?
O3 C8 1.412(6) . ?
O6 C3 1.416(4) . ?
O6 C14 1.426(5) . ?
C1 H1BC 0.9900 . ?
C1 H1BD 0.9900 . ?
C1 H1AA 0.9900 . ?
C1 H1AB 0.9900 . ?
C1 C2 1.505(3) . ?
C1 C2A 1.396(10) . ?
C3 H3AA 0.9900 . ?
C3 H3AB 0.9900 . ?
C3 H3BC 0.9900 . ?
C3 H3BD 0.9900 . ?
C3 C4 1.364(6) . ?
C3 C14A 1.363(6) . ?
C3 O1A 1.446(5) . ?
O5 C13 1.462(7) . ?
O5 C12 1.417(6) . ?
O2 C7 1.434(7) . ?
O2 C6 1.429(7) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.480(10) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.500(13) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.231(7) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.493(9) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 Cl1 1.803(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C11 1.351(7) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C2A H2AA 0.9900 . ?
C2A H2AB 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
O5A C11 1.395(5) . ?
O5A C12A 1.430(7) . ?
O4A C10A 1.421(6) . ?
O4A C9A 1.415(10) . ?
C10A H10C 0.9900 . ?
C10A H10D 0.9900 . ?
C10A C11 1.334(7) . ?
C9A H9AA 0.9900 . ?
C9A H9AB 0.9900 . ?
C9A C8A 1.492(11) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 H11C 0.9900 . ?
C11 H11D 0.9900 . ?
C8A H8AA 0.9900 . ?
C8A H8AB 0.9900 . ?
C8A O3A 1.425(6) . ?
O3A C7A 1.424(6) . ?
C12A H12C 0.9900 . ?
C12A H12D 0.9900 . ?
C12A C13A 1.209(8) . ?
C13A H13C 0.9900 . ?
C13A H13D 0.9900 . ?
C13A O6A 1.446(7) . ?
C6A H6AA 0.9900 . ?
C6A H6AB 0.9900 . ?
C6A O2A 1.428(7) . ?
C6A C7A 1.501(9) . ?
O6A C14A 1.414(6) . ?
O2A C5A 1.446(15) . ?
C14A H14C 0.9900 . ?
C14A H14D 0.9900 . ?
C4A H4AA 0.9900 . ?
C4A H4AB 0.9900 . ?
C4A C5A 1.533(14) . ?
C4A O1A 1.418(6) . ?
C5A H5AA 0.9900 . ?
C5A H5AB 0.9900 . ?
C7A H7AA 0.9900 . ?
C7A H7AB 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S2 Ni1 S6 176.79(2) . . ?
S1 Ni1 S6 87.878(19) . . ?
S1 Ni1 S2 92.992(19) . . ?
S7 Ni1 S6 93.148(19) . . ?
S7 Ni1 S2 86.036(19) . . ?
S7 Ni1 S1 178.59(2) . . ?
C18 S6 Ni1 101.90(6) . . ?
C16 S2 Ni1 102.18(7) . . ?
C15 S1 Ni1 102.37(6) . . ?
C19 S7 Ni1 102.20(6) . . ?
C20 S8 C18 97.45(8) . . ?
C20 S9 C19 97.34(9) . . ?
C17 S4 C16 97.48(9) . . ?
C17 S3 C15 97.34(9) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
S6 C18 S8 122.91(11) . . ?
C19 C18 S6 121.23(14) . . ?
C19 C18 S8 115.86(13) . . ?
S7 C19 S9 122.40(11) . . ?
C18 C19 S7 121.32(13) . . ?
C18 C19 S9 116.28(13) . . ?
S1 C15 S3 123.02(11) . . ?
C16 C15 S1 121.01(14) . . ?
C16 C15 S3 115.97(14) . . ?
S4 C17 S3 113.18(10) . . ?
S5 C17 S4 123.19(12) . . ?
S5 C17 S3 123.62(12) . . ?
S8 C20 S9 113.02(10) . . ?
S10 C20 S8 123.59(11) . . ?
S10 C20 S9 123.38(11) . . ?
S2 C16 S4 122.61(11) . . ?
C15 C16 S2 121.42(14) . . ?
C15 C16 S4 115.97(14) . . ?
C11 O4 C10 120.1(4) . . ?
C5 O1 C4 113.7(7) . . ?
C8 O3 C9 112.5(5) . . ?
C3 O6 C14 117.6(3) . . ?
N1 C1 H1BC 109.8 . . ?
N1 C1 H1BD 109.8 . . ?
N1 C1 H1AA 109.0 . . ?
N1 C1 H1AB 109.0 . . ?
N1 C1 C2 112.86(19) . . ?
H1BC C1 H1BD 108.2 . . ?
H1AA C1 H1AB 107.8 . . ?
C2 C1 H1AA 109.0 . . ?
C2 C1 H1AB 109.0 . . ?
C2A C1 N1 109.4(5) . . ?
C2A C1 H1BC 109.8 . . ?
C2A C1 H1BD 109.8 . . ?
O6 C3 H3AA 108.0 . . ?
O6 C3 H3AB 108.0 . . ?
H3AA C3 H3AB 107.3 . . ?
H3BC C3 H3BD 107.5 . . ?
C4 C3 O6 117.2(3) . . ?
C4 C3 H3AA 108.0 . . ?
C4 C3 H3AB 108.0 . . ?
C14A C3 H3BC 108.5 . . ?
C14A C3 H3BD 108.5 . . ?
C14A C3 O1A 114.9(3) . . ?
O1A C3 H3BC 108.5 . . ?
O1A C3 H3BD 108.5 . . ?
C12 O5 C13 127.9(4) . . ?
C6 O2 C7 111.8(5) . . ?
O3 C9 H9A 109.7 . . ?
O3 C9 H9B 109.7 . . ?
O3 C9 C10 109.6(5) . . ?
H9A C9 H9B 108.2 . . ?
C10 C9 H9A 109.7 . . ?
C10 C9 H9B 109.7 . . ?
O1 C5 H5A 109.7 . . ?
O1 C5 H5B 109.7 . . ?
O1 C5 C6 109.9(9) . . ?
H5A C5 H5B 108.2 . . ?
C6 C5 H5A 109.7 . . ?
C6 C5 H5B 109.7 . . ?
O5 C13 H13A 106.8 . . ?
O5 C13 H13B 106.8 . . ?
H13A C13 H13B 106.6 . . ?
C14 C13 O5 122.2(4) . . ?
C14 C13 H13A 106.8 . . ?
C14 C13 H13B 106.8 . . ?
O6 C14 H14A 106.2 . . ?
O6 C14 H14B 106.2 . . ?
C13 C14 O6 124.4(5) . . ?
C13 C14 H14A 106.2 . . ?
C13 C14 H14B 106.2 . . ?
H14A C14 H14B 106.4 . . ?
O1 C4 H4A 109.1 . . ?
O1 C4 H4B 109.1 . . ?
C3 C4 O1 112.3(4) . . ?
C3 C4 H4A 109.1 . . ?
C3 C4 H4B 109.1 . . ?
H4A C4 H4B 107.9 . . ?
O2 C7 H7A 109.8 . . ?
O2 C7 H7B 109.8 . . ?
O2 C7 C8 109.3(4) . . ?
H7A C7 H7B 108.3 . . ?
C8 C7 H7A 109.8 . . ?
C8 C7 H7B 109.8 . . ?
C1 C2 H2A 109.1 . . ?
C1 C2 H2B 109.1 . . ?
C1 C2 Cl1 112.4(2) . . ?
H2A C2 H2B 107.9 . . ?
Cl1 C2 H2A 109.1 . . ?
Cl1 C2 H2B 109.1 . . ?
O5 C12 H12A 109.1 . . ?
O5 C12 H12B 109.1 . . ?
H12A C12 H12B 107.8 . . ?
C11 C12 O5 112.6(5) . . ?
C11 C12 H12A 109.1 . . ?
C11 C12 H12B 109.1 . . ?
O2 C6 C5 107.7(6) . . ?
O2 C6 H6A 110.2 . . ?
O2 C6 H6B 110.2 . . ?
C5 C6 H6A 110.2 . . ?
C5 C6 H6B 110.2 . . ?
H6A C6 H6B 108.5 . . ?
Cl1A C2A H2AA 110.7 . . ?
Cl1A C2A H2AB 110.7 . . ?
C1 C2A Cl1A 105.3(6) . . ?
C1 C2A H2AA 110.7 . . ?
C1 C2A H2AB 110.7 . . ?
H2AA C2A H2AB 108.8 . . ?
O3 C8 C7 108.6(5) . . ?
O3 C8 H8A 110.0 . . ?
O3 C8 H8B 110.0 . . ?
C7 C8 H8A 110.0 . . ?
C7 C8 H8B 110.0 . . ?
H8A C8 H8B 108.4 . . ?
O4 C10 C9 109.5(5) . . ?
O4 C10 H10A 109.8 . . ?
O4 C10 H10B 109.8 . . ?
C9 C10 H10A 109.8 . . ?
C9 C10 H10B 109.8 . . ?
H10A C10 H10B 108.2 . . ?
C11 O5A C12A 121.8(4) . . ?
C9A O4A C10A 112.1(5) . . ?
O4A C10A H10C 108.4 . . ?
O4A C10A H10D 108.4 . . ?
H10C C10A H10D 107.4 . . ?
C11 C10A O4A 115.6(5) . . ?
C11 C10A H10C 108.4 . . ?
C11 C10A H10D 108.4 . . ?
O4A C9A H9AA 109.7 . . ?
O4A C9A H9AB 109.7 . . ?
O4A C9A C8A 109.6(5) . . ?
H9AA C9A H9AB 108.2 . . ?
C8A C9A H9AA 109.7 . . ?
C8A C9A H9AB 109.7 . . ?
O4 C11 H11A 107.7 . . ?
O4 C11 H11B 107.7 . . ?
C12 C11 O4 118.6(3) . . ?
C12 C11 H11A 107.7 . . ?
C12 C11 H11B 107.7 . . ?
O5A C11 H11C 107.7 . . ?
O5A C11 H11D 107.7 . . ?
C10A C11 O5A 118.3(3) . . ?
C10A C11 H11C 107.7 . . ?
C10A C11 H11D 107.7 . . ?
H11A C11 H11B 107.1 . . ?
H11C C11 H11D 107.1 . . ?
C9A C8A H8AA 110.0 . . ?
C9A C8A H8AB 110.0 . . ?
H8AA C8A H8AB 108.3 . . ?
O3A C8A C9A 108.6(5) . . ?
O3A C8A H8AA 110.0 . . ?
O3A C8A H8AB 110.0 . . ?
C7A O3A C8A 111.7(5) . . ?
O5A C12A H12C 106.9 . . ?
O5A C12A H12D 106.9 . . ?
H12C C12A H12D 106.7 . . ?
C13A C12A O5A 121.9(5) . . ?
C13A C12A H12C 106.9 . . ?
C13A C12A H12D 106.9 . . ?
C12A C13A H13C 105.8 . . ?
C12A C13A H13D 105.8 . . ?
C12A C13A O6A 126.0(5) . . ?
H13C C13A H13D 106.2 . . ?
O6A C13A H13C 105.8 . . ?
O6A C13A H13D 105.8 . . ?
H6AA C6A H6AB 108.2 . . ?
O2A C6A H6AA 109.6 . . ?
O2A C6A H6AB 109.6 . . ?
O2A C6A C7A 110.1(5) . . ?
C7A C6A H6AA 109.6 . . ?
C7A C6A H6AB 109.6 . . ?
C14A O6A C13A 133.1(4) . . ?
C6A O2A C5A 110.6(6) . . ?
C3 C14A O6A 113.7(4) . . ?
C3 C14A H14C 108.8 . . ?
C3 C14A H14D 108.8 . . ?
O6A C14A H14C 108.8 . . ?
O6A C14A H14D 108.8 . . ?
H14C C14A H14D 107.7 . . ?
H4AA C4A H4AB 108.1 . . ?
C5A C4A H4AA 109.6 . . ?
C5A C4A H4AB 109.6 . . ?
O1A C4A H4AA 109.6 . . ?
O1A C4A H4AB 109.6 . . ?
O1A C4A C5A 110.2(8) . . ?
O2A C5A C4A 106.3(8) . . ?
O2A C5A H5AA 110.5 . . ?
O2A C5A H5AB 110.5 . . ?
C4A C5A H5AA 110.5 . . ?
C4A C5A H5AB 110.5 . . ?
H5AA C5A H5AB 108.7 . . ?
C4A O1A C3 116.9(4) . . ?
O3A C7A C6A 108.1(4) . . ?
O3A C7A H7AA 110.1 . . ?
O3A C7A H7AB 110.1 . . ?
C6A C7A H7AA 110.1 . . ?
C6A C7A H7AB 110.1 . . ?
H7AA C7A H7AB 108.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S6 C18 S8 176.79(10) . . . . ?
Ni1 S6 C18 C19 -3.55(17) . . . . ?
Ni1 S2 C16 S4 -177.09(10) . . . . ?
Ni1 S2 C16 C15 2.14(17) . . . . ?
Ni1 S1 C15 S3 179.99(10) . . . . ?
Ni1 S1 C15 C16 0.26(17) . . . . ?
Ni1 S7 C19 S9 -177.57(10) . . . . ?
Ni1 S7 C19 C18 2.62(17) . . . . ?
S6 C18 C19 S7 0.7(2) . . . . ?
S6 C18 C19 S9 -179.14(9) . . . . ?
S1 C15 C16 S2 -1.7(2) . . . . ?
S1 C15 C16 S4 177.56(9) . . . . ?
S8 C18 C19 S7 -179.64(9) . . . . ?
S8 C18 C19 S9 0.5(2) . . . . ?
S3 C15 C16 S2 178.54(10) . . . . ?
S3 C15 C16 S4 -2.2(2) . . . . ?
N1 C1 C2 Cl1 72.5(3) . . . . ?
N1 C1 C2A Cl1A -80.9(6) . . . . ?
C18 S8 C20 S9 1.93(12) . . . . ?
C18 S8 C20 S10 -177.46(13) . . . . ?
C19 S9 C20 S8 -1.70(12) . . . . ?
C19 S9 C20 S10 177.69(13) . . . . ?
C15 S3 C17 S4 -2.03(12) . . . . ?
C15 S3 C17 S5 177.77(13) . . . . ?
C17 S4 C16 S2 179.91(12) . . . . ?
C17 S4 C16 C15 0.65(17) . . . . ?
C17 S3 C15 S1 -177.17(12) . . . . ?
C17 S3 C15 C16 2.56(17) . . . . ?
C20 S8 C18 S6 178.16(12) . . . . ?
C20 S8 C18 C19 -1.51(16) . . . . ?
C20 S9 C19 S7 -179.10(12) . . . . ?
C20 S9 C19 C18 0.72(17) . . . . ?
C16 S4 C17 S3 1.10(12) . . . . ?
C16 S4 C17 S5 -178.70(13) . . . . ?
O1 C5 C6 O2 -65.4(8) . . . . ?
O3 C9 C10 O4 -65.4(6) . . . . ?
O6 C3 C4 O1 52.9(5) . . . . ?
C3 O6 C14 C13 161.0(5) . . . . ?
O5 C13 C14 O6 -8.4(9) . . . . ?
O5 C12 C11 O4 48.7(5) . . . . ?
O2 C7 C8 O3 62.7(6) . . . . ?
C9 O3 C8 C7 168.4(5) . . . . ?
C5 O1 C4 C3 179.6(6) . . . . ?
C13 O5 C12 C11 154.4(5) . . . . ?
C14 O6 C3 C4 -176.3(4) . . . . ?
C4 O1 C5 C6 -175.9(6) . . . . ?
C7 O2 C6 C5 -177.9(7) . . . . ?
C12 O5 C13 C14 154.8(6) . . . . ?
C6 O2 C7 C8 -172.6(5) . . . . ?
C8 O3 C9 C10 -178.8(5) . . . . ?
C10 O4 C11 C12 -166.0(4) . . . . ?
O5A C12A C13A O6A -2.9(9) . . . . ?
O4A C10A C11 O5A 49.2(6) . . . . ?
O4A C9A C8A O3A -64.0(7) . . . . ?
C10A O4A C9A C8A -175.5(5) . . . . ?
C9A O4A C10A C11 -168.9(5) . . . . ?
C9A C8A O3A C7A -179.6(5) . . . . ?
C11 O4 C10 C9 -167.7(4) . . . . ?
C11 O5A C12A C13A 167.4(5) . . . . ?
C8A O3A C7A C6A 167.9(5) . . . . ?
C12A O5A C11 C10A -173.2(4) . . . . ?
C12A C13A O6A C14A 137.4(6) . . . . ?
C13A O6A C14A C3 154.7(5) . . . . ?
C6A O2A C5A C4A 179.5(6) . . . . ?
O2A C6A C7A O3A 61.6(6) . . . . ?
C14A C3 O1A C4A -175.9(4) . . . . ?
C5A C4A O1A C3 -167.4(5) . . . . ?
O1A C3 C14A O6A 54.5(5) . . . . ?
O1A C4A C5A O2A -66.0(9) . . . . ?
C7A C6A O2A C5A -170.0(7) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.496
_oxdiff_exptl_absorpt_empirical_full_min 0.759
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_373k-f2
_database_code_depnum_ccdc_archive 'CCDC 2053404'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-18 downloaded from the CCDC.
;
_audit_creation_date             2020-12-31
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C2 H7 Cl N, C12 H24 O6'
_chemical_formula_sum            'C20 H31 Cl N Ni O6 S10'
_chemical_formula_weight         796.22
_chemical_melting_point          ?
_chemical_oxdiff_formula         C20H30NO6NiS10Cl
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.3571(2)
_cell_length_b                   12.3603(2)
_cell_length_c                   12.9511(3)
_cell_angle_alpha                90.864(2)
_cell_angle_beta                 109.988(2)
_cell_angle_gamma                95.958(2)
_cell_volume                     1696.81(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    15146
_cell_measurement_temperature    373
_cell_measurement_theta_max      28.1780
_cell_measurement_theta_min      1.6920
_shelx_estimated_absorpt_T_max   0.644
_shelx_estimated_absorpt_T_min   0.368
_exptl_absorpt_coefficient_mu    1.300
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             822
_exptl_crystal_size_max          0.961
_exptl_crystal_size_mid          0.624
_exptl_crystal_size_min          0.371
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.881
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            33505
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.881
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.130
_diffrn_reflns_theta_min         1.921
_diffrn_ambient_temperature      373
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00  92.00   0.50    0.24    --   21.85  35.00 -65.00  184
  2  ω     79.00 104.00   0.50    0.24    --   21.85 178.00  60.00   50
  3  ω     50.00  75.00   0.50    0.24    --   21.85 178.00  60.00   50
  4  ω    -25.00  97.00   0.50    0.24    --   21.85  19.00  90.00  244
  5  ω   -101.00 -30.00   0.50    0.24    --  -21.77 -35.00 137.00  142
  6  ω    -18.00  37.00   0.50    0.24    --  -21.77 -99.00   0.00  110
  7  ω    -17.00  37.00   0.50    0.24    --  -21.77 -99.00 -60.00  108
  8  ω    -18.00  37.00   0.50    0.24    --  -21.77 -99.00-120.00  110
  9  ω    -96.00  20.00   0.50    0.24    --  -21.77 -57.00 120.00  232
 10  ω    -67.00  40.00   0.50    0.24    --   21.85 -35.00 137.00  214
 11  ω     67.00 102.00   0.50    0.24    --   21.85-178.00 120.00   70
 12  ω    -68.00  43.00   0.50    0.24    --   21.85 -37.00  60.00  222
 13  ω    -10.00  60.00   0.50    0.24    --  -21.77  19.00  60.00  140
 14  ω    -39.00  57.00   0.50    0.24    --  -21.77  35.00 -65.00  192
 15  ω    -66.00 -41.00   0.50    0.24    --  -21.77 178.00 150.00   50
 16  ω   -123.00 -89.00   0.50    0.24    --  -21.77 178.00 150.00   68
 17  ω   -121.00 -53.00   0.50    0.24    --  -21.77 178.00  60.00  136
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0534493000
_diffrn_orient_matrix_UB_12      0.0209938000
_diffrn_orient_matrix_UB_13      0.0055715000
_diffrn_orient_matrix_UB_21      0.0349883000
_diffrn_orient_matrix_UB_22      0.0155839000
_diffrn_orient_matrix_UB_23      0.0559492000
_diffrn_orient_matrix_UB_31      0.0198953000
_diffrn_orient_matrix_UB_32      0.0515280000
_diffrn_orient_matrix_UB_33      -0.0156501000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5497
_reflns_number_total             8059
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         8059
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0398
_refine_ls_restrained_S_all      0.975
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0851P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1397
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
2. Others
 Sof(Cl1A)=Sof(H1bc)=Sof(H1bd)=Sof(C2A)=Sof(H2Aa)=Sof(H2Ab)=1-FVAR(1)
 Sof(H1aa)=Sof(H1ab)=Sof(C2)=Sof(H2a)=Sof(H2b)=Sof(Cl1)=FVAR(1)
 Sof(H3bc)=Sof(H3bd)=Sof(O5A)=Sof(O4A)=Sof(C10A)=Sof(H10c)=Sof(H10d)=Sof(C9A)=
 Sof(H9Aa)=Sof(H9Ab)=Sof(H11c)=Sof(H11d)=Sof(C8A)=Sof(H8Aa)=Sof(H8Ab)=Sof(O3A)=
 Sof(C12A)=Sof(H12c)=Sof(H12d)=Sof(C13A)=Sof(H13c)=Sof(H13d)=Sof(C6A)=Sof(H6Aa)=
 Sof(H6Ab)=Sof(O6A)=Sof(O2A)=Sof(C14A)=Sof(H14c)=Sof(H14d)=Sof(C4A)=Sof(H4Aa)=
 Sof(H4Ab)=Sof(C5A)=Sof(H5Aa)=Sof(H5Ab)=Sof(O1A)=Sof(C7A)=Sof(H7Aa)=Sof(H7Ab)=1-
 FVAR(2)
 Sof(O4)=Sof(O1)=Sof(O3)=Sof(O6)=Sof(H3aa)=Sof(H3ab)=Sof(O5)=Sof(O2)=Sof(C9)=
 Sof(H9a)=Sof(H9b)=Sof(C5)=Sof(H5a)=Sof(H5b)=Sof(C13)=Sof(H13a)=Sof(H13b)=
 Sof(C14)=Sof(H14a)=Sof(H14b)=Sof(C4)=Sof(H4a)=Sof(H4b)=Sof(C7)=Sof(H7a)=
 Sof(H7b)=Sof(C12)=Sof(H12a)=Sof(H12b)=Sof(C6)=Sof(H6a)=Sof(H6b)=Sof(C8)=
 Sof(H8a)=Sof(H8b)=Sof(C10)=Sof(H10a)=Sof(H10b)=Sof(H11a)=Sof(H11b)=FVAR(2)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1bc,H1bd), C1(H1aa,H1ab), C3(H3aa,H3ab), C3(H3bc,H3bd), C9(H9a,H9b),
 C5(H5a,H5b), C13(H13a,H13b), C14(H14a,H14b), C4(H4a,H4b), C7(H7a,H7b), C2(H2a,
 H2b), C12(H12a,H12b), C6(H6a,H6b), C2A(H2Aa,H2Ab), C8(H8a,H8b), C10(H10a,H10b),
  C10A(H10c,H10d), C9A(H9Aa,H9Ab), C11(H11a,H11b), C11(H11c,H11d), C8A(H8Aa,
 H8Ab), C12A(H12c,H12d), C13A(H13c,H13d), C6A(H6Aa,H6Ab), C14A(H14c,H14d),
 C4A(H4Aa,H4Ab), C5A(H5Aa,H5Ab), C7A(H7Aa,H7Ab)
3.b Idealised Me refined as rotating group:
 N1(H1a,H1b,H1c)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.84495(3) 0.88987(2) 0.51184(2) 0.06072(12) Uani 1 1 d . . . . .
S6 S 0.69178(6) 0.97493(5) 0.52351(5) 0.07388(18) Uani 1 1 d . . . . .
S2 S 1.00501(6) 0.81308(6) 0.50561(5) 0.07595(19) Uani 1 1 d . . . . .
S1 S 0.78858(7) 0.92700(5) 0.34026(6) 0.07562(19) Uani 1 1 d . . . . .
S7 S 0.89911(7) 0.84578(6) 0.68099(6) 0.0782(2) Uani 1 1 d . . . . .
S8 S 0.61288(7) 1.02422(5) 0.71955(6) 0.07449(19) Uani 1 1 d . . . . .
S9 S 0.80093(7) 0.90265(6) 0.86276(6) 0.0819(2) Uani 1 1 d . . . . .
S4 S 1.09869(7) 0.77273(6) 0.31723(6) 0.0824(2) Uani 1 1 d . . . . .
S3 S 0.90596(7) 0.88456(6) 0.16718(6) 0.0837(2) Uani 1 1 d . . . . .
S10 S 0.62510(9) 1.00217(7) 0.95114(7) 0.0961(3) Uani 1 1 d . . . . .
S5 S 1.08849(9) 0.78609(8) 0.08626(7) 0.1039(3) Uani 1 1 d . . . . .
Cl1A Cl 0.8225(8) 0.4510(5) 0.5221(5) 0.1008(12) Uani 0.362(8) 1 d . . P A 2
N1 N 0.6675(2) 0.50269(14) 0.25752(17) 0.0719(5) Uani 1 1 d . . . . .
H1A H 0.656252 0.522278 0.189266 0.086 Uiso 1 1 calc R U . . .
H1B H 0.595129 0.501796 0.270159 0.086 Uiso 1 1 calc R U . . .
H1C H 0.692734 0.436560 0.265513 0.086 Uiso 1 1 calc R U . . .
C18 C 0.7080(2) 0.96469(17) 0.6594(2) 0.0621(5) Uani 1 1 d . . . . .
C19 C 0.7981(2) 0.90831(18) 0.7274(2) 0.0663(6) Uani 1 1 d . . . . .
C15 C 0.9017(2) 0.87569(17) 0.30033(19) 0.0653(6) Uani 1 1 d . . . . .
C17 C 1.0330(3) 0.8124(2) 0.1852(2) 0.0756(6) Uani 1 1 d . . . . .
C20 C 0.6772(2) 0.97790(18) 0.8502(2) 0.0708(6) Uani 1 1 d . . . . .
C16 C 0.9946(2) 0.82481(17) 0.3718(2) 0.0655(6) Uani 1 1 d . . . . .
O4 O 0.7035(7) 0.6183(5) 0.0804(6) 0.0913(17) Uani 0.513(7) 1 d . . P B 1
O1 O 0.5122(7) 0.3210(5) 0.3197(7) 0.1032(19) Uani 0.513(7) 1 d . . P B 1
O3 O 0.4935(6) 0.6524(5) 0.1419(7) 0.0953(17) Uani 0.513(7) 1 d . . P B 1
O6 O 0.7206(4) 0.2823(4) 0.2646(5) 0.0829(14) Uani 0.513(7) 1 d . . P B 1
C1 C 0.7643(4) 0.5814(2) 0.3366(3) 0.1051(10) Uani 1 1 d . . . . .
H1BC H 0.801108 0.631988 0.296382 0.126 Uiso 0.362(8) 1 calc R U P A 2
H1BD H 0.724342 0.622989 0.376714 0.126 Uiso 0.362(8) 1 calc R U P A 2
H1AA H 0.846353 0.569889 0.333851 0.126 Uiso 0.638(8) 1 calc R U P A 1
H1AB H 0.748447 0.654591 0.314017 0.126 Uiso 0.638(8) 1 calc R U P A 1
C3 C 0.6478(4) 0.2043(3) 0.3037(5) 0.1270(15) Uani 1 1 d . . . . .
H3AA H 0.584753 0.164317 0.240469 0.152 Uiso 0.513(7) 1 calc R U P B 1
H3AB H 0.702784 0.152778 0.344349 0.152 Uiso 0.513(7) 1 calc R U P B 1
H3BC H 0.714095 0.214892 0.375196 0.152 Uiso 0.487(7) 1 calc R U P B 2
H3BD H 0.601349 0.133252 0.300951 0.152 Uiso 0.487(7) 1 calc R U P B 2
O5 O 0.7884(7) 0.4146(6) 0.1177(5) 0.1014(18) Uani 0.513(7) 1 d . . P B 1
O2 O 0.4320(8) 0.5285(7) 0.2983(7) 0.116(2) Uani 0.513(7) 1 d . . P B 1
C9 C 0.5414(18) 0.7295(16) 0.085(2) 0.134(8) Uani 0.513(7) 1 d . . P B 1
H9A H 0.603196 0.782199 0.137253 0.161 Uiso 0.513(7) 1 calc R U P B 1
H9B H 0.473597 0.767999 0.039584 0.161 Uiso 0.513(7) 1 calc R U P B 1
C5 C 0.4419(17) 0.3503(19) 0.375(2) 0.106(5) Uani 0.513(7) 1 d . . P B 1
H5A H 0.495764 0.383341 0.446104 0.128 Uiso 0.513(7) 1 calc R U P B 1
H5B H 0.392479 0.286262 0.387495 0.128 Uiso 0.513(7) 1 calc R U P B 1
C13 C 0.8628(14) 0.3377(11) 0.1700(15) 0.104(3) Uani 0.513(7) 1 d . . P B 1
H13A H 0.925919 0.369241 0.238017 0.125 Uiso 0.513(7) 1 calc R U P B 1
H13B H 0.905635 0.310443 0.123563 0.125 Uiso 0.513(7) 1 calc R U P B 1
C14 C 0.7781(7) 0.2457(8) 0.1942(7) 0.087(2) Uani 0.513(7) 1 d . . P B 1
H14A H 0.713986 0.216141 0.125875 0.105 Uiso 0.513(7) 1 calc R U P B 1
H14B H 0.827775 0.187915 0.227327 0.105 Uiso 0.513(7) 1 calc R U P B 1
C4 C 0.5886(8) 0.2416(5) 0.3681(9) 0.104(2) Uani 0.513(7) 1 d . . P B 1
H4A H 0.650994 0.271826 0.436980 0.125 Uiso 0.513(7) 1 calc R U P B 1
H4B H 0.537341 0.181280 0.384575 0.125 Uiso 0.513(7) 1 calc R U P B 1
C7 C 0.3596(15) 0.6024(14) 0.2470(16) 0.124(4) Uani 0.513(7) 1 d . . P B 1
H7A H 0.319666 0.631596 0.294965 0.149 Uiso 0.513(7) 1 calc R U P B 1
H7B H 0.293852 0.568730 0.181655 0.149 Uiso 0.513(7) 1 calc R U P B 1
C2 C 0.7677(6) 0.5734(4) 0.4509(5) 0.109(2) Uani 0.638(8) 1 d . . P A 1
H2A H 0.682173 0.569013 0.451640 0.130 Uiso 0.638(8) 1 calc R U P A 1
H2B H 0.814304 0.639124 0.493416 0.130 Uiso 0.638(8) 1 calc R U P A 1
C12 C 0.8590(12) 0.5051(9) 0.0852(9) 0.124(3) Uani 0.513(7) 1 d . . P B 1
H12A H 0.922326 0.541946 0.150218 0.149 Uiso 0.513(7) 1 calc R U P B 1
H12B H 0.902018 0.477175 0.039126 0.149 Uiso 0.513(7) 1 calc R U P B 1
C6 C 0.3548(12) 0.4299(12) 0.3137(10) 0.118(3) Uani 0.513(7) 1 d . . P B 1
H6A H 0.299957 0.397208 0.242790 0.142 Uiso 0.513(7) 1 calc R U P B 1
H6B H 0.302629 0.449411 0.355195 0.142 Uiso 0.513(7) 1 calc R U P B 1
C2A C 0.8598(9) 0.5308(8) 0.4113(8) 0.108(4) Uani 0.362(8) 1 d . . P A 2
H2AA H 0.929208 0.586629 0.447512 0.130 Uiso 0.362(8) 1 calc R U P A 2
H2AB H 0.890115 0.481689 0.369516 0.130 Uiso 0.362(8) 1 calc R U P A 2
C8 C 0.4384(9) 0.6948(9) 0.2146(12) 0.115(3) Uani 0.513(7) 1 d . . P B 1
H8A H 0.385212 0.749655 0.178987 0.138 Uiso 0.513(7) 1 calc R U P B 1
H8B H 0.504033 0.728935 0.279905 0.138 Uiso 0.513(7) 1 calc R U P B 1
C10 C 0.5983(12) 0.6800(8) 0.0181(10) 0.108(3) Uani 0.513(7) 1 d . . P B 1
H10A H 0.630167 0.735948 -0.020445 0.129 Uiso 0.513(7) 1 calc R U P B 1
H10B H 0.534681 0.630765 -0.036619 0.129 Uiso 0.513(7) 1 calc R U P B 1
O5A O 0.7759(6) 0.4738(7) 0.0817(6) 0.1016(18) Uani 0.487(7) 1 d . . P B 2
O4A O 0.6457(10) 0.6541(6) 0.0882(6) 0.100(2) Uani 0.487(7) 1 d . . P B 2
C10A C 0.6927(14) 0.6344(9) 0.0063(11) 0.125(4) Uani 0.487(7) 1 d . . P B 2
H10C H 0.624381 0.599500 -0.056667 0.150 Uiso 0.487(7) 1 calc R U P B 2
H10D H 0.721466 0.703878 -0.016043 0.150 Uiso 0.487(7) 1 calc R U P B 2
C9A C 0.548(2) 0.7082(17) 0.063(2) 0.153(10) Uani 0.487(7) 1 d . . P B 2
H9AA H 0.482976 0.668913 -0.000220 0.183 Uiso 0.487(7) 1 calc R U P B 2
H9AB H 0.571756 0.777664 0.037413 0.183 Uiso 0.487(7) 1 calc R U P B 2
C11 C 0.7830(7) 0.5756(4) 0.0304(5) 0.156(2) Uani 1 1 d . . . . .
H11A H 0.729935 0.540400 -0.039935 0.188 Uiso 0.513(7) 1 calc R U P B 1
H11B H 0.834827 0.636385 0.015310 0.188 Uiso 0.513(7) 1 calc R U P B 1
H11C H 0.857465 0.620415 0.078316 0.188 Uiso 0.487(7) 1 calc R U P B 2
H11D H 0.798326 0.559870 -0.037168 0.188 Uiso 0.487(7) 1 calc R U P B 2
C8A C 0.4907(13) 0.7300(9) 0.1387(10) 0.118(4) Uani 0.487(7) 1 d . . P B 2
H8AA H 0.415307 0.764607 0.103147 0.141 Uiso 0.487(7) 1 calc R U P B 2
H8AB H 0.547986 0.779851 0.197029 0.141 Uiso 0.487(7) 1 calc R U P B 2
O3A O 0.4584(8) 0.6328(6) 0.1840(6) 0.0967(18) Uani 0.487(7) 1 d . . P B 2
C12A C 0.8754(11) 0.4067(13) 0.1225(9) 0.135(5) Uani 0.487(7) 1 d . . P B 2
H12C H 0.935830 0.438813 0.191514 0.162 Uiso 0.487(7) 1 calc R U P B 2
H12D H 0.918903 0.401284 0.070236 0.162 Uiso 0.487(7) 1 calc R U P B 2
C13A C 0.8208(14) 0.2959(12) 0.1396(15) 0.106(4) Uani 0.487(7) 1 d . . P B 2
H13C H 0.759005 0.264462 0.070929 0.127 Uiso 0.487(7) 1 calc R U P B 2
H13D H 0.886954 0.248594 0.164029 0.127 Uiso 0.487(7) 1 calc R U P B 2
C6A C 0.3568(15) 0.5383(17) 0.2984(12) 0.140(6) Uani 0.487(7) 1 d . . P B 2
H6AA H 0.320655 0.546772 0.355516 0.168 Uiso 0.487(7) 1 calc R U P B 2
H6AB H 0.290754 0.505186 0.232899 0.168 Uiso 0.487(7) 1 calc R U P B 2
O6A O 0.7646(7) 0.3046(5) 0.2174(5) 0.0924(18) Uani 0.487(7) 1 d . . P B 2
O2A O 0.4519(8) 0.4731(7) 0.3323(6) 0.107(2) Uani 0.487(7) 1 d . . P B 2
C14A C 0.7012(9) 0.2031(7) 0.2276(8) 0.102(2) Uani 0.487(7) 1 d . . P B 2
H14C H 0.636705 0.180034 0.157234 0.123 Uiso 0.487(7) 1 calc R U P B 2
H14D H 0.760964 0.149673 0.245102 0.123 Uiso 0.487(7) 1 calc R U P B 2
C4A C 0.5070(13) 0.2976(10) 0.3774(11) 0.118(4) Uani 0.487(7) 1 d . . P B 2
H4AA H 0.571315 0.328796 0.444873 0.142 Uiso 0.487(7) 1 calc R U P B 2
H4AB H 0.474703 0.225842 0.391941 0.142 Uiso 0.487(7) 1 calc R U P B 2
C5A C 0.4004(19) 0.3691(17) 0.3428(19) 0.115(7) Uani 0.487(7) 1 d . . P B 2
H5AA H 0.337584 0.340917 0.273301 0.137 Uiso 0.487(7) 1 calc R U P B 2
H5AB H 0.360024 0.370295 0.397774 0.137 Uiso 0.487(7) 1 calc R U P B 2
O1A O 0.5611(7) 0.2877(6) 0.2954(5) 0.0945(18) Uani 0.487(7) 1 d . . P B 2
C7A C 0.4118(17) 0.6535(14) 0.2727(14) 0.121(4) Uani 0.487(7) 1 d . . P B 2
H7AA H 0.346457 0.701765 0.250365 0.145 Uiso 0.487(7) 1 calc R U P B 2
H7AB H 0.479587 0.686607 0.337079 0.145 Uiso 0.487(7) 1 calc R U P B 2
Cl1 Cl 0.8316(6) 0.4696(4) 0.5085(4) 0.1649(19) Uani 0.638(8) 1 d . . P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S6 2.1699(7) . ?
Ni1 S2 2.1606(7) . ?
Ni1 S1 2.1628(7) . ?
Ni1 S7 2.1584(7) . ?
S6 C18 1.714(2) . ?
S2 C16 1.706(3) . ?
S1 C15 1.712(2) . ?
S7 C19 1.708(2) . ?
S8 C18 1.743(2) . ?
S8 C20 1.730(3) . ?
S9 C19 1.745(2) . ?
S9 C20 1.728(3) . ?
S4 C17 1.718(3) . ?
S4 C16 1.740(2) . ?
S3 C15 1.747(2) . ?
S3 C17 1.725(3) . ?
S10 C20 1.644(2) . ?
S5 C17 1.651(3) . ?
Cl1A C2A 1.893(11) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.477(4) . ?
C18 C19 1.363(3) . ?
C15 C16 1.361(3) . ?
O4 C10 1.485(15) . ?
O4 C11 1.415(10) . ?
O1 C5 1.31(2) . ?
O1 C4 1.390(12) . ?
O3 C9 1.39(2) . ?
O3 C8 1.418(15) . ?
O6 C3 1.416(7) . ?
O6 C14 1.385(11) . ?
C1 H1BC 0.9700 . ?
C1 H1BD 0.9700 . ?
C1 H1AA 0.9700 . ?
C1 H1AB 0.9700 . ?
C1 C2 1.473(6) . ?
C1 C2A 1.396(9) . ?
C3 H3AA 0.9700 . ?
C3 H3AB 0.9700 . ?
C3 H3BC 0.9700 . ?
C3 H3BD 0.9700 . ?
C3 C4 1.340(11) . ?
C3 C14A 1.323(11) . ?
C3 O1A 1.478(10) . ?
O5 C13 1.368(18) . ?
O5 C12 1.460(13) . ?
O2 C7 1.323(19) . ?
O2 C6 1.483(16) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.41(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.506(19) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.519(17) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.530(19) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 Cl1 1.608(8) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C11 1.328(13) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
O5A C11 1.440(10) . ?
O5A C12A 1.429(18) . ?
O4A C10A 1.370(15) . ?
O4A C9A 1.31(3) . ?
C10A H10C 0.9700 . ?
C10A H10D 0.9700 . ?
C10A C11 1.272(15) . ?
C9A H9AA 0.9700 . ?
C9A H9AB 0.9700 . ?
C9A C8A 1.39(3) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 H11C 0.9700 . ?
C11 H11D 0.9700 . ?
C8A H8AA 0.9700 . ?
C8A H8AB 0.9700 . ?
C8A O3A 1.414(14) . ?
O3A C7A 1.449(16) . ?
C12A H12C 0.9700 . ?
C12A H12D 0.9700 . ?
C12A C13A 1.496(18) . ?
C13A H13C 0.9700 . ?
C13A H13D 0.9700 . ?
C13A O6A 1.373(19) . ?
C6A H6AA 0.9700 . ?
C6A H6AB 0.9700 . ?
C6A O2A 1.37(2) . ?
C6A C7A 1.58(2) . ?
O6A C14A 1.411(11) . ?
O2A C5A 1.38(2) . ?
C14A H14C 0.9700 . ?
C14A H14D 0.9700 . ?
C4A H4AA 0.9700 . ?
C4A H4AB 0.9700 . ?
C4A C5A 1.52(2) . ?
C4A O1A 1.407(14) . ?
C5A H5AA 0.9700 . ?
C5A H5AB 0.9700 . ?
C7A H7AA 0.9700 . ?
C7A H7AB 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S2 Ni1 S6 176.67(3) . . ?
S2 Ni1 S1 92.92(3) . . ?
S1 Ni1 S6 88.06(2) . . ?
S7 Ni1 S6 92.94(2) . . ?
S7 Ni1 S2 86.21(2) . . ?
S7 Ni1 S1 177.64(3) . . ?
C18 S6 Ni1 102.10(8) . . ?
C16 S2 Ni1 102.48(9) . . ?
C15 S1 Ni1 102.11(9) . . ?
C19 S7 Ni1 102.34(8) . . ?
C20 S8 C18 97.74(11) . . ?
C20 S9 C19 97.79(12) . . ?
C17 S4 C16 97.68(13) . . ?
C17 S3 C15 97.27(13) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
S6 C18 S8 123.17(14) . . ?
C19 C18 S6 120.98(18) . . ?
C19 C18 S8 115.85(18) . . ?
S7 C19 S9 122.76(14) . . ?
C18 C19 S7 121.50(18) . . ?
C18 C19 S9 115.73(18) . . ?
S1 C15 S3 122.88(15) . . ?
C16 C15 S1 121.37(19) . . ?
C16 C15 S3 115.75(19) . . ?
S4 C17 S3 113.41(14) . . ?
S5 C17 S4 123.06(17) . . ?
S5 C17 S3 123.52(18) . . ?
S9 C20 S8 112.84(13) . . ?
S10 C20 S8 123.49(15) . . ?
S10 C20 S9 123.67(16) . . ?
S2 C16 S4 123.11(15) . . ?
C15 C16 S2 121.10(18) . . ?
C15 C16 S4 115.79(19) . . ?
C11 O4 C10 121.9(9) . . ?
C5 O1 C4 114.1(14) . . ?
C9 O3 C8 115.2(14) . . ?
C14 O6 C3 118.0(6) . . ?
N1 C1 H1BC 109.1 . . ?
N1 C1 H1BD 109.1 . . ?
N1 C1 H1AA 108.8 . . ?
N1 C1 H1AB 108.8 . . ?
H1BC C1 H1BD 107.8 . . ?
H1AA C1 H1AB 107.7 . . ?
C2 C1 N1 113.8(3) . . ?
C2 C1 H1AA 108.8 . . ?
C2 C1 H1AB 108.8 . . ?
C2A C1 N1 112.5(5) . . ?
C2A C1 H1BC 109.1 . . ?
C2A C1 H1BD 109.1 . . ?
O6 C3 H3AA 108.0 . . ?
O6 C3 H3AB 108.0 . . ?
H3AA C3 H3AB 107.2 . . ?
H3BC C3 H3BD 107.4 . . ?
C4 C3 O6 117.2(4) . . ?
C4 C3 H3AA 108.0 . . ?
C4 C3 H3AB 108.0 . . ?
C14A C3 H3BC 108.2 . . ?
C14A C3 H3BD 108.2 . . ?
C14A C3 O1A 116.3(5) . . ?
O1A C3 H3BC 108.2 . . ?
O1A C3 H3BD 108.2 . . ?
C13 O5 C12 112.7(10) . . ?
C7 O2 C6 111.0(11) . . ?
O3 C9 H9A 109.4 . . ?
O3 C9 H9B 109.4 . . ?
O3 C9 C10 111.1(16) . . ?
H9A C9 H9B 108.0 . . ?
C10 C9 H9A 109.4 . . ?
C10 C9 H9B 109.4 . . ?
O1 C5 H5A 109.4 . . ?
O1 C5 H5B 109.4 . . ?
O1 C5 C6 111.2(19) . . ?
H5A C5 H5B 108.0 . . ?
C6 C5 H5A 109.4 . . ?
C6 C5 H5B 109.4 . . ?
O5 C13 H13A 110.2 . . ?
O5 C13 H13B 110.2 . . ?
O5 C13 C14 107.7(10) . . ?
H13A C13 H13B 108.5 . . ?
C14 C13 H13A 110.2 . . ?
C14 C13 H13B 110.2 . . ?
O6 C14 C13 110.9(9) . . ?
O6 C14 H14A 109.5 . . ?
O6 C14 H14B 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 108.0 . . ?
O1 C4 H4A 109.1 . . ?
O1 C4 H4B 109.1 . . ?
C3 C4 O1 112.7(10) . . ?
C3 C4 H4A 109.1 . . ?
C3 C4 H4B 109.1 . . ?
H4A C4 H4B 107.8 . . ?
O2 C7 H7A 109.6 . . ?
O2 C7 H7B 109.6 . . ?
O2 C7 C8 110.3(12) . . ?
H7A C7 H7B 108.1 . . ?
C8 C7 H7A 109.6 . . ?
C8 C7 H7B 109.6 . . ?
C1 C2 H2A 109.0 . . ?
C1 C2 H2B 109.0 . . ?
C1 C2 Cl1 113.0(4) . . ?
H2A C2 H2B 107.8 . . ?
Cl1 C2 H2A 109.0 . . ?
Cl1 C2 H2B 109.0 . . ?
O5 C12 H12A 109.4 . . ?
O5 C12 H12B 109.4 . . ?
H12A C12 H12B 108.0 . . ?
C11 C12 O5 111.0(10) . . ?
C11 C12 H12A 109.4 . . ?
C11 C12 H12B 109.4 . . ?
O2 C6 C5 108.7(15) . . ?
O2 C6 H6A 110.0 . . ?
O2 C6 H6B 110.0 . . ?
C5 C6 H6A 110.0 . . ?
C5 C6 H6B 110.0 . . ?
H6A C6 H6B 108.3 . . ?
Cl1A C2A H2AA 107.7 . . ?
Cl1A C2A H2AB 107.7 . . ?
C1 C2A Cl1A 118.6(7) . . ?
C1 C2A H2AA 107.7 . . ?
C1 C2A H2AB 107.7 . . ?
H2AA C2A H2AB 107.1 . . ?
O3 C8 C7 109.4(10) . . ?
O3 C8 H8A 109.8 . . ?
O3 C8 H8B 109.8 . . ?
C7 C8 H8A 109.8 . . ?
C7 C8 H8B 109.8 . . ?
H8A C8 H8B 108.2 . . ?
O4 C10 H10A 108.8 . . ?
O4 C10 H10B 108.8 . . ?
C9 C10 O4 113.6(14) . . ?
C9 C10 H10A 108.8 . . ?
C9 C10 H10B 108.8 . . ?
H10A C10 H10B 107.7 . . ?
C12A O5A C11 126.4(10) . . ?
C9A O4A C10A 116.7(15) . . ?
O4A C10A H10C 108.3 . . ?
O4A C10A H10D 108.3 . . ?
H10C C10A H10D 107.4 . . ?
C11 C10A O4A 115.9(14) . . ?
C11 C10A H10C 108.3 . . ?
C11 C10A H10D 108.3 . . ?
O4A C9A H9AA 107.0 . . ?
O4A C9A H9AB 107.0 . . ?
O4A C9A C8A 121.3(16) . . ?
H9AA C9A H9AB 106.7 . . ?
C8A C9A H9AA 107.0 . . ?
C8A C9A H9AB 107.0 . . ?
O4 C11 H11A 107.8 . . ?
O4 C11 H11B 107.8 . . ?
C12 C11 O4 117.9(6) . . ?
C12 C11 H11A 107.8 . . ?
C12 C11 H11B 107.8 . . ?
O5A C11 H11C 107.0 . . ?
O5A C11 H11D 107.0 . . ?
C10A C11 O5A 121.5(6) . . ?
C10A C11 H11C 107.0 . . ?
C10A C11 H11D 107.0 . . ?
H11A C11 H11B 107.2 . . ?
H11C C11 H11D 106.7 . . ?
C9A C8A H8AA 109.5 . . ?
C9A C8A H8AB 109.5 . . ?
C9A C8A O3A 110.6(13) . . ?
H8AA C8A H8AB 108.1 . . ?
O3A C8A H8AA 109.5 . . ?
O3A C8A H8AB 109.5 . . ?
C8A O3A C7A 112.2(12) . . ?
O5A C12A H12C 109.9 . . ?
O5A C12A H12D 109.9 . . ?
O5A C12A C13A 109.1(11) . . ?
H12C C12A H12D 108.3 . . ?
C13A C12A H12C 109.9 . . ?
C13A C12A H12D 109.9 . . ?
C12A C13A H13C 109.9 . . ?
C12A C13A H13D 109.9 . . ?
H13C C13A H13D 108.3 . . ?
O6A C13A C12A 109.1(10) . . ?
O6A C13A H13C 109.9 . . ?
O6A C13A H13D 109.9 . . ?
H6AA C6A H6AB 108.3 . . ?
O2A C6A H6AA 109.8 . . ?
O2A C6A H6AB 109.8 . . ?
O2A C6A C7A 109.2(13) . . ?
C7A C6A H6AA 109.8 . . ?
C7A C6A H6AB 109.8 . . ?
C13A O6A C14A 110.5(10) . . ?
C6A O2A C5A 108.7(12) . . ?
C3 C14A O6A 114.0(9) . . ?
C3 C14A H14C 108.8 . . ?
C3 C14A H14D 108.8 . . ?
O6A C14A H14C 108.8 . . ?
O6A C14A H14D 108.8 . . ?
H14C C14A H14D 107.6 . . ?
H4AA C4A H4AB 108.0 . . ?
C5A C4A H4AA 109.4 . . ?
C5A C4A H4AB 109.3 . . ?
O1A C4A H4AA 109.3 . . ?
O1A C4A H4AB 109.3 . . ?
O1A C4A C5A 111.4(14) . . ?
O2A C5A C4A 107.7(15) . . ?
O2A C5A H5AA 110.2 . . ?
O2A C5A H5AB 110.2 . . ?
C4A C5A H5AA 110.2 . . ?
C4A C5A H5AB 110.2 . . ?
H5AA C5A H5AB 108.5 . . ?
C4A O1A C3 119.1(8) . . ?
O3A C7A C6A 105.6(9) . . ?
O3A C7A H7AA 110.6 . . ?
O3A C7A H7AB 110.6 . . ?
C6A C7A H7AA 110.6 . . ?
C6A C7A H7AB 110.6 . . ?
H7AA C7A H7AB 108.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S6 C18 S8 177.23(12) . . . . ?
Ni1 S6 C18 C19 -2.7(2) . . . . ?
Ni1 S2 C16 S4 -178.14(12) . . . . ?
Ni1 S2 C16 C15 1.3(2) . . . . ?
Ni1 S1 C15 S3 -178.86(12) . . . . ?
Ni1 S1 C15 C16 1.2(2) . . . . ?
Ni1 S7 C19 S9 -178.72(13) . . . . ?
Ni1 S7 C19 C18 2.4(2) . . . . ?
S6 C18 C19 S7 0.2(3) . . . . ?
S6 C18 C19 S9 -178.71(12) . . . . ?
S1 C15 C16 S2 -1.8(3) . . . . ?
S1 C15 C16 S4 177.67(11) . . . . ?
S8 C18 C19 S7 -179.73(12) . . . . ?
S8 C18 C19 S9 1.3(3) . . . . ?
S3 C15 C16 S2 178.29(12) . . . . ?
S3 C15 C16 S4 -2.3(3) . . . . ?
N1 C1 C2 Cl1 75.1(6) . . . . ?
N1 C1 C2A Cl1A -71.7(8) . . . . ?
C18 S8 C20 S9 1.81(15) . . . . ?
C18 S8 C20 S10 -177.71(16) . . . . ?
C19 S9 C20 S8 -1.24(16) . . . . ?
C19 S9 C20 S10 178.29(16) . . . . ?
C15 S3 C17 S4 -2.83(16) . . . . ?
C15 S3 C17 S5 178.48(17) . . . . ?
C17 S4 C16 S2 179.67(15) . . . . ?
C17 S4 C16 C15 0.2(2) . . . . ?
C17 S3 C15 S1 -176.84(15) . . . . ?
C17 S3 C15 C16 3.1(2) . . . . ?
C20 S8 C18 S6 178.13(15) . . . . ?
C20 S8 C18 C19 -1.9(2) . . . . ?
C20 S9 C19 S7 -178.96(15) . . . . ?
C20 S9 C19 C18 0.0(2) . . . . ?
C16 S4 C17 S3 1.87(16) . . . . ?
C16 S4 C17 S5 -179.44(16) . . . . ?
O1 C5 C6 O2 -60.7(19) . . . . ?
O3 C9 C10 O4 -58.9(17) . . . . ?
O6 C3 C4 O1 54.5(8) . . . . ?
C3 O6 C14 C13 -174.1(8) . . . . ?
O5 C13 C14 O6 -62.6(12) . . . . ?
O5 C12 C11 O4 53.7(10) . . . . ?
O2 C7 C8 O3 61.0(14) . . . . ?
C9 O3 C8 C7 164.9(13) . . . . ?
C5 O1 C4 C3 172.6(12) . . . . ?
C13 O5 C12 C11 177.3(9) . . . . ?
C14 O6 C3 C4 -177.3(6) . . . . ?
C4 O1 C5 C6 -175.7(12) . . . . ?
C7 O2 C6 C5 -178.4(15) . . . . ?
C12 O5 C13 C14 -177.1(9) . . . . ?
C6 O2 C7 C8 -170.5(10) . . . . ?
C8 O3 C9 C10 177.8(12) . . . . ?
C10 O4 C11 C12 -167.8(8) . . . . ?
O5A C12A C13A O6A -62.2(13) . . . . ?
O4A C10A C11 O5A 49.0(12) . . . . ?
O4A C9A C8A O3A -54(2) . . . . ?
C10A O4A C9A C8A 178.4(15) . . . . ?
C9A O4A C10A C11 -175.5(13) . . . . ?
C9A C8A O3A C7A 173.5(14) . . . . ?
C11 O4 C10 C9 -171.3(9) . . . . ?
C11 O5A C12A C13A -164.2(9) . . . . ?
C8A O3A C7A C6A 169.7(11) . . . . ?
C12A O5A C11 C10A -173.2(10) . . . . ?
C12A C13A O6A C14A 174.2(10) . . . . ?
C13A O6A C14A C3 178.0(9) . . . . ?
C6A O2A C5A C4A 178.4(13) . . . . ?
O2A C6A C7A O3A 61.8(13) . . . . ?
C14A C3 O1A C4A -176.3(7) . . . . ?
C5A C4A O1A C3 -167.6(10) . . . . ?
O1A C3 C14A O6A 53.6(8) . . . . ?
O1A C4A C5A O2A -64.3(17) . . . . ?
C7A C6A O2A C5A -173.4(13) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.136
_oxdiff_exptl_absorpt_empirical_full_min 0.588
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_93k-f-2
_database_code_depnum_ccdc_archive 'CCDC 2053391'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-18 downloaded from the CCDC.
;
_audit_creation_date             2020-11-13
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C2 H7 Cl N, C12 H24 O6'
_chemical_formula_sum            'C20 H31 Cl N Ni O6 S10'
_chemical_formula_weight         796.22
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHNONiSBr
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.2803(3)
_cell_length_b                   12.3375(2)
_cell_length_c                   12.8611(3)
_cell_angle_alpha                91.103(2)
_cell_angle_beta                 110.634(2)
_cell_angle_gamma                96.375(2)
_cell_volume                     1661.43(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    26461
_cell_measurement_temperature    273
_cell_measurement_theta_max      30.8120
_cell_measurement_theta_min      2.1050
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.328
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64798
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             822
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.41
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.830
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            49247
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.830
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.071
_diffrn_reflns_theta_min         2.074
_diffrn_ambient_temperature      273
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.830
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     39.00  78.00   0.50    0.17    --    5.18  28.00-126.00   78
  2  ω    -28.00  19.00   0.50    0.17    --    5.18 -28.00-145.15   94
  3  ω    -69.00 -40.00   0.50    0.17    --    5.18 -28.00-145.15   58
  4  ω    -68.00  19.00   0.50    0.17    --    5.18 -28.00 -97.58  174
  5  ω    -66.00  19.00   0.50    0.17    --    5.18 -28.00 -48.73  170
  6  ω    -69.00  19.00   0.50    0.17    --    5.18 -28.00  -2.06  176
  7  ω    -68.00  19.00   0.50    0.17    --    5.18 -28.00  71.00  174
  8  ω    -70.00  18.00   0.50    0.17    --    5.18 -25.00 132.92  176
  9  ω    -78.00 -40.00   0.50    0.17    --   -5.03 -28.00  71.00   76
 10  ω    -39.00   5.00   0.50    0.17    --   -5.03 -37.00-150.00   88
 11  ω    -75.00 -42.00   0.50    0.17    --   -5.03 -37.00-150.00   66
 12  ω    -11.00  28.00   0.50    0.17    --   -5.03 -99.00 -60.00   78
 13  ω    -18.00  27.00   0.50    0.17    --   -5.03 -99.00-180.00   90
 14  ω      3.00  39.00   0.50    0.17    --    5.18 -99.00-150.00   72
 15  ω     -2.00  24.00   0.50    0.17    --   -5.03  28.00-126.00   52
 16  ω     39.00  65.00   0.50    0.17    --   -5.03  28.00-126.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0017497000
_diffrn_orient_matrix_UB_12      -0.0190071000
_diffrn_orient_matrix_UB_13      -0.0529859000
_diffrn_orient_matrix_UB_21      0.0675837000
_diffrn_orient_matrix_UB_22      0.0100648000
_diffrn_orient_matrix_UB_23      0.0186456000
_diffrn_orient_matrix_UB_31      0.0040710000
_diffrn_orient_matrix_UB_32      -0.0538257000
_diffrn_orient_matrix_UB_33      0.0182058000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6557
_reflns_number_total             8848
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         8848
_refine_ls_number_restraints     39
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0389
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1292
_refine_ls_wR_factor_ref         0.1449
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
2. Restrained distances
 O4-C12 \\sim O4A-C11
 with sigma of 0.04
 C7-C6 \\sim C6A-C5A
 with sigma of 0.04
 O3-C9 \\sim O3A-C8A
 with sigma of 0.02
 O1-C6 \\sim O1A-C5A
 with sigma of 0.04
 O5-C14 \\sim O5A-C13A
 with sigma of 0.04
 O6-C14 \\sim O6A-C13A
 with sigma of 0.02
 O1-O2 \\sim O1A-O2A
 with sigma of 0.04
 C13-C12 \\sim C12A-C11
 with sigma of 0.04
 O6-C13 \\sim O6A-C12A
 with sigma of 0.04
 O5-C13 \\sim O5A-C12A
 with sigma of 0.02
 C5-C7 \\sim C4A-C6A
 with sigma of 0.04
 O5-C12 \\sim O5A-C11
 with sigma of 0.02
 O4-C9 \\sim O4A-C8A
 with sigma of 0.04
 O2-C5 \\sim O2A-C4A
 with sigma of 0.02
 O1-C5 \\sim O1A-C4A
 with sigma of 0.04
 O2-C6 \\sim O2A-C5A
 with sigma of 0.04
 O3-C10 \\sim O3A-C9A
 with sigma of 0.04
 C9-C10 \\sim C8A-C9A
 with sigma of 0.02
 O2-C7 \\sim O2A-C6A
 with sigma of 0.02
 C5-C6 \\sim C4A-C5A
 with sigma of 0.02
 O3-C7 \\sim O3A-C6A
 with sigma of 0.04
 C13-C14 \\sim C12A-C13A
 with sigma of 0.02
 O4-C10 \\sim O4A-C9A
 with sigma of 0.02
 C3-C14 \\sim C14A-C13A
 with sigma of 0.04
 O1-C3 \\sim O1A-C14A
 with sigma of 0.04
 C3-C5 \\sim C14A-C4A
 with sigma of 0.04
 O6-C3 \\sim O6A-C14A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C6A \\sim C7A \\sim O3A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
4. Others
 Sof(H1d)=Sof(H1e)=Sof(C2A)=Sof(H2Aa)=Sof(H2Ab)=1-FVAR(1)
 Sof(H00Z)=Sof(H)=Sof(C2)=Sof(H01E)=Sof(H01F)=FVAR(1)
 Sof(H3c)=Sof(H3d)=Sof(O5A)=Sof(O4A)=Sof(C10A)=Sof(H10c)=Sof(H10d)=Sof(C9A)=
 Sof(H9Aa)=Sof(H9Ab)=Sof(H11a)=Sof(H11b)=Sof(C8A)=Sof(H8Aa)=Sof(H8Ab)=Sof(O3A)=
 Sof(C12A)=Sof(H12a)=Sof(H12b)=Sof(C13A)=Sof(H13a)=Sof(H13b)=Sof(C6A)=Sof(H6Aa)=
 Sof(H6Ab)=Sof(O6A)=Sof(O2A)=Sof(C14A)=Sof(H14a)=Sof(H14b)=Sof(C4A)=Sof(H4Aa)=
 Sof(H4Ab)=Sof(C5A)=Sof(H5Aa)=Sof(H5Ab)=Sof(O1A)=Sof(C7A)=Sof(H7Aa)=Sof(H7Ab)=1-
 FVAR(2)
 Sof(O4)=Sof(O1)=Sof(O3)=Sof(O6)=Sof(H00A)=Sof(H00B)=Sof(O5)=Sof(O2)=Sof(C9)=
 Sof(H00E)=Sof(H00F)=Sof(C5)=Sof(H00G)=Sof(H00H)=Sof(C13)=Sof(H00I)=Sof(H00J)=
 Sof(C14)=Sof(H00K)=Sof(H00L)=Sof(C4)=Sof(H00M)=Sof(H00N)=Sof(C7)=Sof(H00O)=
 Sof(H00P)=Sof(C12)=Sof(H01A)=Sof(H01B)=Sof(C6)=Sof(H01C)=Sof(H01D)=Sof(C8)=
 Sof(H3A)=Sof(H3B)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H0AA)=Sof(H0AB)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C1(H00Z,H), C1(H1d,H1e), C3(H00A,H00B), C3(H3c,H3d), C9(H00E,H00F), C5(H00G,
 H00H), C13(H00I,H00J), C14(H00K,H00L), C4(H00M,H00N), C7(H00O,H00P), C2(H01E,
 H01F), C12(H01A,H01B), C6(H01C,H01D), C2A(H2Aa,H2Ab), C8(H3A,H3B), C10(H10A,
 H10B), C10A(H10c,H10d), C9A(H9Aa,H9Ab), C11(H0AA,H0AB), C11(H11a,H11b),
 C8A(H8Aa,H8Ab), C12A(H12a,H12b), C13A(H13a,H13b), C6A(H6Aa,H6Ab), C14A(H14a,
 H14b), C4A(H4Aa,H4Ab), C5A(H5Aa,H5Ab), C7A(H7Aa,H7Ab)
5.b Idealised Me refined as rotating group:
 N1(H1a,H1b,H1c)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.84535(2) 0.88972(2) 0.51238(2) 0.04337(10) Uani 1 1 d . . . . .
S6 S 0.69211(5) 0.97542(5) 0.52309(4) 0.05337(15) Uani 1 1 d . . . . .
S2 S 1.00575(5) 0.81210(5) 0.50715(5) 0.05371(15) Uani 1 1 d . . . . .
S1 S 0.79025(6) 0.92898(5) 0.34004(5) 0.05420(15) Uani 1 1 d . . . . .
S7 S 0.89916(6) 0.84464(5) 0.68256(5) 0.05538(15) Uani 1 1 d . . . . .
S8 S 0.61387(5) 1.02562(5) 0.72057(5) 0.05337(15) Uani 1 1 d . . . . .
S9 S 0.80201(6) 0.90268(5) 0.86532(5) 0.05771(16) Uani 1 1 d . . . . .
S4 S 1.09927(6) 0.77123(5) 0.31802(5) 0.05891(16) Uani 1 1 d . . . . .
S3 S 0.90742(6) 0.88595(5) 0.16637(5) 0.05887(16) Uani 1 1 d . . . . .
S10 S 0.62634(7) 1.00295(5) 0.95390(6) 0.06728(18) Uani 1 1 d . . . . .
S5 S 1.08939(7) 0.78584(7) 0.08526(6) 0.0735(2) Uani 1 1 d . . . . .
Cl1 Cl 0.83047(10) 0.45903(8) 0.51437(7) 0.1066(3) Uani 1 1 d . . . . .
N1 N 0.66544(17) 0.50180(13) 0.25551(15) 0.0517(4) Uani 1 1 d . . . . .
H1A H 0.658676 0.518005 0.186674 0.062 Uiso 1 1 calc R U . . .
H1B H 0.590360 0.503331 0.263401 0.062 Uiso 1 1 calc R U . . .
H1C H 0.689102 0.435350 0.267786 0.062 Uiso 1 1 calc R U . . .
C18 C 0.7088(2) 0.96529(15) 0.66061(17) 0.0446(4) Uani 1 1 d . . . . .
C19 C 0.7977(2) 0.90830(16) 0.72897(17) 0.0457(4) Uani 1 1 d . . . . .
C15 C 0.9032(2) 0.87633(16) 0.30040(17) 0.0468(4) Uani 1 1 d . . . . .
C17 C 1.0344(2) 0.81306(18) 0.1845(2) 0.0543(5) Uani 1 1 d . . . . .
C20 C 0.6787(2) 0.97824(17) 0.85261(19) 0.0506(5) Uani 1 1 d . . . . .
C16 C 0.9945(2) 0.82433(16) 0.37187(18) 0.0476(4) Uani 1 1 d . . . . .
O4 O 0.7047(5) 0.6195(3) 0.0798(3) 0.0665(10) Uani 0.546(4) 1 d D . P A 1
O1 O 0.5095(4) 0.3191(3) 0.3157(4) 0.0673(10) Uani 0.546(4) 1 d D . P A 1
O3 O 0.4921(4) 0.6520(3) 0.1419(4) 0.0698(11) Uani 0.546(4) 1 d D . P A 1
O6 O 0.7214(3) 0.2821(2) 0.2648(3) 0.0585(9) Uani 0.546(4) 1 d D . P A 1
C1 C 0.7628(3) 0.5833(2) 0.3369(2) 0.0724(7) Uani 1 1 d . . . . .
H00Z H 0.846257 0.574585 0.334555 0.087 Uiso 0.690(7) 1 calc R U P B 1
H H 0.744602 0.656215 0.314991 0.087 Uiso 0.690(7) 1 calc R U P B 1
H1D H 0.798284 0.636061 0.297371 0.087 Uiso 0.310(7) 1 calc R U P B 2
H1E H 0.722700 0.622295 0.379070 0.087 Uiso 0.310(7) 1 calc R U P B 2
C3 C 0.6466(3) 0.2030(2) 0.3034(4) 0.0933(11) Uani 1 1 d D . . . .
H00A H 0.581766 0.163293 0.238858 0.112 Uiso 0.546(4) 1 calc R U P A 1
H00B H 0.701686 0.150953 0.343692 0.112 Uiso 0.546(4) 1 calc R U P A 1
H3C H 0.714132 0.213267 0.376023 0.112 Uiso 0.454(4) 1 calc R U P A 2
H3D H 0.599012 0.131500 0.299150 0.112 Uiso 0.454(4) 1 calc R U P A 2
O5 O 0.7898(4) 0.4148(4) 0.1165(4) 0.0699(10) Uani 0.546(4) 1 d D . P A 1
O2 O 0.4313(5) 0.5268(4) 0.2980(4) 0.0798(12) Uani 0.546(4) 1 d D . P A 1
C9 C 0.5520(11) 0.7325(7) 0.0934(8) 0.082(3) Uani 0.546(4) 1 d D . P A 1
H00E H 0.620881 0.776924 0.151309 0.099 Uiso 0.546(4) 1 calc R U P A 1
H00F H 0.490779 0.779824 0.052469 0.099 Uiso 0.546(4) 1 calc R U P A 1
C5 C 0.4342(16) 0.3497(11) 0.3717(13) 0.091(4) Uani 0.546(4) 1 d D . P A 1
H00G H 0.487858 0.379723 0.445798 0.109 Uiso 0.546(4) 1 calc R U P A 1
H00H H 0.380007 0.285980 0.379458 0.109 Uiso 0.546(4) 1 calc R U P A 1
C13 C 0.8255(10) 0.3040(8) 0.1395(8) 0.090(2) Uani 0.546(4) 1 d D . P A 1
H00I H 0.806210 0.265265 0.067950 0.108 Uiso 0.546(4) 1 calc R U P A 1
H00J H 0.917572 0.311921 0.176139 0.108 Uiso 0.546(4) 1 calc R U P A 1
C14 C 0.7813(5) 0.2449(5) 0.1933(5) 0.0672(14) Uani 0.546(4) 1 d D . P A 1
H00K H 0.849952 0.206380 0.238721 0.081 Uiso 0.546(4) 1 calc R U P A 1
H00L H 0.719268 0.190479 0.140810 0.081 Uiso 0.546(4) 1 calc R U P A 1
C4 C 0.5889(6) 0.2394(4) 0.3683(5) 0.0775(16) Uani 0.546(4) 1 d . . P A 1
H00M H 0.652599 0.271231 0.437797 0.093 Uiso 0.546(4) 1 calc R U P A 1
H00N H 0.537632 0.178756 0.385237 0.093 Uiso 0.546(4) 1 calc R U P A 1
C7 C 0.3548(8) 0.6077(9) 0.2397(9) 0.094(2) Uani 0.546(4) 1 d D . P A 1
H00O H 0.313340 0.638139 0.286035 0.113 Uiso 0.546(4) 1 calc R U P A 1
H00P H 0.289088 0.574165 0.172085 0.113 Uiso 0.546(4) 1 calc R U P A 1
C2 C 0.7668(5) 0.5730(3) 0.4522(3) 0.0801(15) Uani 0.690(7) 1 d . . P B 1
H01E H 0.680553 0.570735 0.452241 0.096 Uiso 0.690(7) 1 calc R U P B 1
H01F H 0.816688 0.637726 0.496985 0.096 Uiso 0.690(7) 1 calc R U P B 1
C12 C 0.8578(7) 0.5050(6) 0.0833(6) 0.0867(18) Uani 0.546(4) 1 d D . P A 1
H01A H 0.923170 0.542221 0.149118 0.104 Uiso 0.546(4) 1 calc R U P A 1
H01B H 0.900241 0.476876 0.036624 0.104 Uiso 0.546(4) 1 calc R U P A 1
C6 C 0.3527(6) 0.4332(7) 0.3116(6) 0.0885(19) Uani 0.546(4) 1 d D . P A 1
H01C H 0.295119 0.402009 0.239210 0.106 Uiso 0.546(4) 1 calc R U P A 1
H01D H 0.301646 0.454733 0.353585 0.106 Uiso 0.546(4) 1 calc R U P A 1
C2A C 0.8611(8) 0.5315(7) 0.4101(7) 0.074(3) Uani 0.310(7) 1 d . . P B 2
H2AA H 0.933314 0.586899 0.445502 0.088 Uiso 0.310(7) 1 calc R U P B 2
H2AB H 0.887512 0.481508 0.365773 0.088 Uiso 0.310(7) 1 calc R U P B 2
C8 C 0.4384(6) 0.6970(5) 0.2114(8) 0.089(2) Uani 0.546(4) 1 d . . P A 1
H3A H 0.387963 0.753320 0.174495 0.107 Uiso 0.546(4) 1 calc R U P A 1
H3B H 0.504953 0.730004 0.278776 0.107 Uiso 0.546(4) 1 calc R U P A 1
C10 C 0.6031(7) 0.6794(5) 0.0175(6) 0.0796(17) Uani 0.546(4) 1 d D . P A 1
H10A H 0.535654 0.630085 -0.036545 0.096 Uiso 0.546(4) 1 calc R U P A 1
H10B H 0.634976 0.734296 -0.022398 0.096 Uiso 0.546(4) 1 calc R U P A 1
O5A O 0.7750(4) 0.4744(5) 0.0810(4) 0.0678(12) Uani 0.454(4) 1 d D . P A 2
O4A O 0.6470(6) 0.6545(4) 0.0886(4) 0.0685(13) Uani 0.454(4) 1 d D . P A 2
C10A C 0.6996(10) 0.6351(6) 0.0038(7) 0.091(3) Uani 0.454(4) 1 d . . P A 2
H10C H 0.630943 0.602828 -0.062699 0.110 Uiso 0.454(4) 1 calc R U P A 2
H10D H 0.733336 0.704954 -0.014548 0.110 Uiso 0.454(4) 1 calc R U P A 2
C9A C 0.5324(11) 0.7062(9) 0.0481(8) 0.076(3) Uani 0.454(4) 1 d D . P A 2
H9AA H 0.466000 0.658170 -0.008376 0.091 Uiso 0.454(4) 1 calc R U P A 2
H9AB H 0.548717 0.773263 0.014490 0.091 Uiso 0.454(4) 1 calc R U P A 2
C11 C 0.7837(6) 0.5760(3) 0.0287(4) 0.1221(17) Uani 1 1 d D . . . .
H0AA H 0.729088 0.541305 -0.043131 0.146 Uiso 0.546(4) 1 calc R U P A 1
H0AB H 0.837580 0.636617 0.014753 0.146 Uiso 0.546(4) 1 calc R U P A 1
H11A H 0.860610 0.620294 0.077265 0.146 Uiso 0.454(4) 1 calc R U P A 2
H11B H 0.798471 0.558363 -0.039238 0.146 Uiso 0.454(4) 1 calc R U P A 2
C8A C 0.4898(8) 0.7308(6) 0.1409(7) 0.0790(19) Uani 0.454(4) 1 d D . P A 2
H8AA H 0.557530 0.776412 0.198576 0.095 Uiso 0.454(4) 1 calc R U P A 2
H8AB H 0.416307 0.770531 0.114606 0.095 Uiso 0.454(4) 1 calc R U P A 2
O3A O 0.4572(5) 0.6334(4) 0.1848(5) 0.0669(13) Uani 0.454(4) 1 d D U P A 2
C12A C 0.8760(7) 0.4106(7) 0.1234(6) 0.085(2) Uani 0.454(4) 1 d D . P A 2
H12A H 0.889778 0.377900 0.060031 0.102 Uiso 0.454(4) 1 calc R U P A 2
H12B H 0.952334 0.460417 0.163325 0.102 Uiso 0.454(4) 1 calc R U P A 2
C13A C 0.8695(8) 0.3419(8) 0.1809(8) 0.073(2) Uani 0.454(4) 1 d D . P A 2
H13A H 0.943083 0.360122 0.248724 0.087 Uiso 0.454(4) 1 calc R U P A 2
H13B H 0.885589 0.277236 0.146405 0.087 Uiso 0.454(4) 1 calc R U P A 2
C6A C 0.3583(9) 0.5457(10) 0.2977(8) 0.095(3) Uani 0.454(4) 1 d D U P A 2
H6AA H 0.322884 0.557471 0.355033 0.115 Uiso 0.454(4) 1 calc R U P A 2
H6AB H 0.289502 0.513175 0.231479 0.115 Uiso 0.454(4) 1 calc R U P A 2
O6A O 0.7654(5) 0.3052(4) 0.2175(4) 0.0655(12) Uani 0.454(4) 1 d D . P A 2
O2A O 0.4524(5) 0.4732(5) 0.3345(5) 0.0761(14) Uani 0.454(4) 1 d D . P A 2
C14A C 0.6987(7) 0.2036(4) 0.2275(6) 0.0736(18) Uani 0.454(4) 1 d D . P A 2
H14A H 0.632187 0.181327 0.156067 0.088 Uiso 0.454(4) 1 calc R U P A 2
H14B H 0.757684 0.149346 0.243630 0.088 Uiso 0.454(4) 1 calc R U P A 2
C4A C 0.5058(9) 0.2929(6) 0.3748(8) 0.082(2) Uani 0.454(4) 1 d D . P A 2
H4AA H 0.572130 0.315792 0.446183 0.098 Uiso 0.454(4) 1 calc R U P A 2
H4AB H 0.465311 0.221000 0.381275 0.098 Uiso 0.454(4) 1 calc R U P A 2
C5A C 0.4093(19) 0.3707(13) 0.349(2) 0.112(7) Uani 0.454(4) 1 d D . P A 2
H5AA H 0.338759 0.342982 0.281629 0.134 Uiso 0.454(4) 1 calc R U P A 2
H5AB H 0.376122 0.373036 0.408849 0.134 Uiso 0.454(4) 1 calc R U P A 2
O1A O 0.5608(5) 0.2859(4) 0.2953(4) 0.0685(13) Uani 0.454(4) 1 d D . P A 2
C7A C 0.4152(12) 0.6544(10) 0.2719(9) 0.089(3) Uani 0.454(4) 1 d . U P A 2
H7AA H 0.351457 0.704495 0.250392 0.106 Uiso 0.454(4) 1 calc R U P A 2
H7AB H 0.486063 0.686848 0.336811 0.106 Uiso 0.454(4) 1 calc R U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S6 2.1664(6) . ?
Ni1 S2 2.1595(6) . ?
Ni1 S1 2.1612(6) . ?
Ni1 S7 2.1572(6) . ?
S6 C18 1.720(2) . ?
S2 C16 1.710(2) . ?
S1 C15 1.713(2) . ?
S7 C19 1.717(2) . ?
S8 C18 1.741(2) . ?
S8 C20 1.737(2) . ?
S9 C19 1.740(2) . ?
S9 C20 1.722(2) . ?
S4 C17 1.727(2) . ?
S4 C16 1.743(2) . ?
S3 C15 1.747(2) . ?
S3 C17 1.724(2) . ?
S10 C20 1.645(2) . ?
S5 C17 1.648(2) . ?
Cl1 C2 1.730(5) . ?
Cl1 C2A 1.739(8) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.489(3) . ?
C18 C19 1.353(3) . ?
C15 C16 1.349(3) . ?
O4 C10 1.437(8) . ?
O4 C11 1.422(7) . ?
O1 C5 1.369(14) . ?
O1 C4 1.422(8) . ?
O3 C9 1.416(11) . ?
O3 C8 1.383(10) . ?
O6 C3 1.430(4) . ?
O6 C14 1.415(7) . ?
C1 H00Z 0.9700 . ?
C1 H 0.9700 . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C1 C2 1.476(5) . ?
C1 C2A 1.402(8) . ?
C3 H00A 0.9700 . ?
C3 H00B 0.9700 . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C3 C4 1.324(8) . ?
C3 C14A 1.306(8) . ?
C3 O1A 1.465(7) . ?
O5 C13 1.473(9) . ?
O5 C12 1.439(7) . ?
O2 C7 1.437(10) . ?
O2 C6 1.428(9) . ?
C9 H00E 0.9700 . ?
C9 H00F 0.9700 . ?
C9 C10 1.472(13) . ?
C5 H00G 0.9700 . ?
C5 H00H 0.9700 . ?
C5 C6 1.499(17) . ?
C13 H00I 0.9700 . ?
C13 H00J 0.9700 . ?
C13 C14 1.201(10) . ?
C14 H00K 0.9700 . ?
C14 H00L 0.9700 . ?
C4 H00M 0.9700 . ?
C4 H00N 0.9700 . ?
C7 H00O 0.9700 . ?
C7 H00P 0.9700 . ?
C7 C8 1.505(12) . ?
C2 H01E 0.9700 . ?
C2 H01F 0.9700 . ?
C12 H01A 0.9700 . ?
C12 H01B 0.9700 . ?
C12 C11 1.316(8) . ?
C6 H01C 0.9700 . ?
C6 H01D 0.9700 . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?
C8 H3A 0.9700 . ?
C8 H3B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
O5A C11 1.445(7) . ?
O5A C12A 1.412(9) . ?
O4A C10A 1.441(11) . ?
O4A C9A 1.439(12) . ?
C10A H10C 0.9700 . ?
C10A H10D 0.9700 . ?
C10A C11 1.218(10) . ?
C9A H9AA 0.9700 . ?
C9A H9AB 0.9700 . ?
C9A C8A 1.473(14) . ?
C11 H0AA 0.9700 . ?
C11 H0AB 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C8A H8AA 0.9700 . ?
C8A H8AB 0.9700 . ?
C8A O3A 1.405(9) . ?
O3A C7A 1.391(12) . ?
C12A H12A 0.9700 . ?
C12A H12B 0.9700 . ?
C12A C13A 1.149(12) . ?
C13A H13A 0.9700 . ?
C13A H13B 0.9700 . ?
C13A O6A 1.444(10) . ?
C6A H6AA 0.9700 . ?
C6A H6AB 0.9700 . ?
C6A O2A 1.423(12) . ?
C6A C7A 1.515(14) . ?
O6A C14A 1.420(8) . ?
O2A C5A 1.343(15) . ?
C14A H14A 0.9700 . ?
C14A H14B 0.9700 . ?
C4A H4AA 0.9700 . ?
C4A H4AB 0.9700 . ?
C4A C5A 1.49(2) . ?
C4A O1A 1.377(11) . ?
C5A H5AA 0.9700 . ?
C5A H5AB 0.9700 . ?
C7A H7AA 0.9700 . ?
C7A H7AB 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S2 Ni1 S6 176.72(2) . . ?
S2 Ni1 S1 93.00(2) . . ?
S1 Ni1 S6 87.91(2) . . ?
S7 Ni1 S6 93.11(2) . . ?
S7 Ni1 S2 86.08(2) . . ?
S7 Ni1 S1 178.03(2) . . ?
C18 S6 Ni1 101.97(7) . . ?
C16 S2 Ni1 102.10(8) . . ?
C15 S1 Ni1 102.02(7) . . ?
C19 S7 Ni1 102.15(7) . . ?
C20 S8 C18 97.38(10) . . ?
C20 S9 C19 97.59(10) . . ?
C17 S4 C16 97.39(11) . . ?
C17 S3 C15 97.26(11) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
S6 C18 S8 123.01(12) . . ?
C19 C18 S6 121.12(16) . . ?
C19 C18 S8 115.87(16) . . ?
S7 C19 S9 122.27(12) . . ?
C18 C19 S7 121.49(16) . . ?
C18 C19 S9 116.25(16) . . ?
S1 C15 S3 122.57(13) . . ?
C16 C15 S1 121.38(16) . . ?
C16 C15 S3 116.05(17) . . ?
S3 C17 S4 113.21(13) . . ?
S5 C17 S4 122.99(15) . . ?
S5 C17 S3 123.80(15) . . ?
S9 C20 S8 112.89(12) . . ?
S10 C20 S8 123.13(13) . . ?
S10 C20 S9 123.98(14) . . ?
S2 C16 S4 122.50(13) . . ?
C15 C16 S2 121.47(17) . . ?
C15 C16 S4 116.03(17) . . ?
C11 O4 C10 120.8(5) . . ?
C5 O1 C4 114.0(8) . . ?
C8 O3 C9 112.5(6) . . ?
C14 O6 C3 118.1(4) . . ?
N1 C1 H00Z 108.9 . . ?
N1 C1 H 108.9 . . ?
N1 C1 H1D 109.5 . . ?
N1 C1 H1E 109.5 . . ?
H00Z C1 H 107.7 . . ?
H1D C1 H1E 108.1 . . ?
C2 C1 N1 113.2(2) . . ?
C2 C1 H00Z 108.9 . . ?
C2 C1 H 108.9 . . ?
C2A C1 N1 110.6(4) . . ?
C2A C1 H1D 109.5 . . ?
C2A C1 H1E 109.5 . . ?
O6 C3 H00A 108.0 . . ?
O6 C3 H00B 108.0 . . ?
H00A C3 H00B 107.2 . . ?
H3C C3 H3D 107.5 . . ?
C4 C3 O6 117.3(3) . . ?
C4 C3 H00A 108.0 . . ?
C4 C3 H00B 108.0 . . ?
C14A C3 H3C 108.5 . . ?
C14A C3 H3D 108.5 . . ?
C14A C3 O1A 115.3(4) . . ?
O1A C3 H3C 108.5 . . ?
O1A C3 H3D 108.5 . . ?
C12 O5 C13 128.1(6) . . ?
C6 O2 C7 110.9(7) . . ?
O3 C9 H00E 109.7 . . ?
O3 C9 H00F 109.7 . . ?
O3 C9 C10 109.7(6) . . ?
H00E C9 H00F 108.2 . . ?
C10 C9 H00E 109.7 . . ?
C10 C9 H00F 109.7 . . ?
O1 C5 H00G 109.4 . . ?
O1 C5 H00H 109.4 . . ?
O1 C5 C6 111.2(11) . . ?
H00G C5 H00H 108.0 . . ?
C6 C5 H00G 109.4 . . ?
C6 C5 H00H 109.4 . . ?
O5 C13 H00I 106.9 . . ?
O5 C13 H00J 106.9 . . ?
H00I C13 H00J 106.7 . . ?
C14 C13 O5 121.8(6) . . ?
C14 C13 H00I 106.9 . . ?
C14 C13 H00J 106.9 . . ?
O6 C14 H00K 106.4 . . ?
O6 C14 H00L 106.4 . . ?
C13 C14 O6 123.7(6) . . ?
C13 C14 H00K 106.4 . . ?
C13 C14 H00L 106.4 . . ?
H00K C14 H00L 106.5 . . ?
O1 C4 H00M 109.4 . . ?
O1 C4 H00N 109.4 . . ?
C3 C4 O1 111.0(5) . . ?
C3 C4 H00M 109.4 . . ?
C3 C4 H00N 109.4 . . ?
H00M C4 H00N 108.0 . . ?
O2 C7 H00O 109.8 . . ?
O2 C7 H00P 109.8 . . ?
O2 C7 C8 109.5(6) . . ?
H00O C7 H00P 108.2 . . ?
C8 C7 H00O 109.8 . . ?
C8 C7 H00P 109.8 . . ?
Cl1 C2 H01E 108.6 . . ?
Cl1 C2 H01F 108.6 . . ?
C1 C2 Cl1 114.7(3) . . ?
C1 C2 H01E 108.6 . . ?
C1 C2 H01F 108.6 . . ?
H01E C2 H01F 107.6 . . ?
O5 C12 H01A 108.9 . . ?
O5 C12 H01B 108.9 . . ?
H01A C12 H01B 107.7 . . ?
C11 C12 O5 113.3(6) . . ?
C11 C12 H01A 108.9 . . ?
C11 C12 H01B 108.9 . . ?
O2 C6 C5 110.0(8) . . ?
O2 C6 H01C 109.7 . . ?
O2 C6 H01D 109.7 . . ?
C5 C6 H01C 109.7 . . ?
C5 C6 H01D 109.7 . . ?
H01C C6 H01D 108.2 . . ?
Cl1 C2A H2AA 107.7 . . ?
Cl1 C2A H2AB 107.7 . . ?
C1 C2A Cl1 118.4(6) . . ?
C1 C2A H2AA 107.7 . . ?
C1 C2A H2AB 107.7 . . ?
H2AA C2A H2AB 107.1 . . ?
O3 C8 C7 108.5(6) . . ?
O3 C8 H3A 110.0 . . ?
O3 C8 H3B 110.0 . . ?
C7 C8 H3A 110.0 . . ?
C7 C8 H3B 110.0 . . ?
H3A C8 H3B 108.4 . . ?
O4 C10 C9 109.9(6) . . ?
O4 C10 H10A 109.7 . . ?
O4 C10 H10B 109.7 . . ?
C9 C10 H10A 109.7 . . ?
C9 C10 H10B 109.7 . . ?
H10A C10 H10B 108.2 . . ?
C12A O5A C11 124.7(6) . . ?
C9A O4A C10A 112.8(8) . . ?
O4A C10A H10C 108.5 . . ?
O4A C10A H10D 108.5 . . ?
H10C C10A H10D 107.5 . . ?
C11 C10A O4A 115.1(8) . . ?
C11 C10A H10C 108.5 . . ?
C11 C10A H10D 108.5 . . ?
O4A C9A H9AA 109.7 . . ?
O4A C9A H9AB 109.7 . . ?
O4A C9A C8A 109.7(7) . . ?
H9AA C9A H9AB 108.2 . . ?
C8A C9A H9AA 109.7 . . ?
C8A C9A H9AB 109.7 . . ?
O4 C11 H0AA 108.0 . . ?
O4 C11 H0AB 108.0 . . ?
C12 C11 O4 117.3(4) . . ?
C12 C11 H0AA 108.0 . . ?
C12 C11 H0AB 108.0 . . ?
O5A C11 H11A 106.5 . . ?
O5A C11 H11B 106.5 . . ?
C10A C11 O5A 123.2(5) . . ?
C10A C11 H11A 106.5 . . ?
C10A C11 H11B 106.5 . . ?
H0AA C11 H0AB 107.2 . . ?
H11A C11 H11B 106.5 . . ?
C9A C8A H8AA 109.6 . . ?
C9A C8A H8AB 109.6 . . ?
H8AA C8A H8AB 108.2 . . ?
O3A C8A C9A 110.1(7) . . ?
O3A C8A H8AA 109.6 . . ?
O3A C8A H8AB 109.6 . . ?
C7A O3A C8A 111.2(8) . . ?
O5A C12A H12A 107.2 . . ?
O5A C12A H12B 107.2 . . ?
H12A C12A H12B 106.8 . . ?
C13A C12A O5A 120.5(8) . . ?
C13A C12A H12A 107.2 . . ?
C13A C12A H12B 107.2 . . ?
C12A C13A H13A 105.1 . . ?
C12A C13A H13B 105.1 . . ?
C12A C13A O6A 128.7(9) . . ?
H13A C13A H13B 105.9 . . ?
O6A C13A H13A 105.1 . . ?
O6A C13A H13B 105.1 . . ?
H6AA C6A H6AB 108.0 . . ?
O2A C6A H6AA 109.4 . . ?
O2A C6A H6AB 109.4 . . ?
O2A C6A C7A 110.9(8) . . ?
C7A C6A H6AA 109.4 . . ?
C7A C6A H6AB 109.4 . . ?
C14A O6A C13A 137.0(6) . . ?
C5A O2A C6A 115.7(10) . . ?
C3 C14A O6A 115.7(5) . . ?
C3 C14A H14A 108.4 . . ?
C3 C14A H14B 108.4 . . ?
O6A C14A H14A 108.4 . . ?
O6A C14A H14B 108.4 . . ?
H14A C14A H14B 107.4 . . ?
H4AA C4A H4AB 107.8 . . ?
C5A C4A H4AA 109.0 . . ?
C5A C4A H4AB 109.0 . . ?
O1A C4A H4AA 109.0 . . ?
O1A C4A H4AB 109.0 . . ?
O1A C4A C5A 112.8(10) . . ?
O2A C5A C4A 115.1(11) . . ?
O2A C5A H5AA 108.5 . . ?
O2A C5A H5AB 108.5 . . ?
C4A C5A H5AA 108.5 . . ?
C4A C5A H5AB 108.5 . . ?
H5AA C5A H5AB 107.5 . . ?
C4A O1A C3 118.6(5) . . ?
O3A C7A C6A 106.8(8) . . ?
O3A C7A H7AA 110.4 . . ?
O3A C7A H7AB 110.4 . . ?
C6A C7A H7AA 110.4 . . ?
C6A C7A H7AB 110.4 . . ?
H7AA C7A H7AB 108.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S6 C18 S8 177.13(10) . . . . ?
Ni1 S6 C18 C19 -3.29(19) . . . . ?
Ni1 S2 C16 S4 -178.08(11) . . . . ?
Ni1 S2 C16 C15 2.04(19) . . . . ?
Ni1 S1 C15 S3 -179.15(11) . . . . ?
Ni1 S1 C15 C16 1.04(19) . . . . ?
Ni1 S7 C19 S9 -178.18(11) . . . . ?
Ni1 S7 C19 C18 2.29(19) . . . . ?
S6 C18 C19 S7 0.7(3) . . . . ?
S6 C18 C19 S9 -178.83(11) . . . . ?
S1 C15 C16 S2 -2.2(3) . . . . ?
S1 C15 C16 S4 177.90(10) . . . . ?
S8 C18 C19 S7 -179.67(11) . . . . ?
S8 C18 C19 S9 0.8(2) . . . . ?
S3 C15 C16 S2 177.97(11) . . . . ?
S3 C15 C16 S4 -1.9(2) . . . . ?
N1 C1 C2 Cl1 71.5(4) . . . . ?
N1 C1 C2A Cl1 -74.8(7) . . . . ?
C18 S8 C20 S9 1.99(13) . . . . ?
C18 S8 C20 S10 -177.69(14) . . . . ?
C19 S9 C20 S8 -1.66(14) . . . . ?
C19 S9 C20 S10 178.02(15) . . . . ?
C15 S3 C17 S4 -2.24(14) . . . . ?
C15 S3 C17 S5 177.92(15) . . . . ?
C17 S4 C16 S2 -179.60(14) . . . . ?
C17 S4 C16 C15 0.29(18) . . . . ?
C17 S3 C15 S1 -177.28(13) . . . . ?
C17 S3 C15 C16 2.53(18) . . . . ?
C20 S8 C18 S6 177.92(13) . . . . ?
C20 S8 C18 C19 -1.68(18) . . . . ?
C20 S9 C19 S7 -178.99(13) . . . . ?
C20 S9 C19 C18 0.56(19) . . . . ?
C16 S4 C17 S3 1.43(14) . . . . ?
C16 S4 C17 S5 -178.72(15) . . . . ?
O1 C5 C6 O2 -58.1(12) . . . . ?
O3 C9 C10 O4 -66.2(7) . . . . ?
O6 C3 C4 O1 55.8(6) . . . . ?
C3 O6 C14 C13 165.4(7) . . . . ?
O5 C13 C14 O6 -18.3(13) . . . . ?
O5 C12 C11 O4 53.3(7) . . . . ?
O2 C7 C8 O3 61.8(9) . . . . ?
C9 O3 C8 C7 168.5(6) . . . . ?
C5 O1 C4 C3 171.8(8) . . . . ?
C13 O5 C12 C11 155.0(7) . . . . ?
C14 O6 C3 C4 -178.5(5) . . . . ?
C4 O1 C5 C6 -179.7(8) . . . . ?
C7 O2 C6 C5 179.6(8) . . . . ?
C12 O5 C13 C14 160.3(8) . . . . ?
C6 O2 C7 C8 -171.4(7) . . . . ?
C8 O3 C9 C10 -178.0(6) . . . . ?
C10 O4 C11 C12 -167.2(5) . . . . ?
O5A C12A C13A O6A 2.0(15) . . . . ?
O4A C10A C11 O5A 45.8(9) . . . . ?
O4A C9A C8A O3A -63.6(9) . . . . ?
C10A O4A C9A C8A -175.8(7) . . . . ?
C9A O4A C10A C11 -168.5(7) . . . . ?
C9A C8A O3A C7A -179.4(8) . . . . ?
C11 O4 C10 C9 -169.5(5) . . . . ?
C11 O5A C12A C13A 166.1(8) . . . . ?
C8A O3A C7A C6A 169.0(8) . . . . ?
C12A O5A C11 C10A -171.8(7) . . . . ?
C12A C13A O6A C14A 134.1(10) . . . . ?
C13A O6A C14A C3 153.4(8) . . . . ?
C6A O2A C5A C4A 173.4(12) . . . . ?
O2A C6A C7A O3A 62.7(10) . . . . ?
C14A C3 O1A C4A -177.7(6) . . . . ?
C5A C4A O1A C3 -173.0(9) . . . . ?
O1A C3 C14A O6A 54.3(7) . . . . ?
O1A C4A C5A O2A -56.8(19) . . . . ?
C7A C6A O2A C5A -173.6(11) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.606
_oxdiff_exptl_absorpt_empirical_full_min 0.635
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_153k-f
_database_code_depnum_ccdc_archive 'CCDC 2053394'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-18 downloaded from the CCDC.
;
_audit_creation_date             2020-12-31
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C2 H7 Cl N, C12 H24 O6'
_chemical_formula_sum            'C20 H31 Cl N Ni O6 S10'
_chemical_formula_weight         796.22
_chemical_melting_point          ?
_chemical_oxdiff_formula         C20H30NO6NiS10Cl
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.2185(3)
_cell_length_b                   12.3084(3)
_cell_length_c                   12.7536(3)
_cell_angle_alpha                92.083(2)
_cell_angle_beta                 111.733(2)
_cell_angle_gamma                96.128(2)
_cell_volume                     1621.02(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    28564
_cell_measurement_temperature    153
_cell_measurement_theta_max      30.9790
_cell_measurement_theta_min      2.2800
_shelx_estimated_absorpt_T_max   0.792
_shelx_estimated_absorpt_T_min   0.454
_exptl_absorpt_coefficient_mu    1.361
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42090
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             822
_exptl_crystal_size_max          0.69
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0902
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.836
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            41879
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.836
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.920
_diffrn_reflns_theta_min         2.073
_diffrn_ambient_temperature      153
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.836
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -56.00  18.00   0.50    0.35    --    5.18 -31.00  -4.02  148
  2  ω     39.00  78.00   0.50    0.35    --    5.18  51.00 -81.00   78
  3  ω     -8.00  19.00   0.50    0.35    --    5.18 -28.00 -96.36   54
  4  ω    -69.00 -22.00   0.50    0.35    --    5.18 -28.00 -96.36   94
  5  ω    -63.00 -34.00   0.50    0.35    --    5.18 -27.00-127.27   58
  6  ω    -28.00  19.00   0.50    0.35    --    5.18 -28.00-177.36   94
  7  ω    -17.00  18.00   0.50    0.35    --    5.18 -27.00-127.27   70
  8  ω    -69.00 -43.00   0.50    0.35    --    5.18 -19.00 -60.00   52
  9  ω    -31.00  18.00   0.50    0.35    --    5.18 -19.00 -60.00   98
 10  ω    -61.00  18.00   0.50    0.35    --    5.18 -37.00  60.00  158
 11  ω    -67.00  19.00   0.50    0.35    --    5.18 -51.00 132.00  172
 12  ω    -64.00  18.00   0.50    0.35    --    5.18 -37.00 150.00  164
 13  ω    -17.00  29.00   0.50    0.35    --   -4.95 -99.00-180.00   92
 14  ω    -16.00  28.00   0.50    0.35    --   -4.95 -99.00 -30.00   88
 15  ω    -76.00 -31.00   0.50    0.35    --   -4.95 -51.00 132.00   90
 16  ω     40.00  67.00   0.50    0.35    --   -4.95  51.00 -81.00   54
 17  ω    -10.00  16.00   0.50    0.35    --   -4.95  51.00 -81.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0551059000
_diffrn_orient_matrix_UB_12      -0.0324577000
_diffrn_orient_matrix_UB_13      0.0021433000
_diffrn_orient_matrix_UB_21      -0.0212035000
_diffrn_orient_matrix_UB_22      -0.0154803000
_diffrn_orient_matrix_UB_23      -0.0588008000
_diffrn_orient_matrix_UB_31      0.0350067000
_diffrn_orient_matrix_UB_32      -0.0457038000
_diffrn_orient_matrix_UB_33      0.0121152000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6920
_reflns_number_total             8598
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         8598
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0438
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0819P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1218
_refine_ls_wR_factor_ref         0.1293
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
2. Others
 Sof(Cl1A)=Sof(H1bc)=Sof(H1bd)=Sof(C2A)=Sof(H2Aa)=Sof(H2Ab)=1-FVAR(1)
 Sof(H1aa)=Sof(H1ab)=Sof(C2)=Sof(H2a)=Sof(H2b)=Sof(Cl1)=FVAR(1)
 Sof(H3bc)=Sof(H3bd)=Sof(O5A)=Sof(O4A)=Sof(C10A)=Sof(H10c)=Sof(H10d)=Sof(C9A)=
 Sof(H9Aa)=Sof(H9Ab)=Sof(H11c)=Sof(H11d)=Sof(C8A)=Sof(H8Aa)=Sof(H8Ab)=Sof(O3A)=
 Sof(C12A)=Sof(H12c)=Sof(H12d)=Sof(C13A)=Sof(H13c)=Sof(H13d)=Sof(C6A)=Sof(H6Aa)=
 Sof(H6Ab)=Sof(O6A)=Sof(O2A)=Sof(C14A)=Sof(H14c)=Sof(H14d)=Sof(C4A)=Sof(H4Aa)=
 Sof(H4Ab)=Sof(C5A)=Sof(H5Aa)=Sof(H5Ab)=Sof(O1A)=Sof(C7A)=Sof(H7Aa)=Sof(H7Ab)=1-
 FVAR(2)
 Sof(O4)=Sof(O1)=Sof(O3)=Sof(O6)=Sof(H3aa)=Sof(H3ab)=Sof(O5)=Sof(O2)=Sof(C9)=
 Sof(H9a)=Sof(H9b)=Sof(C5)=Sof(H5a)=Sof(H5b)=Sof(C13)=Sof(H13a)=Sof(H13b)=
 Sof(C14)=Sof(H14a)=Sof(H14b)=Sof(C4)=Sof(H4a)=Sof(H4b)=Sof(C7)=Sof(H7a)=
 Sof(H7b)=Sof(C12)=Sof(H12a)=Sof(H12b)=Sof(C6)=Sof(H6a)=Sof(H6b)=Sof(C8)=
 Sof(H8a)=Sof(H8b)=Sof(C10)=Sof(H10a)=Sof(H10b)=Sof(H11a)=Sof(H11b)=FVAR(2)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1bc,H1bd), C1(H1aa,H1ab), C3(H3aa,H3ab), C3(H3bc,H3bd), C9(H9a,H9b),
 C5(H5a,H5b), C13(H13a,H13b), C14(H14a,H14b), C4(H4a,H4b), C7(H7a,H7b), C2(H2a,
 H2b), C12(H12a,H12b), C6(H6a,H6b), C2A(H2Aa,H2Ab), C8(H8a,H8b), C10(H10a,H10b),
  C10A(H10c,H10d), C9A(H9Aa,H9Ab), C11(H11a,H11b), C11(H11c,H11d), C8A(H8Aa,
 H8Ab), C12A(H12c,H12d), C13A(H13c,H13d), C6A(H6Aa,H6Ab), C14A(H14c,H14d),
 C4A(H4Aa,H4Ab), C5A(H5Aa,H5Ab), C7A(H7Aa,H7Ab)
3.b Idealised Me refined as rotating group:
 N1(H1a,H1b,H1c)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.84535(2) 0.89065(2) 0.51205(2) 0.02617(9) Uani 1 1 d . . . . .
S6 S 0.69183(5) 0.97792(4) 0.52242(4) 0.03431(13) Uani 1 1 d . . . . .
S2 S 1.00578(5) 0.81104(4) 0.50743(4) 0.03192(12) Uani 1 1 d . . . . .
S1 S 0.79434(5) 0.93583(4) 0.34061(4) 0.03272(12) Uani 1 1 d . . . . .
S7 S 0.89729(5) 0.84207(4) 0.68234(4) 0.03150(12) Uani 1 1 d . . . . .
S8 S 0.61350(5) 1.02793(4) 0.72134(5) 0.03357(13) Uani 1 1 d . . . . .
S9 S 0.80098(5) 0.90102(4) 0.86680(4) 0.03280(12) Uani 1 1 d . . . . .
S4 S 1.10019(5) 0.77046(5) 0.31753(5) 0.03733(13) Uani 1 1 d . . . . .
S3 S 0.91159(5) 0.89233(4) 0.16615(4) 0.03439(13) Uani 1 1 d . . . . .
S10 S 0.62529(6) 1.00326(5) 0.95582(5) 0.04077(14) Uani 1 1 d . . . . .
S5 S 1.09172(6) 0.78827(5) 0.08374(5) 0.04456(15) Uani 1 1 d . . . . .
Cl1A Cl 0.8079(9) 0.4690(8) 0.5120(5) 0.0565(19) Uani 0.178(6) 1 d . . P A 2
N1 N 0.66774(16) 0.50222(12) 0.25479(14) 0.0291(3) Uani 1 1 d . . . . .
H1A H 0.663307 0.517615 0.184287 0.035 Uiso 1 1 calc R U . . .
H1B H 0.588820 0.504225 0.259099 0.035 Uiso 1 1 calc R U . . .
H1C H 0.691829 0.434240 0.268639 0.035 Uiso 1 1 calc R U . . .
C18 C 0.70837(18) 0.96675(15) 0.66045(17) 0.0278(4) Uani 1 1 d . . . . .
C19 C 0.79643(19) 0.90713(15) 0.72977(16) 0.0275(4) Uani 1 1 d . . . . .
C15 C 0.90616(19) 0.88159(15) 0.30015(17) 0.0289(4) Uani 1 1 d . . . . .
C17 C 1.0375(2) 0.81582(17) 0.18406(18) 0.0338(4) Uani 1 1 d . . . . .
C20 C 0.6774(2) 0.97911(15) 0.85341(18) 0.0316(4) Uani 1 1 d . . . . .
C16 C 0.99682(19) 0.82558(15) 0.37231(17) 0.0288(4) Uani 1 1 d . . . . .
O4 O 0.7138(3) 0.6172(2) 0.0821(3) 0.0345(7) Uani 0.497(2) 1 d . . P B 1
O1 O 0.5013(3) 0.3208(3) 0.3076(3) 0.0400(8) Uani 0.497(2) 1 d . . P B 1
O3 O 0.4978(3) 0.6543(2) 0.1358(3) 0.0378(7) Uani 0.497(2) 1 d . . P B 1
O6 O 0.7206(3) 0.2816(2) 0.2655(3) 0.0334(7) Uani 0.497(2) 1 d . . P B 1
C1 C 0.7646(2) 0.58487(17) 0.34029(19) 0.0387(5) Uani 1 1 d . . . . .
H1BC H 0.796154 0.642904 0.301620 0.046 Uiso 0.178(6) 1 calc R U P A 2
H1BD H 0.723836 0.619500 0.387536 0.046 Uiso 0.178(6) 1 calc R U P A 2
H1AA H 0.743036 0.659222 0.320138 0.046 Uiso 0.822(6) 1 calc R U P A 1
H1AB H 0.851201 0.579080 0.338651 0.046 Uiso 0.822(6) 1 calc R U P A 1
C3 C 0.6455(3) 0.20313(19) 0.2999(3) 0.0573(7) Uani 1 1 d . . . . .
H3AA H 0.581740 0.160298 0.231112 0.069 Uiso 0.497(2) 1 calc R U P B 1
H3AB H 0.703119 0.151929 0.344527 0.069 Uiso 0.497(2) 1 calc R U P B 1
H3BC H 0.714894 0.214179 0.376285 0.069 Uiso 0.503(2) 1 calc R U P B 2
H3BD H 0.595982 0.129946 0.293384 0.069 Uiso 0.503(2) 1 calc R U P B 2
O5 O 0.7956(3) 0.4114(3) 0.1174(3) 0.0363(7) Uani 0.497(2) 1 d . . P B 1
O2 O 0.4279(3) 0.5312(3) 0.2897(3) 0.0409(8) Uani 0.497(2) 1 d . . P B 1
C9 C 0.5617(7) 0.7346(5) 0.0908(6) 0.0395(14) Uani 0.497(2) 1 d . . P B 1
H9A H 0.632604 0.779780 0.153236 0.047 Uiso 0.497(2) 1 calc R U P B 1
H9B H 0.499921 0.783501 0.047158 0.047 Uiso 0.497(2) 1 calc R U P B 1
C5 C 0.4342(11) 0.3625(13) 0.3695(11) 0.039(2) Uani 0.497(2) 1 d . . P B 1
H5A H 0.496344 0.401468 0.441403 0.047 Uiso 0.497(2) 1 calc R U P B 1
H5B H 0.382195 0.301562 0.388077 0.047 Uiso 0.497(2) 1 calc R U P B 1
C13 C 0.8212(6) 0.3040(4) 0.1306(5) 0.0417(12) Uani 0.497(2) 1 d . . P B 1
H13A H 0.785627 0.265222 0.053881 0.050 Uiso 0.497(2) 1 calc R U P B 1
H13B H 0.916390 0.306024 0.158079 0.050 Uiso 0.497(2) 1 calc R U P B 1
C14 C 0.7826(4) 0.2428(4) 0.1942(4) 0.0373(10) Uani 0.497(2) 1 d . . P B 1
H14A H 0.859283 0.211230 0.244145 0.045 Uiso 0.497(2) 1 calc R U P B 1
H14B H 0.722527 0.180925 0.143965 0.045 Uiso 0.497(2) 1 calc R U P B 1
C4 C 0.5796(5) 0.2397(4) 0.3624(5) 0.0459(12) Uani 0.497(2) 1 d . . P B 1
H4A H 0.642084 0.271196 0.437644 0.055 Uiso 0.497(2) 1 calc R U P B 1
H4B H 0.523938 0.177052 0.374027 0.055 Uiso 0.497(2) 1 calc R U P B 1
C7 C 0.3540(6) 0.6129(5) 0.2297(6) 0.0485(13) Uani 0.497(2) 1 d . . P B 1
H7A H 0.310037 0.645194 0.275468 0.058 Uiso 0.497(2) 1 calc R U P B 1
H7B H 0.286918 0.578982 0.157464 0.058 Uiso 0.497(2) 1 calc R U P B 1
C2 C 0.7689(3) 0.5699(2) 0.4586(2) 0.0440(8) Uani 0.822(6) 1 d . . P A 1
H2A H 0.679744 0.562804 0.457524 0.053 Uiso 0.822(6) 1 calc R U P A 1
H2B H 0.818515 0.635746 0.508953 0.053 Uiso 0.822(6) 1 calc R U P A 1
C12 C 0.8684(5) 0.4985(4) 0.0874(4) 0.0431(11) Uani 0.497(2) 1 d . . P B 1
H12A H 0.940021 0.532921 0.156664 0.052 Uiso 0.497(2) 1 calc R U P B 1
H12B H 0.906992 0.467912 0.036290 0.052 Uiso 0.497(2) 1 calc R U P B 1
C6 C 0.3474(5) 0.4395(4) 0.3020(4) 0.0445(11) Uani 0.497(2) 1 d . . P B 1
H6A H 0.290709 0.403281 0.226739 0.053 Uiso 0.497(2) 1 calc R U P B 1
H6B H 0.292238 0.463058 0.341482 0.053 Uiso 0.497(2) 1 calc R U P B 1
C2A C 0.8650(14) 0.5355(12) 0.4066(14) 0.054(4) Uani 0.178(6) 1 d . . P A 2
H2AA H 0.942270 0.590020 0.445272 0.065 Uiso 0.178(6) 1 calc R U P A 2
H2AB H 0.887200 0.480067 0.361018 0.065 Uiso 0.178(6) 1 calc R U P A 2
C8 C 0.4413(5) 0.7003(4) 0.2063(4) 0.0447(12) Uani 0.497(2) 1 d . . P B 1
H8A H 0.391317 0.759063 0.168512 0.054 Uiso 0.497(2) 1 calc R U P B 1
H8B H 0.509775 0.732990 0.278287 0.054 Uiso 0.497(2) 1 calc R U P B 1
C10 C 0.6146(5) 0.6790(4) 0.0163(5) 0.0429(11) Uani 0.497(2) 1 d . . P B 1
H10A H 0.544591 0.629309 -0.042396 0.051 Uiso 0.497(2) 1 calc R U P B 1
H10B H 0.650982 0.734055 -0.022134 0.051 Uiso 0.497(2) 1 calc R U P B 1
O5A O 0.7752(3) 0.4808(3) 0.0790(3) 0.0365(7) Uani 0.503(2) 1 d . . P B 2
O4A O 0.6445(3) 0.6601(3) 0.0905(3) 0.0382(7) Uani 0.503(2) 1 d . . P B 2
C10A C 0.6950(5) 0.6419(4) 0.0057(5) 0.0454(11) Uani 0.503(2) 1 d . . P B 2
H10C H 0.623778 0.606692 -0.063418 0.055 Uiso 0.503(2) 1 calc R U P B 2
H10D H 0.726908 0.713761 -0.013130 0.055 Uiso 0.503(2) 1 calc R U P B 2
C9A C 0.5270(7) 0.7086(5) 0.0486(6) 0.0425(15) Uani 0.503(2) 1 d . . P B 2
H9AA H 0.458744 0.657433 -0.009939 0.051 Uiso 0.503(2) 1 calc R U P B 2
H9AB H 0.540966 0.776809 0.013509 0.051 Uiso 0.503(2) 1 calc R U P B 2
C11 C 0.7934(4) 0.5781(2) 0.0342(3) 0.0737(10) Uani 1 1 d . . . . .
H11A H 0.852569 0.641223 0.028443 0.088 Uiso 0.497(2) 1 calc R U P B 1
H11B H 0.738956 0.547865 -0.044035 0.088 Uiso 0.497(2) 1 calc R U P B 1
H11C H 0.871919 0.622337 0.089551 0.088 Uiso 0.503(2) 1 calc R U P B 2
H11D H 0.811447 0.561337 -0.034576 0.088 Uiso 0.503(2) 1 calc R U P B 2
C8A C 0.4853(5) 0.7338(4) 0.1433(4) 0.0419(10) Uani 0.503(2) 1 d . . P B 2
H8AA H 0.554899 0.782884 0.203083 0.050 Uiso 0.503(2) 1 calc R U P B 2
H8AB H 0.407419 0.771987 0.115756 0.050 Uiso 0.503(2) 1 calc R U P B 2
O3A O 0.4570(3) 0.6346(2) 0.1888(3) 0.0363(7) Uani 0.503(2) 1 d . . P B 2
C12A C 0.8776(5) 0.4177(4) 0.1216(4) 0.0433(11) Uani 0.503(2) 1 d . . P B 2
H12C H 0.894343 0.388505 0.055716 0.052 Uiso 0.503(2) 1 calc R U P B 2
H12D H 0.955223 0.469187 0.167660 0.052 Uiso 0.503(2) 1 calc R U P B 2
C13A C 0.8724(5) 0.3361(5) 0.1819(5) 0.0407(11) Uani 0.503(2) 1 d . . P B 2
H13C H 0.950839 0.349199 0.252283 0.049 Uiso 0.503(2) 1 calc R U P B 2
H13D H 0.881011 0.270044 0.139924 0.049 Uiso 0.503(2) 1 calc R U P B 2
C6A C 0.3602(5) 0.5453(4) 0.3040(4) 0.0440(11) Uani 0.503(2) 1 d . . P B 2
H6AA H 0.328171 0.556504 0.365721 0.053 Uiso 0.503(2) 1 calc R U P B 2
H6AB H 0.286168 0.512564 0.235519 0.053 Uiso 0.503(2) 1 calc R U P B 2
O6A O 0.7680(3) 0.3083(2) 0.2145(3) 0.0367(7) Uani 0.503(2) 1 d . . P B 2
O2A O 0.4564(3) 0.4733(3) 0.3360(3) 0.0388(7) Uani 0.503(2) 1 d . . P B 2
C14A C 0.7016(4) 0.2041(3) 0.2203(4) 0.0380(10) Uani 0.503(2) 1 d . . P B 2
H14C H 0.633367 0.180619 0.144980 0.046 Uiso 0.503(2) 1 calc R U P B 2
H14D H 0.763712 0.149620 0.237653 0.046 Uiso 0.503(2) 1 calc R U P B 2
C4A C 0.5092(5) 0.2931(4) 0.3751(5) 0.0438(11) Uani 0.503(2) 1 d . . P B 2
H4AA H 0.578346 0.325897 0.446706 0.053 Uiso 0.503(2) 1 calc R U P B 2
H4AB H 0.476734 0.218843 0.388239 0.053 Uiso 0.503(2) 1 calc R U P B 2
C5A C 0.3993(12) 0.3635(12) 0.3407(12) 0.046(3) Uani 0.503(2) 1 d . . P B 2
H5AA H 0.333096 0.335337 0.265726 0.055 Uiso 0.503(2) 1 calc R U P B 2
H5AB H 0.357605 0.362910 0.396865 0.055 Uiso 0.503(2) 1 calc R U P B 2
O1A O 0.5600(3) 0.2853(3) 0.2898(3) 0.0375(7) Uani 0.503(2) 1 d . . P B 2
C7A C 0.4165(6) 0.6534(4) 0.2802(5) 0.0452(12) Uani 0.503(2) 1 d . . P B 2
H7AA H 0.350742 0.704731 0.260040 0.054 Uiso 0.503(2) 1 calc R U P B 2
H7AB H 0.491129 0.686223 0.348146 0.054 Uiso 0.503(2) 1 calc R U P B 2
Cl1 Cl 0.8420(2) 0.45152(15) 0.51415(16) 0.0622(5) Uani 0.822(6) 1 d . . P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S6 2.1658(5) . ?
Ni1 S2 2.1573(5) . ?
Ni1 S1 2.1557(5) . ?
Ni1 S7 2.1553(5) . ?
S6 C18 1.713(2) . ?
S2 C16 1.706(2) . ?
S1 C15 1.7084(19) . ?
S7 C19 1.7183(18) . ?
S8 C18 1.7446(19) . ?
S8 C20 1.727(2) . ?
S9 C19 1.7340(19) . ?
S9 C20 1.7307(19) . ?
S4 C17 1.723(2) . ?
S4 C16 1.7397(19) . ?
S3 C15 1.7418(19) . ?
S3 C17 1.731(2) . ?
S10 C20 1.6467(19) . ?
S5 C17 1.646(2) . ?
Cl1A C2A 1.869(16) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N1 C1 1.487(3) . ?
C18 C19 1.361(3) . ?
C15 C16 1.364(3) . ?
O4 C10 1.433(6) . ?
O4 C11 1.370(4) . ?
O1 C5 1.395(17) . ?
O1 C4 1.429(6) . ?
O3 C9 1.419(8) . ?
O3 C8 1.412(6) . ?
O6 C3 1.402(3) . ?
O6 C14 1.431(5) . ?
C1 H1BC 0.9900 . ?
C1 H1BD 0.9900 . ?
C1 H1AA 0.9900 . ?
C1 H1AB 0.9900 . ?
C1 C2 1.510(3) . ?
C1 C2A 1.354(15) . ?
C3 H3AA 0.9900 . ?
C3 H3AB 0.9900 . ?
C3 H3BC 0.9900 . ?
C3 H3BD 0.9900 . ?
C3 C4 1.365(6) . ?
C3 C14A 1.378(5) . ?
C3 O1A 1.444(4) . ?
O5 C13 1.386(6) . ?
O5 C12 1.427(5) . ?
O2 C7 1.432(6) . ?
O2 C6 1.419(6) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.477(9) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.491(14) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.284(7) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.491(7) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 Cl1 1.788(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C11 1.389(6) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C2A H2AA 0.9900 . ?
C2A H2AB 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
O5A C11 1.373(4) . ?
O5A C12A 1.406(6) . ?
O4A C10A 1.416(6) . ?
O4A C9A 1.432(8) . ?
C10A H10C 0.9900 . ?
C10A H10D 0.9900 . ?
C10A C11 1.369(6) . ?
C9A H9AA 0.9900 . ?
C9A H9AB 0.9900 . ?
C9A C8A 1.482(9) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 H11C 0.9900 . ?
C11 H11D 0.9900 . ?
C8A H8AA 0.9900 . ?
C8A H8AB 0.9900 . ?
C8A O3A 1.427(5) . ?
O3A C7A 1.418(6) . ?
C12A H12C 0.9900 . ?
C12A H12D 0.9900 . ?
C12A C13A 1.297(7) . ?
C13A H13C 0.9900 . ?
C13A H13D 0.9900 . ?
C13A O6A 1.396(6) . ?
C6A H6AA 0.9900 . ?
C6A H6AB 0.9900 . ?
C6A O2A 1.422(6) . ?
C6A C7A 1.502(7) . ?
O6A C14A 1.432(5) . ?
O2A C5A 1.446(15) . ?
C14A H14C 0.9900 . ?
C14A H14D 0.9900 . ?
C4A H4AA 0.9900 . ?
C4A H4AB 0.9900 . ?
C4A C5A 1.523(14) . ?
C4A O1A 1.407(6) . ?
C5A H5AA 0.9900 . ?
C5A H5AB 0.9900 . ?
C7A H7AA 0.9900 . ?
C7A H7AB 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S2 Ni1 S6 176.87(2) . . ?
S1 Ni1 S6 87.815(19) . . ?
S1 Ni1 S2 93.02(2) . . ?
S7 Ni1 S6 93.201(19) . . ?
S7 Ni1 S2 86.008(19) . . ?
S7 Ni1 S1 178.743(19) . . ?
C18 S6 Ni1 101.90(7) . . ?
C16 S2 Ni1 102.33(7) . . ?
C15 S1 Ni1 102.35(7) . . ?
C19 S7 Ni1 102.20(7) . . ?
C20 S8 C18 97.53(9) . . ?
C20 S9 C19 97.28(9) . . ?
C17 S4 C16 97.60(10) . . ?
C17 S3 C15 97.37(10) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
S6 C18 S8 123.10(12) . . ?
C19 C18 S6 121.46(14) . . ?
C19 C18 S8 115.43(15) . . ?
S7 C19 S9 122.41(11) . . ?
C18 C19 S7 121.01(15) . . ?
C18 C19 S9 116.58(14) . . ?
S1 C15 S3 123.06(12) . . ?
C16 C15 S1 121.07(15) . . ?
C16 C15 S3 115.86(14) . . ?
S4 C17 S3 113.21(11) . . ?
S5 C17 S4 123.23(13) . . ?
S5 C17 S3 123.56(13) . . ?
S8 C20 S9 113.14(11) . . ?
S10 C20 S8 123.50(12) . . ?
S10 C20 S9 123.35(13) . . ?
S2 C16 S4 122.91(12) . . ?
C15 C16 S2 121.18(14) . . ?
C15 C16 S4 115.91(15) . . ?
C11 O4 C10 118.9(4) . . ?
C5 O1 C4 113.6(7) . . ?
C8 O3 C9 112.9(4) . . ?
C3 O6 C14 117.1(3) . . ?
N1 C1 H1BC 109.8 . . ?
N1 C1 H1BD 109.8 . . ?
N1 C1 H1AA 109.1 . . ?
N1 C1 H1AB 109.1 . . ?
N1 C1 C2 112.31(18) . . ?
H1BC C1 H1BD 108.2 . . ?
H1AA C1 H1AB 107.9 . . ?
C2 C1 H1AA 109.1 . . ?
C2 C1 H1AB 109.1 . . ?
C2A C1 N1 109.6(7) . . ?
C2A C1 H1BC 109.8 . . ?
C2A C1 H1BD 109.8 . . ?
O6 C3 H3AA 107.9 . . ?
O6 C3 H3AB 107.9 . . ?
H3AA C3 H3AB 107.2 . . ?
H3BC C3 H3BD 107.6 . . ?
C4 C3 O6 117.7(3) . . ?
C4 C3 H3AA 107.9 . . ?
C4 C3 H3AB 107.9 . . ?
C14A C3 H3BC 108.7 . . ?
C14A C3 H3BD 108.7 . . ?
C14A C3 O1A 114.4(3) . . ?
O1A C3 H3BC 108.7 . . ?
O1A C3 H3BD 108.7 . . ?
C13 O5 C12 127.4(4) . . ?
C6 O2 C7 111.8(4) . . ?
O3 C9 H9A 109.9 . . ?
O3 C9 H9B 109.9 . . ?
O3 C9 C10 109.0(5) . . ?
H9A C9 H9B 108.3 . . ?
C10 C9 H9A 109.9 . . ?
C10 C9 H9B 109.9 . . ?
O1 C5 H5A 109.7 . . ?
O1 C5 H5B 109.7 . . ?
O1 C5 C6 109.7(9) . . ?
H5A C5 H5B 108.2 . . ?
C6 C5 H5A 109.7 . . ?
C6 C5 H5B 109.7 . . ?
O5 C13 H13A 106.7 . . ?
O5 C13 H13B 106.7 . . ?
H13A C13 H13B 106.6 . . ?
C14 C13 O5 122.4(4) . . ?
C14 C13 H13A 106.7 . . ?
C14 C13 H13B 106.7 . . ?
O6 C14 H14A 106.5 . . ?
O6 C14 H14B 106.5 . . ?
C13 C14 O6 123.4(4) . . ?
C13 C14 H14A 106.5 . . ?
C13 C14 H14B 106.5 . . ?
H14A C14 H14B 106.5 . . ?
O1 C4 H4A 109.3 . . ?
O1 C4 H4B 109.3 . . ?
C3 C4 O1 111.5(4) . . ?
C3 C4 H4A 109.3 . . ?
C3 C4 H4B 109.3 . . ?
H4A C4 H4B 108.0 . . ?
O2 C7 H7A 109.8 . . ?
O2 C7 H7B 109.8 . . ?
O2 C7 C8 109.6(4) . . ?
H7A C7 H7B 108.2 . . ?
C8 C7 H7A 109.8 . . ?
C8 C7 H7B 109.8 . . ?
C1 C2 H2A 109.2 . . ?
C1 C2 H2B 109.2 . . ?
C1 C2 Cl1 112.1(2) . . ?
H2A C2 H2B 107.9 . . ?
Cl1 C2 H2A 109.2 . . ?
Cl1 C2 H2B 109.2 . . ?
O5 C12 H12A 109.1 . . ?
O5 C12 H12B 109.1 . . ?
H12A C12 H12B 107.8 . . ?
C11 C12 O5 112.6(4) . . ?
C11 C12 H12A 109.1 . . ?
C11 C12 H12B 109.1 . . ?
O2 C6 C5 107.1(6) . . ?
O2 C6 H6A 110.3 . . ?
O2 C6 H6B 110.3 . . ?
C5 C6 H6A 110.3 . . ?
C5 C6 H6B 110.3 . . ?
H6A C6 H6B 108.5 . . ?
Cl1A C2A H2AA 110.7 . . ?
Cl1A C2A H2AB 110.7 . . ?
C1 C2A Cl1A 105.2(9) . . ?
C1 C2A H2AA 110.7 . . ?
C1 C2A H2AB 110.7 . . ?
H2AA C2A H2AB 108.8 . . ?
O3 C8 C7 109.1(4) . . ?
O3 C8 H8A 109.9 . . ?
O3 C8 H8B 109.9 . . ?
C7 C8 H8A 109.9 . . ?
C7 C8 H8B 109.9 . . ?
H8A C8 H8B 108.3 . . ?
O4 C10 C9 109.8(5) . . ?
O4 C10 H10A 109.7 . . ?
O4 C10 H10B 109.7 . . ?
C9 C10 H10A 109.7 . . ?
C9 C10 H10B 109.7 . . ?
H10A C10 H10B 108.2 . . ?
C11 O5A C12A 120.3(3) . . ?
C10A O4A C9A 112.3(5) . . ?
O4A C10A H10C 108.5 . . ?
O4A C10A H10D 108.5 . . ?
H10C C10A H10D 107.5 . . ?
C11 C10A O4A 115.0(4) . . ?
C11 C10A H10C 108.5 . . ?
C11 C10A H10D 108.5 . . ?
O4A C9A H9AA 109.8 . . ?
O4A C9A H9AB 109.8 . . ?
O4A C9A C8A 109.5(5) . . ?
H9AA C9A H9AB 108.2 . . ?
C8A C9A H9AA 109.8 . . ?
C8A C9A H9AB 109.8 . . ?
O4 C11 C12 118.3(3) . . ?
O4 C11 H11A 107.7 . . ?
O4 C11 H11B 107.7 . . ?
C12 C11 H11A 107.7 . . ?
C12 C11 H11B 107.7 . . ?
O5A C11 H11C 107.9 . . ?
O5A C11 H11D 107.9 . . ?
C10A C11 O5A 117.6(3) . . ?
C10A C11 H11C 107.9 . . ?
C10A C11 H11D 107.9 . . ?
H11A C11 H11B 107.1 . . ?
H11C C11 H11D 107.2 . . ?
C9A C8A H8AA 109.7 . . ?
C9A C8A H8AB 109.7 . . ?
H8AA C8A H8AB 108.2 . . ?
O3A C8A C9A 109.6(4) . . ?
O3A C8A H8AA 109.7 . . ?
O3A C8A H8AB 109.7 . . ?
C7A O3A C8A 112.3(4) . . ?
O5A C12A H12C 106.7 . . ?
O5A C12A H12D 106.7 . . ?
H12C C12A H12D 106.6 . . ?
C13A C12A O5A 122.3(5) . . ?
C13A C12A H12C 106.7 . . ?
C13A C12A H12D 106.7 . . ?
C12A C13A H13C 106.7 . . ?
C12A C13A H13D 106.7 . . ?
C12A C13A O6A 122.4(4) . . ?
H13C C13A H13D 106.6 . . ?
O6A C13A H13C 106.7 . . ?
O6A C13A H13D 106.7 . . ?
H6AA C6A H6AB 108.2 . . ?
O2A C6A H6AA 109.7 . . ?
O2A C6A H6AB 109.7 . . ?
O2A C6A C7A 109.7(4) . . ?
C7A C6A H6AA 109.7 . . ?
C7A C6A H6AB 109.7 . . ?
C13A O6A C14A 131.4(4) . . ?
C6A O2A C5A 110.5(6) . . ?
C3 C14A O6A 114.4(3) . . ?
C3 C14A H14C 108.7 . . ?
C3 C14A H14D 108.7 . . ?
O6A C14A H14C 108.7 . . ?
O6A C14A H14D 108.7 . . ?
H14C C14A H14D 107.6 . . ?
H4AA C4A H4AB 108.1 . . ?
C5A C4A H4AA 109.6 . . ?
C5A C4A H4AB 109.6 . . ?
O1A C4A H4AA 109.6 . . ?
O1A C4A H4AB 109.6 . . ?
O1A C4A C5A 110.3(7) . . ?
O2A C5A C4A 106.5(8) . . ?
O2A C5A H5AA 110.4 . . ?
O2A C5A H5AB 110.4 . . ?
C4A C5A H5AA 110.4 . . ?
C4A C5A H5AB 110.4 . . ?
H5AA C5A H5AB 108.6 . . ?
C4A O1A C3 116.1(3) . . ?
O3A C7A C6A 108.1(4) . . ?
O3A C7A H7AA 110.1 . . ?
O3A C7A H7AB 110.1 . . ?
C6A C7A H7AA 110.1 . . ?
C6A C7A H7AB 110.1 . . ?
H7AA C7A H7AB 108.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S6 C18 S8 177.03(10) . . . . ?
Ni1 S6 C18 C19 -4.06(18) . . . . ?
Ni1 S2 C16 S4 -177.04(10) . . . . ?
Ni1 S2 C16 C15 2.62(18) . . . . ?
Ni1 S1 C15 S3 179.69(10) . . . . ?
Ni1 S1 C15 C16 0.35(18) . . . . ?
Ni1 S7 C19 S9 -177.38(10) . . . . ?
Ni1 S7 C19 C18 2.49(18) . . . . ?
S6 C18 C19 S7 1.1(2) . . . . ?
S6 C18 C19 S9 -178.98(10) . . . . ?
S1 C15 C16 S2 -2.1(2) . . . . ?
S1 C15 C16 S4 177.56(10) . . . . ?
S8 C18 C19 S7 -179.87(10) . . . . ?
S8 C18 C19 S9 0.0(2) . . . . ?
S3 C15 C16 S2 178.49(10) . . . . ?
S3 C15 C16 S4 -1.8(2) . . . . ?
N1 C1 C2 Cl1 72.0(3) . . . . ?
N1 C1 C2A Cl1A -79.9(9) . . . . ?
C18 S8 C20 S9 1.81(13) . . . . ?
C18 S8 C20 S10 -177.60(14) . . . . ?
C19 S9 C20 S8 -1.80(13) . . . . ?
C19 S9 C20 S10 177.61(14) . . . . ?
C15 S3 C17 S4 -1.89(13) . . . . ?
C15 S3 C17 S5 177.74(14) . . . . ?
C17 S4 C16 S2 -179.90(13) . . . . ?
C17 S4 C16 C15 0.42(17) . . . . ?
C17 S3 C15 S1 -177.12(13) . . . . ?
C17 S3 C15 C16 2.26(17) . . . . ?
C20 S8 C18 S6 177.86(13) . . . . ?
C20 S8 C18 C19 -1.12(17) . . . . ?
C20 S9 C19 S7 -179.02(13) . . . . ?
C20 S9 C19 C18 1.10(18) . . . . ?
C16 S4 C17 S3 1.11(13) . . . . ?
C16 S4 C17 S5 -178.52(14) . . . . ?
O1 C5 C6 O2 -66.3(9) . . . . ?
O3 C9 C10 O4 -65.6(6) . . . . ?
O6 C3 C4 O1 53.2(5) . . . . ?
C3 O6 C14 C13 158.9(5) . . . . ?
O5 C13 C14 O6 -6.0(9) . . . . ?
O5 C12 C11 O4 47.7(5) . . . . ?
O2 C7 C8 O3 62.6(6) . . . . ?
C9 O3 C8 C7 168.2(5) . . . . ?
C5 O1 C4 C3 -178.6(6) . . . . ?
C13 O5 C12 C11 153.6(5) . . . . ?
C14 O6 C3 C4 -176.2(4) . . . . ?
C4 O1 C5 C6 -175.5(6) . . . . ?
C7 O2 C6 C5 -177.6(7) . . . . ?
C12 O5 C13 C14 154.4(5) . . . . ?
C6 O2 C7 C8 -172.8(4) . . . . ?
C8 O3 C9 C10 -178.6(4) . . . . ?
C10 O4 C11 C12 -165.5(4) . . . . ?
O5A C12A C13A O6A -3.7(9) . . . . ?
O4A C10A C11 O5A 49.0(6) . . . . ?
O4A C9A C8A O3A -63.2(6) . . . . ?
C10A O4A C9A C8A -175.4(4) . . . . ?
C9A O4A C10A C11 -168.7(4) . . . . ?
C9A C8A O3A C7A 180.0(5) . . . . ?
C11 O4 C10 C9 -166.7(4) . . . . ?
C11 O5A C12A C13A 167.8(5) . . . . ?
C8A O3A C7A C6A 167.0(4) . . . . ?
C12A O5A C11 C10A -172.9(4) . . . . ?
C12A C13A O6A C14A 139.6(5) . . . . ?
C13A O6A C14A C3 152.3(5) . . . . ?
C6A O2A C5A C4A 179.9(6) . . . . ?
O2A C6A C7A O3A 61.4(6) . . . . ?
C14A C3 O1A C4A -174.9(4) . . . . ?
C5A C4A O1A C3 -167.4(6) . . . . ?
O1A C3 C14A O6A 53.7(5) . . . . ?
O1A C4A C5A O2A -65.8(9) . . . . ?
C7A C6A O2A C5A -170.3(7) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 7.274
_oxdiff_exptl_absorpt_empirical_full_min 0.402
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_333k-f
_database_code_depnum_ccdc_archive 'CCDC 2053402'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-18 downloaded from the CCDC.
;
_audit_creation_date             2020-11-24
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C2 H7 Cl N, C12 H24 O6'
_chemical_formula_sum            'C20 H31 Cl N Ni O6 S10'
_chemical_formula_weight         796.22
_chemical_melting_point          ?
_chemical_oxdiff_formula         C20H30NO6NiS10Cl
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.3046(5)
_cell_length_b                   12.3319(4)
_cell_length_c                   12.9008(6)
_cell_angle_alpha                90.991(3)
_cell_angle_beta                 110.208(4)
_cell_angle_gamma                96.173(3)
_cell_volume                     1675.11(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    12594
_cell_measurement_temperature    333
_cell_measurement_theta_max      27.4430
_cell_measurement_theta_min      1.7220
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.317
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45105
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             822
_exptl_crystal_size_max          0.69
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0948
_diffrn_reflns_av_unetI/netI     0.0561
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            27105
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.934
_diffrn_ambient_temperature      333
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -24.00 104.00   0.50    0.42    --   21.85  19.00  90.00  256
  2  ω    -21.00 104.00   0.50    0.42    --   21.85  57.00 120.00  250
  3  ω    -26.00 104.00   0.50    0.42    --   21.85  77.00 -90.00  260
  4  ω    -17.00  95.00   0.50    0.42    --   21.85  57.00-120.00  224
  5  ω    -22.00  60.00   0.50    0.42    --  -21.77  19.00-150.00  164
  6  ω    -40.00  56.00   0.50    0.42    --  -21.77  37.00  30.00  192
  7  ω    -49.00 -23.00   0.50    0.42    --  -21.77  57.00  90.00   52
  8  ω    -39.00  17.00   0.50    0.42    --  -21.77  37.00 -60.00  112
  9  ω     30.00  59.00   0.50    0.42    --  -21.77  37.00 -60.00   58
 10  ω      8.00  60.00   0.50    0.42    --   21.85-110.00 136.00  104
 11  ω    -18.00  80.00   0.50    0.42    --   21.85 -99.00  60.00  196
 12  ω      0.00  60.00   0.50    0.42    --  -21.77  57.00  90.00  120
 13  ω    -82.00  -3.00   0.50    0.42    --  -21.77 110.00-128.00  158
 14  ω    -18.00  36.00   0.50    0.42    --  -21.77 -99.00 -60.00  108
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0213697000
_diffrn_orient_matrix_UB_12      -0.0564091000
_diffrn_orient_matrix_UB_13      -0.0013483000
_diffrn_orient_matrix_UB_21      -0.0136562000
_diffrn_orient_matrix_UB_22      -0.0040691000
_diffrn_orient_matrix_UB_23      -0.0579804000
_diffrn_orient_matrix_UB_31      0.0623977000
_diffrn_orient_matrix_UB_32      -0.0126426000
_diffrn_orient_matrix_UB_33      0.0089805000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4604
_reflns_number_total             6845
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         6845
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0751
_refine_ls_R_factor_gt           0.0516
_refine_ls_restrained_S_all      0.985
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1420
_refine_ls_wR_factor_ref         0.1641
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
2. Rigid body (RIGU) restrains
 O3, C9, C10, O4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(Cl1A)=Sof(H1bc)=Sof(H1bd)=Sof(C2A)=Sof(H2Aa)=Sof(H2Ab)=1-FVAR(1)
 Sof(H1aa)=Sof(H1ab)=Sof(C2)=Sof(H2a)=Sof(H2b)=Sof(Cl1)=FVAR(1)
 Sof(H3bc)=Sof(H3bd)=Sof(O5A)=Sof(O4A)=Sof(C10A)=Sof(H10c)=Sof(H10d)=Sof(C9A)=
 Sof(H9Aa)=Sof(H9Ab)=Sof(H11c)=Sof(H11d)=Sof(C8A)=Sof(H8Aa)=Sof(H8Ab)=Sof(O3A)=
 Sof(C12A)=Sof(H12c)=Sof(H12d)=Sof(C13A)=Sof(H13c)=Sof(H13d)=Sof(C6A)=Sof(H6Aa)=
 Sof(H6Ab)=Sof(O6A)=Sof(O2A)=Sof(C14A)=Sof(H14c)=Sof(H14d)=Sof(C4A)=Sof(H4Aa)=
 Sof(H4Ab)=Sof(C5A)=Sof(H5Aa)=Sof(H5Ab)=Sof(O1A)=Sof(C7A)=Sof(H7Aa)=Sof(H7Ab)=1-
 FVAR(2)
 Sof(O4)=Sof(O1)=Sof(O3)=Sof(O6)=Sof(H3aa)=Sof(H3ab)=Sof(O5)=Sof(O2)=Sof(C9)=
 Sof(H9a)=Sof(H9b)=Sof(C5)=Sof(H5a)=Sof(H5b)=Sof(C13)=Sof(H13a)=Sof(H13b)=
 Sof(C14)=Sof(H14a)=Sof(H14b)=Sof(C4)=Sof(H4a)=Sof(H4b)=Sof(C7)=Sof(H7a)=
 Sof(H7b)=Sof(C12)=Sof(H12a)=Sof(H12b)=Sof(C6)=Sof(H6a)=Sof(H6b)=Sof(C8)=
 Sof(H8a)=Sof(H8b)=Sof(C10)=Sof(H10a)=Sof(H10b)=Sof(H11a)=Sof(H11b)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1bc,H1bd), C1(H1aa,H1ab), C3(H3aa,H3ab), C3(H3bc,H3bd), C9(H9a,H9b),
 C5(H5a,H5b), C13(H13a,H13b), C14(H14a,H14b), C4(H4a,H4b), C7(H7a,H7b), C2(H2a,
 H2b), C12(H12a,H12b), C6(H6a,H6b), C2A(H2Aa,H2Ab), C8(H8a,H8b), C10(H10a,H10b),
  C10A(H10c,H10d), C9A(H9Aa,H9Ab), C11(H11a,H11b), C11(H11c,H11d), C8A(H8Aa,
 H8Ab), C12A(H12c,H12d), C13A(H13c,H13d), C6A(H6Aa,H6Ab), C14A(H14c,H14d),
 C4A(H4Aa,H4Ab), C5A(H5Aa,H5Ab), C7A(H7Aa,H7Ab)
4.b Idealised Me refined as rotating group:
 N1(H1a,H1b,H1c)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.84525(4) 0.88974(3) 0.51211(3) 0.05647(17) Uani 1 1 d . . . . .
S6 S 0.69207(8) 0.97516(8) 0.52340(7) 0.0682(3) Uani 1 1 d . . . . .
S2 S 1.00508(8) 0.81255(8) 0.50621(7) 0.0694(3) Uani 1 1 d . . . . .
S1 S 0.78923(9) 0.92754(8) 0.34028(7) 0.0695(3) Uani 1 1 d . . . . .
S7 S 0.89945(9) 0.84554(8) 0.68169(8) 0.0715(3) Uani 1 1 d . . . . .
S8 S 0.61347(8) 1.02476(8) 0.72011(8) 0.0685(3) Uani 1 1 d . . . . .
S9 S 0.80150(9) 0.90268(9) 0.86391(8) 0.0748(3) Uani 1 1 d . . . . .
S4 S 1.09878(9) 0.77201(9) 0.31760(8) 0.0755(3) Uani 1 1 d . . . . .
S3 S 0.90650(9) 0.88488(9) 0.16686(8) 0.0762(3) Uani 1 1 d . . . . .
S10 S 0.62570(11) 1.00265(9) 0.95215(9) 0.0870(3) Uani 1 1 d . . . . .
S5 S 1.08883(11) 0.78578(11) 0.08577(9) 0.0928(4) Uani 1 1 d . . . . .
Cl1A Cl 0.8260(11) 0.4519(8) 0.5244(8) 0.0986(19) Uani 0.360(10) 1 d . . P A 2
N1 N 0.6657(3) 0.5020(2) 0.2565(2) 0.0664(7) Uani 1 1 d . . . . .
H1A H 0.663617 0.514984 0.188249 0.080 Uiso 1 1 calc R U . . .
H1B H 0.590031 0.508485 0.261169 0.080 Uiso 1 1 calc R U . . .
H1C H 0.684861 0.434554 0.271786 0.080 Uiso 1 1 calc R U . . .
C18 C 0.7083(3) 0.9647(3) 0.6596(3) 0.0580(8) Uani 1 1 d . . . . .
C19 C 0.7977(3) 0.9079(3) 0.7281(3) 0.0611(8) Uani 1 1 d . . . . .
C15 C 0.9029(3) 0.8759(3) 0.3002(3) 0.0600(8) Uani 1 1 d . . . . .
C17 C 1.0342(3) 0.8126(3) 0.1845(3) 0.0677(9) Uani 1 1 d . . . . .
C20 C 0.6774(3) 0.9780(3) 0.8512(3) 0.0640(8) Uani 1 1 d . . . . .
C16 C 0.9942(3) 0.8243(3) 0.3718(3) 0.0601(8) Uani 1 1 d . . . . .
O4 O 0.7046(9) 0.6190(7) 0.0807(8) 0.083(2) Uani 0.522(9) 1 d . . P B 1
O1 O 0.5105(8) 0.3197(7) 0.3185(9) 0.088(2) Uani 0.522(9) 1 d . . P B 1
O3 O 0.4934(8) 0.6511(8) 0.1421(9) 0.090(2) Uani 0.522(9) 1 d . . P B 1
O6 O 0.7213(6) 0.2831(6) 0.2650(6) 0.0736(19) Uani 0.522(9) 1 d . . P B 1
C1 C 0.7638(4) 0.5822(4) 0.3372(4) 0.0936(13) Uani 1 1 d . . . . .
H1BC H 0.800610 0.633843 0.297583 0.112 Uiso 0.360(10) 1 calc R U P A 2
H1BD H 0.724332 0.622635 0.378851 0.112 Uiso 0.360(10) 1 calc R U P A 2
H1AA H 0.846593 0.571691 0.334701 0.112 Uiso 0.640(10) 1 calc R U P A 1
H1AB H 0.747307 0.655556 0.315376 0.112 Uiso 0.640(10) 1 calc R U P A 1
C3 C 0.6468(5) 0.2039(4) 0.3019(6) 0.1159(19) Uani 1 1 d . . . . .
H3AA H 0.582407 0.165585 0.237290 0.139 Uiso 0.522(9) 1 calc R U P B 1
H3AB H 0.701087 0.150838 0.340785 0.139 Uiso 0.522(9) 1 calc R U P B 1
H3BC H 0.712380 0.211930 0.374685 0.139 Uiso 0.478(9) 1 calc R U P B 2
H3BD H 0.598755 0.132413 0.295466 0.139 Uiso 0.478(9) 1 calc R U P B 2
O5 O 0.7892(9) 0.4161(8) 0.1170(7) 0.091(2) Uani 0.522(9) 1 d . . P B 1
O2 O 0.4312(10) 0.5276(9) 0.3001(9) 0.101(3) Uani 0.522(9) 1 d . . P B 1
C9 C 0.550(2) 0.7332(16) 0.0951(14) 0.095(4) Uani 0.522(9) 1 d . . P B 1
H9A H 0.618177 0.777554 0.152393 0.114 Uiso 0.522(9) 1 calc R U P B 1
H9B H 0.487972 0.780119 0.055107 0.114 Uiso 0.522(9) 1 calc R U P B 1
C5 C 0.433(2) 0.358(2) 0.3676(17) 0.108(6) Uani 0.522(9) 1 d . . P B 1
H5A H 0.486849 0.390896 0.439789 0.130 Uiso 0.522(9) 1 calc R U P B 1
H5B H 0.380809 0.295857 0.379977 0.130 Uiso 0.522(9) 1 calc R U P B 1
C13 C 0.853(3) 0.321(3) 0.156(2) 0.117(7) Uani 0.522(9) 1 d . . P B 1
H13A H 0.872877 0.287789 0.096950 0.141 Uiso 0.522(9) 1 calc R U P B 1
H13B H 0.931776 0.344407 0.216368 0.141 Uiso 0.522(9) 1 calc R U P B 1
C14 C 0.7809(10) 0.2462(12) 0.1923(9) 0.088(4) Uani 0.522(9) 1 d . . P B 1
H14A H 0.834451 0.191976 0.229327 0.106 Uiso 0.522(9) 1 calc R U P B 1
H14B H 0.714947 0.209300 0.127790 0.106 Uiso 0.522(9) 1 calc R U P B 1
C4 C 0.5884(10) 0.2395(8) 0.3682(12) 0.096(3) Uani 0.522(9) 1 d . . P B 1
H4A H 0.651552 0.269803 0.437550 0.115 Uiso 0.522(9) 1 calc R U P B 1
H4B H 0.537047 0.178407 0.384224 0.115 Uiso 0.522(9) 1 calc R U P B 1
C7 C 0.357(2) 0.6076(18) 0.244(2) 0.116(6) Uani 0.522(9) 1 d . . P B 1
H7A H 0.316206 0.638233 0.289909 0.140 Uiso 0.522(9) 1 calc R U P B 1
H7B H 0.291971 0.574327 0.176684 0.140 Uiso 0.522(9) 1 calc R U P B 1
C2 C 0.7661(8) 0.5719(6) 0.4512(6) 0.098(3) Uani 0.640(10) 1 d . . P A 1
H2A H 0.679835 0.566442 0.451060 0.118 Uiso 0.640(10) 1 calc R U P A 1
H2B H 0.812698 0.637474 0.495441 0.118 Uiso 0.640(10) 1 calc R U P A 1
C12 C 0.8562(15) 0.5060(12) 0.0837(11) 0.107(4) Uani 0.522(9) 1 d . . P B 1
H12A H 0.920193 0.543449 0.149065 0.129 Uiso 0.522(9) 1 calc R U P B 1
H12B H 0.899558 0.477975 0.037802 0.129 Uiso 0.522(9) 1 calc R U P B 1
C6 C 0.3543(14) 0.4332(14) 0.3145(11) 0.105(4) Uani 0.522(9) 1 d . . P B 1
H6A H 0.304584 0.453156 0.358359 0.126 Uiso 0.522(9) 1 calc R U P B 1
H6B H 0.296390 0.401939 0.243164 0.126 Uiso 0.522(9) 1 calc R U P B 1
C2A C 0.8584(11) 0.5294(12) 0.4091(11) 0.103(5) Uani 0.360(10) 1 d . . P A 2
H2AA H 0.931227 0.583688 0.443299 0.123 Uiso 0.360(10) 1 calc R U P A 2
H2AB H 0.883488 0.478171 0.365050 0.123 Uiso 0.360(10) 1 calc R U P A 2
C8 C 0.4390(12) 0.6965(11) 0.2141(13) 0.107(4) Uani 0.522(9) 1 d . . P B 1
H8A H 0.388297 0.752843 0.178080 0.128 Uiso 0.522(9) 1 calc R U P B 1
H8B H 0.505492 0.729276 0.280565 0.128 Uiso 0.522(9) 1 calc R U P B 1
C10 C 0.6010(15) 0.6795(9) 0.0183(13) 0.096(3) Uani 0.522(9) 1 d . . P B 1
H10A H 0.534025 0.629857 -0.034498 0.116 Uiso 0.522(9) 1 calc R U P B 1
H10B H 0.631730 0.734202 -0.022501 0.116 Uiso 0.522(9) 1 calc R U P B 1
O5A O 0.7753(8) 0.4734(10) 0.0809(8) 0.088(2) Uani 0.478(9) 1 d . . P B 2
O4A O 0.6460(12) 0.6524(8) 0.0878(8) 0.089(3) Uani 0.478(9) 1 d . . P B 2
C10A C 0.6946(18) 0.6336(12) 0.0050(15) 0.120(5) Uani 0.478(9) 1 d . . P B 2
H10C H 0.626137 0.598945 -0.059136 0.143 Uiso 0.478(9) 1 calc R U P B 2
H10D H 0.724367 0.703531 -0.016144 0.143 Uiso 0.478(9) 1 calc R U P B 2
C9A C 0.535(2) 0.7073(18) 0.0479(16) 0.095(5) Uani 0.478(9) 1 d . . P B 2
H9AA H 0.468579 0.662393 -0.010663 0.114 Uiso 0.478(9) 1 calc R U P B 2
H9AB H 0.554010 0.775931 0.018200 0.114 Uiso 0.478(9) 1 calc R U P B 2
C11 C 0.7829(10) 0.5760(6) 0.0292(7) 0.147(3) Uani 1 1 d . . . . .
H11A H 0.728684 0.540910 -0.041701 0.177 Uiso 0.522(9) 1 calc R U P B 1
H11B H 0.836029 0.636476 0.014502 0.177 Uiso 0.522(9) 1 calc R U P B 1
H11C H 0.858013 0.621060 0.077625 0.177 Uiso 0.478(9) 1 calc R U P B 2
H11D H 0.798384 0.559913 -0.038542 0.177 Uiso 0.478(9) 1 calc R U P B 2
C8A C 0.4909(14) 0.7275(14) 0.1397(13) 0.103(4) Uani 0.478(9) 1 d . . P B 2
H8AA H 0.557880 0.772329 0.197540 0.124 Uiso 0.478(9) 1 calc R U P B 2
H8AB H 0.418309 0.768158 0.114237 0.124 Uiso 0.478(9) 1 calc R U P B 2
O3A O 0.4574(10) 0.6333(8) 0.1832(8) 0.087(2) Uani 0.478(9) 1 d . . P B 2
C12A C 0.8763(14) 0.4089(19) 0.1220(12) 0.118(6) Uani 0.478(9) 1 d . . P B 2
H12C H 0.909073 0.391774 0.064134 0.142 Uiso 0.478(9) 1 calc R U P B 2
H12D H 0.944797 0.448655 0.182862 0.142 Uiso 0.478(9) 1 calc R U P B 2
C13A C 0.832(4) 0.318(4) 0.156(3) 0.23(2) Uani 0.478(9) 1 d . . P B 2
H13C H 0.785564 0.273361 0.088897 0.275 Uiso 0.478(9) 1 calc R U P B 2
H13D H 0.907184 0.282581 0.193003 0.275 Uiso 0.478(9) 1 calc R U P B 2
C6A C 0.3561(18) 0.5434(19) 0.2963(14) 0.116(6) Uani 0.478(9) 1 d . . P B 2
H6AA H 0.320003 0.554118 0.353301 0.139 Uiso 0.478(9) 1 calc R U P B 2
H6AB H 0.288641 0.511099 0.230156 0.139 Uiso 0.478(9) 1 calc R U P B 2
O6A O 0.7643(8) 0.3040(7) 0.2172(8) 0.083(2) Uani 0.478(9) 1 d . . P B 2
O2A O 0.4521(11) 0.4726(11) 0.3324(9) 0.100(3) Uani 0.478(9) 1 d . . P B 2
C14A C 0.7018(11) 0.2060(11) 0.2279(10) 0.092(3) Uani 0.478(9) 1 d . . P B 2
H14C H 0.637596 0.182493 0.156634 0.110 Uiso 0.478(9) 1 calc R U P B 2
H14D H 0.762057 0.152806 0.245656 0.110 Uiso 0.478(9) 1 calc R U P B 2
C4A C 0.5089(18) 0.2960(14) 0.3803(17) 0.117(6) Uani 0.478(9) 1 d . . P B 2
H4AA H 0.574781 0.328367 0.447348 0.140 Uiso 0.478(9) 1 calc R U P B 2
H4AB H 0.478745 0.223611 0.395745 0.140 Uiso 0.478(9) 1 calc R U P B 2
C5A C 0.406(4) 0.361(2) 0.350(3) 0.20(2) Uani 0.478(9) 1 d . . P B 2
H5AA H 0.370445 0.363246 0.408739 0.241 Uiso 0.478(9) 1 calc R U P B 2
H5AB H 0.339601 0.329673 0.283235 0.241 Uiso 0.478(9) 1 calc R U P B 2
O1A O 0.5611(9) 0.2870(8) 0.2957(7) 0.089(2) Uani 0.478(9) 1 d . . P B 2
C7A C 0.415(2) 0.653(2) 0.272(2) 0.117(7) Uani 0.478(9) 1 d . . P B 2
H7AA H 0.351652 0.704082 0.251269 0.141 Uiso 0.478(9) 1 calc R U P B 2
H7AB H 0.484892 0.684173 0.336330 0.141 Uiso 0.478(9) 1 calc R U P B 2
Cl1 Cl 0.8305(7) 0.4674(6) 0.5074(6) 0.146(2) Uani 0.640(10) 1 d . . P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S6 2.1658(9) . ?
Ni1 S2 2.1538(9) . ?
Ni1 S1 2.1592(10) . ?
Ni1 S7 2.1553(10) . ?
S6 C18 1.712(3) . ?
S2 C16 1.705(3) . ?
S1 C15 1.718(3) . ?
S7 C19 1.709(3) . ?
S8 C18 1.742(3) . ?
S8 C20 1.730(4) . ?
S9 C19 1.741(3) . ?
S9 C20 1.728(3) . ?
S4 C17 1.725(4) . ?
S4 C16 1.738(3) . ?
S3 C15 1.739(3) . ?
S3 C17 1.729(4) . ?
S10 C20 1.637(3) . ?
S5 C17 1.639(3) . ?
Cl1A C2A 1.900(16) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.491(5) . ?
C18 C19 1.360(5) . ?
C15 C16 1.351(5) . ?
O4 C10 1.461(18) . ?
O4 C11 1.414(12) . ?
O1 C5 1.36(3) . ?
O1 C4 1.408(16) . ?
O3 C9 1.40(2) . ?
O3 C8 1.416(18) . ?
O6 C3 1.418(10) . ?
O6 C14 1.423(14) . ?
C1 H1BC 0.9700 . ?
C1 H1BD 0.9700 . ?
C1 H1AA 0.9700 . ?
C1 H1AB 0.9700 . ?
C1 C2 1.470(8) . ?
C1 C2A 1.384(12) . ?
C3 H3AA 0.9700 . ?
C3 H3AB 0.9700 . ?
C3 H3BC 0.9700 . ?
C3 H3BD 0.9700 . ?
C3 C4 1.340(15) . ?
C3 C14A 1.307(15) . ?
C3 O1A 1.469(13) . ?
O5 C13 1.44(3) . ?
O5 C12 1.430(17) . ?
O2 C7 1.41(3) . ?
O2 C6 1.43(2) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.49(2) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.38(3) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.36(4) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.49(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 Cl1 1.608(10) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C11 1.304(16) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
O5A C11 1.449(14) . ?
O5A C12A 1.42(2) . ?
O4A C10A 1.39(2) . ?
O4A C9A 1.43(2) . ?
C10A H10C 0.9700 . ?
C10A H10D 0.9700 . ?
C10A C11 1.242(19) . ?
C9A H9AA 0.9700 . ?
C9A H9AB 0.9700 . ?
C9A C8A 1.46(3) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 H11C 0.9700 . ?
C11 H11D 0.9700 . ?
C8A H8AA 0.9700 . ?
C8A H8AB 0.9700 . ?
C8A O3A 1.37(2) . ?
O3A C7A 1.41(2) . ?
C12A H12C 0.9700 . ?
C12A H12D 0.9700 . ?
C12A C13A 1.32(5) . ?
C13A H13C 0.9700 . ?
C13A H13D 0.9700 . ?
C13A O6A 1.28(3) . ?
C6A H6AA 0.9700 . ?
C6A H6AB 0.9700 . ?
C6A O2A 1.42(2) . ?
C6A C7A 1.53(3) . ?
O6A C14A 1.367(17) . ?
O2A C5A 1.47(3) . ?
C14A H14C 0.9700 . ?
C14A H14D 0.9700 . ?
C4A H4AA 0.9700 . ?
C4A H4AB 0.9700 . ?
C4A C5A 1.43(5) . ?
C4A O1A 1.417(18) . ?
C5A H5AA 0.9700 . ?
C5A H5AB 0.9700 . ?
C7A H7AA 0.9700 . ?
C7A H7AB 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S2 Ni1 S6 176.74(4) . . ?
S2 Ni1 S1 93.00(3) . . ?
S2 Ni1 S7 86.12(3) . . ?
S1 Ni1 S6 87.93(3) . . ?
S7 Ni1 S6 93.05(3) . . ?
S7 Ni1 S1 177.84(4) . . ?
C18 S6 Ni1 101.96(11) . . ?
C16 S2 Ni1 102.30(12) . . ?
C15 S1 Ni1 102.12(12) . . ?
C19 S7 Ni1 102.32(12) . . ?
C20 S8 C18 97.83(15) . . ?
C20 S9 C19 97.70(16) . . ?
C17 S4 C16 97.92(17) . . ?
C17 S3 C15 97.31(17) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
S6 C18 S8 123.13(19) . . ?
C19 C18 S6 121.3(2) . . ?
C19 C18 S8 115.6(2) . . ?
S7 C19 S9 122.6(2) . . ?
C18 C19 S7 121.3(2) . . ?
C18 C19 S9 116.1(2) . . ?
S1 C15 S3 122.6(2) . . ?
C16 C15 S1 120.9(3) . . ?
C16 C15 S3 116.5(2) . . ?
S4 C17 S3 112.74(18) . . ?
S5 C17 S4 123.5(2) . . ?
S5 C17 S3 123.8(2) . . ?
S9 C20 S8 112.71(18) . . ?
S10 C20 S8 123.6(2) . . ?
S10 C20 S9 123.7(2) . . ?
S2 C16 S4 122.8(2) . . ?
C15 C16 S2 121.7(2) . . ?
C15 C16 S4 115.5(3) . . ?
C11 O4 C10 120.7(12) . . ?
C5 O1 C4 120.2(16) . . ?
C9 O3 C8 110.9(13) . . ?
C3 O6 C14 117.6(9) . . ?
N1 C1 H1BC 109.5 . . ?
N1 C1 H1BD 109.5 . . ?
N1 C1 H1AA 109.0 . . ?
N1 C1 H1AB 109.0 . . ?
H1BC C1 H1BD 108.1 . . ?
H1AA C1 H1AB 107.8 . . ?
C2 C1 N1 112.9(4) . . ?
C2 C1 H1AA 109.0 . . ?
C2 C1 H1AB 109.0 . . ?
C2A C1 N1 110.7(6) . . ?
C2A C1 H1BC 109.5 . . ?
C2A C1 H1BD 109.5 . . ?
O6 C3 H3AA 108.0 . . ?
O6 C3 H3AB 108.0 . . ?
H3AA C3 H3AB 107.2 . . ?
H3BC C3 H3BD 107.4 . . ?
C4 C3 O6 117.4(6) . . ?
C4 C3 H3AA 108.0 . . ?
C4 C3 H3AB 108.0 . . ?
C14A C3 H3BC 108.2 . . ?
C14A C3 H3BD 108.2 . . ?
C14A C3 O1A 116.2(7) . . ?
O1A C3 H3BC 108.2 . . ?
O1A C3 H3BD 108.2 . . ?
C12 O5 C13 119.1(17) . . ?
C7 O2 C6 112.0(14) . . ?
O3 C9 H9A 110.2 . . ?
O3 C9 H9B 110.2 . . ?
O3 C9 C10 107.7(14) . . ?
H9A C9 H9B 108.5 . . ?
C10 C9 H9A 110.2 . . ?
C10 C9 H9B 110.2 . . ?
O1 C5 H5A 107.6 . . ?
O1 C5 H5B 107.6 . . ?
O1 C5 C6 118.8(14) . . ?
H5A C5 H5B 107.0 . . ?
C6 C5 H5A 107.6 . . ?
C6 C5 H5B 107.6 . . ?
O5 C13 H13A 109.1 . . ?
O5 C13 H13B 109.1 . . ?
H13A C13 H13B 107.8 . . ?
C14 C13 O5 112.5(19) . . ?
C14 C13 H13A 109.1 . . ?
C14 C13 H13B 109.1 . . ?
O6 C14 H14A 107.8 . . ?
O6 C14 H14B 107.8 . . ?
C13 C14 O6 118.2(15) . . ?
C13 C14 H14A 107.8 . . ?
C13 C14 H14B 107.8 . . ?
H14A C14 H14B 107.1 . . ?
O1 C4 H4A 109.4 . . ?
O1 C4 H4B 109.4 . . ?
C3 C4 O1 111.3(14) . . ?
C3 C4 H4A 109.4 . . ?
C3 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
O2 C7 H7A 109.6 . . ?
O2 C7 H7B 109.6 . . ?
O2 C7 C8 110.4(15) . . ?
H7A C7 H7B 108.1 . . ?
C8 C7 H7A 109.6 . . ?
C8 C7 H7B 109.6 . . ?
C1 C2 H2A 109.0 . . ?
C1 C2 H2B 109.0 . . ?
C1 C2 Cl1 112.9(6) . . ?
H2A C2 H2B 107.8 . . ?
Cl1 C2 H2A 109.0 . . ?
Cl1 C2 H2B 109.0 . . ?
O5 C12 H12A 108.9 . . ?
O5 C12 H12B 108.9 . . ?
H12A C12 H12B 107.7 . . ?
C11 C12 O5 113.4(14) . . ?
C11 C12 H12A 108.9 . . ?
C11 C12 H12B 108.9 . . ?
O2 C6 H6A 110.1 . . ?
O2 C6 H6B 110.1 . . ?
C5 C6 O2 108.2(15) . . ?
C5 C6 H6A 110.1 . . ?
C5 C6 H6B 110.1 . . ?
H6A C6 H6B 108.4 . . ?
Cl1A C2A H2AA 107.4 . . ?
Cl1A C2A H2AB 107.4 . . ?
C1 C2A Cl1A 119.6(9) . . ?
C1 C2A H2AA 107.4 . . ?
C1 C2A H2AB 107.4 . . ?
H2AA C2A H2AB 107.0 . . ?
O3 C8 C7 108.7(13) . . ?
O3 C8 H8A 109.9 . . ?
O3 C8 H8B 109.9 . . ?
C7 C8 H8A 109.9 . . ?
C7 C8 H8B 109.9 . . ?
H8A C8 H8B 108.3 . . ?
O4 C10 C9 109.9(15) . . ?
O4 C10 H10A 109.7 . . ?
O4 C10 H10B 109.7 . . ?
C9 C10 H10A 109.7 . . ?
C9 C10 H10B 109.7 . . ?
H10A C10 H10B 108.2 . . ?
C12A O5A C11 125.1(14) . . ?
C10A O4A C9A 111.5(17) . . ?
O4A C10A H10C 108.4 . . ?
O4A C10A H10D 108.4 . . ?
H10C C10A H10D 107.4 . . ?
C11 C10A O4A 115.6(19) . . ?
C11 C10A H10C 108.4 . . ?
C11 C10A H10D 108.4 . . ?
O4A C9A H9AA 110.0 . . ?
O4A C9A H9AB 110.0 . . ?
O4A C9A C8A 108.5(15) . . ?
H9AA C9A H9AB 108.4 . . ?
C8A C9A H9AA 110.0 . . ?
C8A C9A H9AB 110.0 . . ?
O4 C11 H11A 108.2 . . ?
O4 C11 H11B 108.2 . . ?
C12 C11 O4 116.6(8) . . ?
C12 C11 H11A 108.2 . . ?
C12 C11 H11B 108.2 . . ?
O5A C11 H11C 106.9 . . ?
O5A C11 H11D 106.9 . . ?
C10A C11 O5A 121.7(9) . . ?
C10A C11 H11C 106.9 . . ?
C10A C11 H11D 106.9 . . ?
H11A C11 H11B 107.3 . . ?
H11C C11 H11D 106.7 . . ?
C9A C8A H8AA 109.0 . . ?
C9A C8A H8AB 109.0 . . ?
H8AA C8A H8AB 107.8 . . ?
O3A C8A C9A 113.0(17) . . ?
O3A C8A H8AA 109.0 . . ?
O3A C8A H8AB 109.0 . . ?
C8A O3A C7A 112.9(17) . . ?
O5A C12A H12C 110.1 . . ?
O5A C12A H12D 110.1 . . ?
H12C C12A H12D 108.4 . . ?
C13A C12A O5A 108(2) . . ?
C13A C12A H12C 110.1 . . ?
C13A C12A H12D 110.1 . . ?
C12A C13A H13C 104.7 . . ?
C12A C13A H13D 104.7 . . ?
H13C C13A H13D 105.7 . . ?
O6A C13A C12A 130(3) . . ?
O6A C13A H13C 104.7 . . ?
O6A C13A H13D 104.7 . . ?
H6AA C6A H6AB 108.3 . . ?
O2A C6A H6AA 109.9 . . ?
O2A C6A H6AB 109.9 . . ?
O2A C6A C7A 109.1(15) . . ?
C7A C6A H6AA 109.9 . . ?
C7A C6A H6AB 109.9 . . ?
C13A O6A C14A 125(2) . . ?
C6A O2A C5A 114(2) . . ?
C3 C14A O6A 116.7(15) . . ?
C3 C14A H14C 108.1 . . ?
C3 C14A H14D 108.1 . . ?
O6A C14A H14C 108.1 . . ?
O6A C14A H14D 108.1 . . ?
H14C C14A H14D 107.3 . . ?
H4AA C4A H4AB 107.9 . . ?
C5A C4A H4AA 109.2 . . ?
C5A C4A H4AB 109.2 . . ?
O1A C4A H4AA 109.2 . . ?
O1A C4A H4AB 109.2 . . ?
O1A C4A C5A 112(2) . . ?
O2A C5A H5AA 109.8 . . ?
O2A C5A H5AB 109.8 . . ?
C4A C5A O2A 110(2) . . ?
C4A C5A H5AA 109.8 . . ?
C4A C5A H5AB 109.8 . . ?
H5AA C5A H5AB 108.2 . . ?
C4A O1A C3 118.8(13) . . ?
O3A C7A C6A 107.2(16) . . ?
O3A C7A H7AA 110.3 . . ?
O3A C7A H7AB 110.3 . . ?
C6A C7A H7AA 110.3 . . ?
C6A C7A H7AB 110.3 . . ?
H7AA C7A H7AB 108.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S6 C18 S8 177.01(17) . . . . ?
Ni1 S6 C18 C19 -2.9(3) . . . . ?
Ni1 S2 C16 S4 -178.35(17) . . . . ?
Ni1 S2 C16 C15 2.0(3) . . . . ?
Ni1 S1 C15 S3 -179.17(17) . . . . ?
Ni1 S1 C15 C16 1.7(3) . . . . ?
Ni1 S7 C19 S9 -178.25(18) . . . . ?
Ni1 S7 C19 C18 1.9(3) . . . . ?
S6 C18 C19 S7 0.7(4) . . . . ?
S6 C18 C19 S9 -179.13(18) . . . . ?
S1 C15 C16 S2 -2.6(4) . . . . ?
S1 C15 C16 S4 177.67(16) . . . . ?
S8 C18 C19 S7 -179.21(17) . . . . ?
S8 C18 C19 S9 1.0(4) . . . . ?
S3 C15 C16 S2 178.20(17) . . . . ?
S3 C15 C16 S4 -1.5(4) . . . . ?
N1 C1 C2 Cl1 74.9(7) . . . . ?
N1 C1 C2A Cl1A -75.2(11) . . . . ?
C18 S8 C20 S9 2.2(2) . . . . ?
C18 S8 C20 S10 -177.8(2) . . . . ?
C19 S9 C20 S8 -1.8(2) . . . . ?
C19 S9 C20 S10 178.2(2) . . . . ?
C15 S3 C17 S4 -2.1(2) . . . . ?
C15 S3 C17 S5 178.1(2) . . . . ?
C17 S4 C16 S2 -179.7(2) . . . . ?
C17 S4 C16 C15 0.0(3) . . . . ?
C17 S3 C15 S1 -176.9(2) . . . . ?
C17 S3 C15 C16 2.2(3) . . . . ?
C20 S8 C18 S6 178.2(2) . . . . ?
C20 S8 C18 C19 -1.9(3) . . . . ?
C20 S9 C19 S7 -179.3(2) . . . . ?
C20 S9 C19 C18 0.5(3) . . . . ?
C16 S4 C17 S3 1.5(2) . . . . ?
C16 S4 C17 S5 -178.7(2) . . . . ?
O1 C5 C6 O2 -60(2) . . . . ?
O3 C9 C10 O4 -66.3(14) . . . . ?
O6 C3 C4 O1 55.9(10) . . . . ?
C3 O6 C14 C13 -180.0(15) . . . . ?
O5 C13 C14 O6 -48(2) . . . . ?
O5 C12 C11 O4 53.9(13) . . . . ?
O2 C7 C8 O3 62.1(19) . . . . ?
C9 O3 C8 C7 168.4(15) . . . . ?
C5 O1 C4 C3 173.4(13) . . . . ?
C13 O5 C12 C11 166.7(13) . . . . ?
C14 O6 C3 C4 -178.4(8) . . . . ?
C4 O1 C5 C6 -177.2(15) . . . . ?
C7 O2 C6 C5 178.4(17) . . . . ?
C12 O5 C13 C14 175.5(14) . . . . ?
C6 O2 C7 C8 -171.0(14) . . . . ?
C8 O3 C9 C10 -178.2(12) . . . . ?
C10 O4 C11 C12 -167.1(11) . . . . ?
O5A C12A C13A O6A -47(5) . . . . ?
O4A C10A C11 O5A 48.1(16) . . . . ?
O4A C9A C8A O3A -61.8(17) . . . . ?
C10A O4A C9A C8A -178.3(14) . . . . ?
C9A O4A C10A C11 -172.4(13) . . . . ?
C9A C8A O3A C7A -179.7(16) . . . . ?
C11 O4 C10 C9 -169.3(11) . . . . ?
C11 O5A C12A C13A -176(2) . . . . ?
C8A O3A C7A C6A 168.9(15) . . . . ?
C12A O5A C11 C10A -172.7(13) . . . . ?
C12A C13A O6A C14A 165(3) . . . . ?
C13A O6A C14A C3 173(2) . . . . ?
C6A O2A C5A C4A 176.8(17) . . . . ?
O2A C6A C7A O3A 63.5(18) . . . . ?
C14A C3 O1A C4A -173.6(11) . . . . ?
C5A C4A O1A C3 -166.3(13) . . . . ?
O1A C3 C14A O6A 52.0(11) . . . . ?
O1A C4A C5A O2A -62(2) . . . . ?
C7A C6A O2A C5A -175.4(17) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.023
_oxdiff_exptl_absorpt_empirical_full_min 0.358
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_313k
_database_code_depnum_ccdc_archive 'CCDC 2053309'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-18 downloaded from the CCDC.
;
_audit_creation_date             2020-11-10
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C2 H7 Br1 N, C12 H24 O6'
_chemical_formula_sum            'C20 H31 Br N Ni O6 S10'
_chemical_formula_weight         840.68
_chemical_melting_point          ?
_chemical_oxdiff_formula         BrCHNONiS
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.1694(4)
_cell_length_b                   12.1413(4)
_cell_length_c                   13.7408(6)
_cell_angle_alpha                65.543(4)
_cell_angle_beta                 81.123(3)
_cell_angle_gamma                78.362(3)
_cell_volume                     1656.09(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    14855
_cell_measurement_temperature    313
_cell_measurement_theta_max      28.8650
_cell_measurement_theta_min      1.8570
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.458
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65712
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             858
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0668
_diffrn_reflns_av_unetI/netI     0.0631
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.892
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            33146
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.032
_diffrn_reflns_theta_min         1.867
_diffrn_ambient_temperature      313
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -25.00 104.00   0.50    1.37    --   21.69  19.00 -30.00  258
  2  ω     46.00  93.00   0.50    1.37    --   21.69 178.00 -60.00   94
  3  ω     58.00 103.00   0.50    1.37    --   21.69 158.00-116.00   90
  4  ω    -19.00 101.00   0.50    1.37    --   21.69  57.00   0.00  240
  5  ω    -25.00  58.00   0.50    1.37    --  -21.62  19.00  60.00  166
  6  ω    -63.00 -17.00   0.50    1.37    --  -21.62 118.00  89.00   92
  7  ω   -109.00 -78.00   0.50    1.37    --  -21.62 158.00-116.00   62
  8  ω    -23.00  20.00   0.50    1.37    --   21.69 -19.00 -90.00   86
  9  ω    -68.00  44.00   0.50    1.37    --   21.69 -37.00-120.00  224
 10  ω    -75.00 -31.00   0.50    1.37    --   21.69 -19.00 -90.00   88
 11  ω     68.00 100.00   0.50    1.37    --   21.69-158.00-150.00   64
 12  ω     20.00  81.00   0.50    1.37    --   21.69-118.00   3.00  122
 13  ω    -17.00  38.00   0.50    1.37    --  -21.62 -99.00  60.00  110
 14  ω    -17.00  38.00   0.50    1.37    --  -21.62 -99.00   0.00  110
 15  ω    -19.00  20.00   0.50    1.37    --  -21.62 -57.00  30.00   78
 16  ω   -108.00 -33.00   0.50    1.37    --  -21.62 -57.00  30.00  150
 17  ω    -81.00 -55.00   0.50    1.37    --  -21.62-158.00-150.00   52
 18  ω   -106.00  20.00   0.50    1.37    --  -21.62 -57.00-180.00  252
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0313295000
_diffrn_orient_matrix_UB_12      0.0053049000
_diffrn_orient_matrix_UB_13      0.0386315000
_diffrn_orient_matrix_UB_21      -0.0275884000
_diffrn_orient_matrix_UB_22      -0.0483388000
_diffrn_orient_matrix_UB_23      0.0410936000
_diffrn_orient_matrix_UB_31      0.0498783000
_diffrn_orient_matrix_UB_32      -0.0430488000
_diffrn_orient_matrix_UB_33      -0.0074260000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5059
_reflns_number_total             7890
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.541
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         7890
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0416
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0400P)²+0.0424P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.1076
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C15 \\sim C16: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C1A \\sim N1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
C1 \\sim C2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
3. Others
 1*[Sof(Br1)]+1*[Sof(Br1B)]+1*[Sof(Br1A)]=1 with esd of 0.0001
 Sof(H1BD)=Sof(H1BE)=Sof(H1BF)=Sof(C1A)=Sof(H1AD)=Sof(H1AE)=Sof(C2A)=Sof(H2AA)=
 Sof(H2AB)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=
 Sof(H2B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C8(H8A,H8B), C11(H11A,H11B), C12(H12A,H12B), C9(H9A,H9B),
 C14(H14A,H14B), C3(H3A,H3B), C13(H13A,H13B), C7(H7A,H7B), C4(H4A,H4B), C6(H6A,
 H6B), C5(H5A,H5B), C1A(H1AD,H1AE), C1(H1A,H1B), C2(H2A,H2B), C2A(H2AA,H2AB)
4.b Idealised Me refined as rotating group:
 N1(H1BD,H1BE,H1BF), N1(H1AA,H1AB,H1AC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.13363(3) 0.46411(3) 0.88310(3) 0.04162(11) Uani 1 1 d . . . . .
S1 S 0.10023(6) 0.33944(6) 0.81739(6) 0.04619(18) Uani 1 1 d . . . . .
S3 S 0.20773(6) 0.07260(6) 0.86685(6) 0.04869(18) Uani 1 1 d . . . . .
S9 S 0.05420(7) 0.84313(6) 0.92163(6) 0.05016(19) Uani 1 1 d . . . . .
S4 S 0.35682(6) 0.06289(6) 1.02461(6) 0.04873(18) Uani 1 1 d . . . . .
S2 S 0.26470(7) 0.32810(6) 0.98881(6) 0.05094(19) Uani 1 1 d . . . . .
S7 S 0.16008(7) 0.58095(6) 0.95833(6) 0.0524(2) Uani 1 1 d . . . . .
S6 S 0.01161(7) 0.60764(6) 0.77188(6) 0.0547(2) Uani 1 1 d . . . . .
S8 S -0.07961(7) 0.87131(7) 0.74729(7) 0.0614(2) Uani 1 1 d . . . . .
S5 S 0.36379(8) -0.16243(6) 0.98838(7) 0.0645(2) Uani 1 1 d . . . . .
S10 S -0.09525(8) 1.08304(7) 0.80847(8) 0.0707(3) Uani 1 1 d . . . . .
Br1A Br 0.07748(8) 0.14493(10) 0.53963(10) 0.0855(4) Uani 0.543(2) 1 d . . P A
3
O5 O 0.35966(18) 0.39311(18) 0.61872(16) 0.0600(5) Uani 1 1 d . . . . .
O6 O 0.56775(19) 0.22081(18) 0.62494(16) 0.0653(6) Uani 1 1 d . . . . .
O4 O 0.25635(19) 0.5342(2) 0.42170(18) 0.0695(6) Uani 1 1 d . . . . .
O1 O 0.6423(2) 0.1417(2) 0.45691(19) 0.0717(6) Uani 1 1 d . . . . .
N1 N 0.3992(2) 0.2927(2) 0.4597(2) 0.0585(7) Uani 1 1 d . U . . .
H1BD H 0.429447 0.281570 0.400029 0.070 Uiso 0.451(12) 1 calc R U P B 2
H1BE H 0.460506 0.287333 0.496534 0.070 Uiso 0.451(12) 1 calc R U P B 2
H1BF H 0.353770 0.366332 0.442668 0.070 Uiso 0.451(12) 1 calc R U P B 2
H1AA H 0.479294 0.267027 0.453142 0.070 Uiso 0.549(12) 1 calc R U P B 1
H1AB H 0.381007 0.308953 0.518214 0.070 Uiso 0.549(12) 1 calc R U P B 1
H1AC H 0.378360 0.360143 0.402278 0.070 Uiso 0.549(12) 1 calc R U P B 1
O3 O 0.3214(2) 0.4659(2) 0.25332(19) 0.0780(7) Uani 1 1 d . . . . .
O2 O 0.5435(2) 0.3064(3) 0.26362(19) 0.0938(8) Uani 1 1 d . . . . .
C19 C 0.0701(2) 0.7155(2) 0.8904(2) 0.0420(6) Uani 1 1 d . . . . .
C15 C 0.1972(2) 0.2082(2) 0.8852(2) 0.0392(6) Uani 1 1 d . U . . .
C16 C 0.2670(2) 0.2031(2) 0.9597(2) 0.0397(6) Uani 1 1 d . U . . .
C18 C 0.0061(2) 0.7271(2) 0.8095(2) 0.0450(6) Uani 1 1 d . . . . .
C20 C -0.0432(2) 0.9397(2) 0.8250(2) 0.0514(7) Uani 1 1 d . . . . .
C17 C 0.3118(2) -0.0162(2) 0.9613(2) 0.0462(6) Uani 1 1 d . . . . .
C10 C 0.3032(3) 0.5181(3) 0.5884(3) 0.0668(9) Uani 1 1 d . . . . .
H10A H 0.363640 0.571669 0.549851 0.080 Uiso 1 1 calc R U . . .
H10B H 0.270523 0.533490 0.651968 0.080 Uiso 1 1 calc R U . . .
C8 C 0.1761(3) 0.5713(3) 0.3417(3) 0.0760(10) Uani 1 1 d . . . . .
H8A H 0.130094 0.651362 0.332555 0.091 Uiso 1 1 calc R U . . .
H8B H 0.118350 0.514043 0.362728 0.091 Uiso 1 1 calc R U . . .
C11 C 0.4480(3) 0.3599(3) 0.6940(3) 0.0684(9) Uani 1 1 d . . . . .
H11A H 0.409043 0.369624 0.758715 0.082 Uiso 1 1 calc R U . . .
H11B H 0.510684 0.412515 0.664076 0.082 Uiso 1 1 calc R U . . .
C12 C 0.5045(3) 0.2303(3) 0.7198(3) 0.0715(9) Uani 1 1 d . . . . .
H12A H 0.561203 0.204285 0.774811 0.086 Uiso 1 1 calc R U . . .
H12B H 0.441471 0.177989 0.746633 0.086 Uiso 1 1 calc R U . . .
C9 C 0.2027(3) 0.5436(3) 0.5191(3) 0.0736(10) Uani 1 1 d . . . . .
H9A H 0.146240 0.485020 0.554573 0.088 Uiso 1 1 calc R U . . .
H9B H 0.157674 0.625190 0.504765 0.088 Uiso 1 1 calc R U . . .
C14 C 0.7170(3) 0.1164(3) 0.5409(3) 0.0803(11) Uani 1 1 d . . . . .
H14A H 0.765284 0.181702 0.520996 0.096 Uiso 1 1 calc R U . . .
H14B H 0.772889 0.040563 0.552503 0.096 Uiso 1 1 calc R U . . .
C3 C 0.7091(3) 0.1722(4) 0.3549(3) 0.0839(11) Uani 1 1 d . . . . .
H3A H 0.771957 0.103784 0.355797 0.101 Uiso 1 1 calc R U . . .
H3B H 0.749262 0.242032 0.339447 0.101 Uiso 1 1 calc R U . . .
C13 C 0.6386(4) 0.1060(3) 0.6410(3) 0.0850(11) Uani 1 1 d . . . . .
H13A H 0.585592 0.045125 0.658280 0.102 Uiso 1 1 calc R U . . .
H13B H 0.689314 0.080848 0.700121 0.102 Uiso 1 1 calc R U . . .
C7 C 0.2449(3) 0.5769(3) 0.2401(3) 0.0717(9) Uani 1 1 d . . . . .
H7A H 0.187877 0.595051 0.186948 0.086 Uiso 1 1 calc R U . . .
H7B H 0.294007 0.642399 0.214130 0.086 Uiso 1 1 calc R U . . .
C4 C 0.6289(4) 0.2008(4) 0.2725(3) 0.0925(13) Uani 1 1 d . . . . .
H4A H 0.676868 0.214208 0.204489 0.111 Uiso 1 1 calc R U . . .
H4B H 0.585801 0.132420 0.289591 0.111 Uiso 1 1 calc R U . . .
C6 C 0.4015(4) 0.4708(4) 0.1618(3) 0.0970(14) Uani 1 1 d . . . . .
H6A H 0.456743 0.528840 0.147834 0.116 Uiso 1 1 calc R U . . .
H6B H 0.354072 0.499520 0.100113 0.116 Uiso 1 1 calc R U . . .
C5 C 0.4724(4) 0.3521(5) 0.1761(3) 0.1263(19) Uani 1 1 d . . . . .
H5A H 0.417292 0.295037 0.186743 0.152 Uiso 1 1 calc R U . . .
H5B H 0.525626 0.358907 0.111649 0.152 Uiso 1 1 calc R U . . .
C1A C 0.3187(17) 0.1931(17) 0.5290(15) 0.105(5) Uani 0.451(12) 1 d . U P B 2
H1AD H 0.319781 0.146470 0.486037 0.126 Uiso 0.451(12) 1 calc R U P B 2
H1AE H 0.367088 0.139453 0.588620 0.126 Uiso 0.451(12) 1 calc R U P B 2
C1 C 0.3323(16) 0.1984(14) 0.4685(16) 0.139(5) Uani 0.549(12) 1 d . U P B 1
H1A H 0.374750 0.161909 0.419350 0.167 Uiso 0.549(12) 1 calc R U P B 1
H1B H 0.339654 0.135306 0.540324 0.167 Uiso 0.549(12) 1 calc R U P B 1
Br1B Br 0.10474(18) 0.2291(2) 0.4750(2) 0.0805(10) Uani 0.228(2) 1 d . . P B 2
Br1 Br 0.1213(3) 0.2047(4) 0.5677(3) 0.1306(17) Uani 0.229(2) 1 d . . P B 1
C2 C 0.2113(9) 0.2256(9) 0.4504(9) 0.133(5) Uani 0.549(12) 1 d . U P B 1
H2A H 0.192819 0.173391 0.418748 0.159 Uiso 0.549(12) 1 calc R U P B 1
H2B H 0.193251 0.309952 0.400099 0.159 Uiso 0.549(12) 1 calc R U P B 1
C2A C 0.2158(13) 0.1991(15) 0.5687(14) 0.141(7) Uani 0.451(12) 1 d . . P B 2
H2AA H 0.200126 0.263692 0.595203 0.169 Uiso 0.451(12) 1 calc R U P B 2
H2AB H 0.206386 0.122505 0.629325 0.169 Uiso 0.451(12) 1 calc R U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S1 2.1700(8) . ?
Ni1 S2 2.1621(7) . ?
Ni1 S7 2.1553(8) . ?
Ni1 S6 2.1701(7) . ?
S1 C15 1.722(2) . ?
S3 C15 1.745(2) . ?
S3 C17 1.732(3) . ?
S9 C19 1.741(3) . ?
S9 C20 1.722(3) . ?
S4 C16 1.740(2) . ?
S4 C17 1.719(3) . ?
S2 C16 1.717(3) . ?
S7 C19 1.708(2) . ?
S6 C18 1.718(3) . ?
S8 C18 1.746(2) . ?
S8 C20 1.731(3) . ?
S5 C17 1.652(2) . ?
S10 C20 1.651(3) . ?
O5 C10 1.430(3) . ?
O5 C11 1.420(4) . ?
O6 C12 1.421(4) . ?
O6 C13 1.404(4) . ?
O4 C8 1.394(4) . ?
O4 C9 1.419(4) . ?
O1 C14 1.423(4) . ?
O1 C3 1.421(4) . ?
N1 H1BD 0.8900 . ?
N1 H1BE 0.8900 . ?
N1 H1BF 0.8900 . ?
N1 H1AA 0.8900 . ?
N1 H1AB 0.8900 . ?
N1 H1AC 0.8900 . ?
N1 C1A 1.547(19) . ?
N1 C1 1.444(15) . ?
O3 C7 1.401(4) . ?
O3 C6 1.413(4) . ?
O2 C4 1.408(4) . ?
O2 C5 1.396(4) . ?
C19 C18 1.357(4) . ?
C15 C16 1.354(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C9 1.486(5) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C7 1.469(5) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.485(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C13 1.484(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.438(5) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C5 1.448(5) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C1A H1AD 0.9700 . ?
C1A H1AE 0.9700 . ?
C1A C2A 1.20(2) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.362(19) . ?
Br1B C2A 1.803(16) . ?
Br1 C2 1.714(13) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S1 Ni1 S6 88.54(3) . . ?
S2 Ni1 S1 93.19(3) . . ?
S2 Ni1 S6 176.27(3) . . ?
S7 Ni1 S1 176.11(3) . . ?
S7 Ni1 S2 85.60(3) . . ?
S7 Ni1 S6 92.89(3) . . ?
C15 S1 Ni1 101.78(9) . . ?
C17 S3 C15 97.21(12) . . ?
C20 S9 C19 97.22(13) . . ?
C17 S4 C16 97.45(12) . . ?
C16 S2 Ni1 102.17(9) . . ?
C19 S7 Ni1 102.77(10) . . ?
C18 S6 Ni1 101.79(9) . . ?
C20 S8 C18 97.68(13) . . ?
C11 O5 C10 111.9(2) . . ?
C13 O6 C12 114.3(2) . . ?
C8 O4 C9 115.2(2) . . ?
C3 O1 C14 112.8(3) . . ?
H1BD N1 H1BE 109.5 . . ?
H1BD N1 H1BF 109.5 . . ?
H1BE N1 H1BF 109.5 . . ?
H1AA N1 H1AB 109.5 . . ?
H1AA N1 H1AC 109.5 . . ?
H1AB N1 H1AC 109.5 . . ?
C1A N1 H1BD 109.5 . . ?
C1A N1 H1BE 109.5 . . ?
C1A N1 H1BF 109.5 . . ?
C1 N1 H1AA 109.5 . . ?
C1 N1 H1AB 109.5 . . ?
C1 N1 H1AC 109.5 . . ?
C7 O3 C6 113.5(3) . . ?
C5 O2 C4 114.9(3) . . ?
S7 C19 S9 122.24(16) . . ?
C18 C19 S9 116.83(18) . . ?
C18 C19 S7 120.92(19) . . ?
S1 C15 S3 122.72(16) . . ?
C16 C15 S1 121.46(19) . . ?
C16 C15 S3 115.77(18) . . ?
S2 C16 S4 122.37(16) . . ?
C15 C16 S4 116.24(19) . . ?
C15 C16 S2 121.38(18) . . ?
S6 C18 S8 123.32(17) . . ?
C19 C18 S6 121.62(18) . . ?
C19 C18 S8 115.1(2) . . ?
S9 C20 S8 113.19(14) . . ?
S10 C20 S9 122.90(19) . . ?
S10 C20 S8 123.90(18) . . ?
S4 C17 S3 113.31(14) . . ?
S5 C17 S3 123.80(17) . . ?
S5 C17 S4 122.88(17) . . ?
O5 C10 H10A 109.8 . . ?
O5 C10 H10B 109.8 . . ?
O5 C10 C9 109.4(3) . . ?
H10A C10 H10B 108.2 . . ?
C9 C10 H10A 109.8 . . ?
C9 C10 H10B 109.8 . . ?
O4 C8 H8A 109.6 . . ?
O4 C8 H8B 109.6 . . ?
O4 C8 C7 110.2(3) . . ?
H8A C8 H8B 108.1 . . ?
C7 C8 H8A 109.6 . . ?
C7 C8 H8B 109.6 . . ?
O5 C11 H11A 109.9 . . ?
O5 C11 H11B 109.9 . . ?
O5 C11 C12 108.8(3) . . ?
H11A C11 H11B 108.3 . . ?
C12 C11 H11A 109.9 . . ?
C12 C11 H11B 109.9 . . ?
O6 C12 C11 108.5(3) . . ?
O6 C12 H12A 110.0 . . ?
O6 C12 H12B 110.0 . . ?
C11 C12 H12A 110.0 . . ?
C11 C12 H12B 110.0 . . ?
H12A C12 H12B 108.4 . . ?
O4 C9 C10 107.9(3) . . ?
O4 C9 H9A 110.1 . . ?
O4 C9 H9B 110.1 . . ?
C10 C9 H9A 110.1 . . ?
C10 C9 H9B 110.1 . . ?
H9A C9 H9B 108.4 . . ?
O1 C14 H14A 109.7 . . ?
O1 C14 H14B 109.7 . . ?
O1 C14 C13 109.8(3) . . ?
H14A C14 H14B 108.2 . . ?
C13 C14 H14A 109.7 . . ?
C13 C14 H14B 109.7 . . ?
O1 C3 H3A 109.5 . . ?
O1 C3 H3B 109.5 . . ?
O1 C3 C4 110.7(3) . . ?
H3A C3 H3B 108.1 . . ?
C4 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
O6 C13 C14 108.3(3) . . ?
O6 C13 H13A 110.0 . . ?
O6 C13 H13B 110.0 . . ?
C14 C13 H13A 110.0 . . ?
C14 C13 H13B 110.0 . . ?
H13A C13 H13B 108.4 . . ?
O3 C7 C8 111.0(3) . . ?
O3 C7 H7A 109.4 . . ?
O3 C7 H7B 109.4 . . ?
C8 C7 H7A 109.4 . . ?
C8 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
O2 C4 C3 110.4(3) . . ?
O2 C4 H4A 109.6 . . ?
O2 C4 H4B 109.6 . . ?
C3 C4 H4A 109.6 . . ?
C3 C4 H4B 109.6 . . ?
H4A C4 H4B 108.1 . . ?
O3 C6 H6A 109.3 . . ?
O3 C6 H6B 109.3 . . ?
O3 C6 C5 111.6(3) . . ?
H6A C6 H6B 108.0 . . ?
C5 C6 H6A 109.3 . . ?
C5 C6 H6B 109.3 . . ?
O2 C5 C6 111.9(4) . . ?
O2 C5 H5A 109.2 . . ?
O2 C5 H5B 109.2 . . ?
C6 C5 H5A 109.2 . . ?
C6 C5 H5B 109.2 . . ?
H5A C5 H5B 107.9 . . ?
N1 C1A H1AD 104.2 . . ?
N1 C1A H1AE 104.2 . . ?
H1AD C1A H1AE 105.5 . . ?
C2A C1A N1 132.2(16) . . ?
C2A C1A H1AD 104.2 . . ?
C2A C1A H1AE 104.2 . . ?
N1 C1 H1A 107.2 . . ?
N1 C1 H1B 107.2 . . ?
H1A C1 H1B 106.8 . . ?
C2 C1 N1 120.6(13) . . ?
C2 C1 H1A 107.2 . . ?
C2 C1 H1B 107.2 . . ?
C1 C2 Br1 110.7(10) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
Br1 C2 H2A 109.5 . . ?
Br1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
C1A C2A Br1B 112.2(12) . . ?
C1A C2A H2AA 109.2 . . ?
C1A C2A H2AB 109.2 . . ?
Br1B C2A H2AA 109.2 . . ?
Br1B C2A H2AB 109.2 . . ?
H2AA C2A H2AB 107.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S1 C15 S3 178.67(13) . . . . ?
Ni1 S1 C15 C16 1.3(2) . . . . ?
Ni1 S2 C16 S4 -178.75(13) . . . . ?
Ni1 S2 C16 C15 0.4(2) . . . . ?
Ni1 S7 C19 S9 178.36(14) . . . . ?
Ni1 S7 C19 C18 -0.9(2) . . . . ?
Ni1 S6 C18 S8 179.85(15) . . . . ?
Ni1 S6 C18 C19 0.5(3) . . . . ?
S1 C15 C16 S4 178.02(13) . . . . ?
S1 C15 C16 S2 -1.2(3) . . . . ?
S3 C15 C16 S4 0.4(3) . . . . ?
S3 C15 C16 S2 -178.79(14) . . . . ?
S9 C19 C18 S6 -179.01(15) . . . . ?
S9 C19 C18 S8 1.6(3) . . . . ?
S7 C19 C18 S6 0.3(3) . . . . ?
S7 C19 C18 S8 -179.12(14) . . . . ?
O5 C10 C9 O4 -66.3(3) . . . . ?
O5 C11 C12 O6 63.5(3) . . . . ?
O4 C8 C7 O3 53.6(4) . . . . ?
O1 C14 C13 O6 -65.3(4) . . . . ?
O1 C3 C4 O2 64.3(4) . . . . ?
N1 C1A C2A Br1B 82.8(17) . . . . ?
N1 C1 C2 Br1 -92.3(15) . . . . ?
O3 C6 C5 O2 -59.4(6) . . . . ?
C19 S9 C20 S8 0.50(18) . . . . ?
C19 S9 C20 S10 -179.15(19) . . . . ?
C15 S3 C17 S4 -0.91(17) . . . . ?
C15 S3 C17 S5 179.29(18) . . . . ?
C16 S4 C17 S3 1.09(17) . . . . ?
C16 S4 C17 S5 -179.11(18) . . . . ?
C18 S8 C20 S9 0.17(18) . . . . ?
C18 S8 C20 S10 179.82(19) . . . . ?
C20 S9 C19 S7 179.44(17) . . . . ?
C20 S9 C19 C18 -1.3(2) . . . . ?
C20 S8 C18 S6 179.55(18) . . . . ?
C20 S8 C18 C19 -1.0(2) . . . . ?
C17 S3 C15 S1 -177.26(17) . . . . ?
C17 S3 C15 C16 0.3(2) . . . . ?
C17 S4 C16 S2 178.28(17) . . . . ?
C17 S4 C16 C15 -0.9(2) . . . . ?
C10 O5 C11 C12 -178.8(3) . . . . ?
C8 O4 C9 C10 -171.9(3) . . . . ?
C11 O5 C10 C9 -173.9(2) . . . . ?
C12 O6 C13 C14 -169.3(3) . . . . ?
C9 O4 C8 C7 170.6(3) . . . . ?
C14 O1 C3 C4 -178.1(3) . . . . ?
C3 O1 C14 C13 170.6(3) . . . . ?
C13 O6 C12 C11 172.2(3) . . . . ?
C7 O3 C6 C5 -175.8(3) . . . . ?
C4 O2 C5 C6 -170.6(4) . . . . ?
C6 O3 C7 C8 -172.2(3) . . . . ?
C5 O2 C4 C3 171.5(4) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.756
_oxdiff_exptl_absorpt_empirical_full_min 0.400
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_253k-f
_database_code_depnum_ccdc_archive 'CCDC 2053399'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-18 downloaded from the CCDC.
;
_audit_creation_date             2020-12-31
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C2 H7 Cl N, C12 H24 O6'
_chemical_formula_sum            'C20 H31 Cl N Ni O6 S10'
_chemical_formula_weight         796.22
_chemical_melting_point          ?
_chemical_oxdiff_formula         C20H31NO6NiS10Cl
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.27840(10)
_cell_length_b                   12.34600(10)
_cell_length_c                   12.86190(10)
_cell_angle_alpha                91.1450(10)
_cell_angle_beta                 110.6780(10)
_cell_angle_gamma                96.4220(10)
_cell_volume                     1661.63(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    27000
_cell_measurement_temperature    253
_cell_measurement_theta_max      72.0620
_cell_measurement_theta_min      3.5940
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    7.765
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54517
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             822
_exptl_crystal_size_max          0.291
_exptl_crystal_size_mid          0.249
_exptl_crystal_size_min          0.153
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            41385
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.249
_diffrn_reflns_theta_min         3.610
_diffrn_ambient_temperature      253
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     16.00  94.00   0.50    0.50    --    5.00  46.00-150.00  156
  2  ω    -83.00  12.00   0.50    0.50    --    5.00  46.00-150.00  190
  3  ω      3.00  50.00   0.50    0.50    --  -38.00  55.00  55.27   94
  4  ω    -54.00 -28.00   0.50    0.50    --  -38.00  55.00  55.27   52
  5  ω   -101.00 -24.00   0.50    0.50    --  -42.00  53.00 -87.93  154
  6  ω   -128.00 -63.00   0.50    0.50    --  -42.00  55.00-162.12  130
  7  ω     -5.00  46.00   0.50    0.50    --  -42.00  55.00-162.12  102
  8  ω     17.00  46.00   0.50    0.50    --  -42.00  53.00 -87.93   58
  9  ω    -75.00 -38.00   0.50    0.50    --  -50.00  54.00 146.87   74
 10  ω      3.00  38.00   0.50    0.50    --  -50.00  54.00 146.87   70
 11  ω     -4.00  38.00   0.50    0.50    --  -50.00  55.00  32.87   84
 12  ω      2.00  31.00   0.50    0.50    --  -58.00  55.00 -86.41   58
 13  ω     -2.00  31.00   0.50    0.50    --  -58.00  55.00 -12.31   66
 14  ω    -14.00  31.00   0.50    0.50    --  -58.00  55.00-125.47   90
 15  ω      5.00  31.00   0.50    0.50    --  -58.00  55.00 108.94   52
 16  ω      1.00  27.00   0.50    0.50    --  -62.00  54.00-151.82   52
 17  ω      2.00  27.00   0.50    0.50    --  -62.00  55.00  24.85   50
 18  ω    -16.00  23.00   0.50    0.50    --  -66.00  55.00  50.44   78
 19  ω     -4.00  22.00   0.50    0.50    --  -66.00  55.00 170.19   52
 20  ω     -2.00  23.00   0.50    0.50    --  -66.00  55.00  98.10   50
 21  ω    -10.00  23.00   0.50    0.50    --  -66.00  55.00 -23.04   66
 22  ω     -9.00  17.00   0.50    0.50    --  -70.00  55.00  68.85   52
 23  ω     -6.00  19.00   0.50    0.50    --  -70.00  55.00 -44.51   50
 24  ω    -14.00  17.00   0.50    0.50    --  -70.00  55.00-151.04   62
 25  ω    -24.00  19.00   0.50    0.50    --  -70.00  53.00 149.79   86
 26  ω    -13.00  13.00   0.50    0.50    --  -74.00  53.00 -61.99   52
 27  ω    -24.00  11.00   0.50    0.50    --  -78.00  55.00-166.49   70
 28  ω    -15.00  11.00   0.50    0.50    --  -78.00  53.00-123.26   52
 29  ω    -15.00  11.00   0.50    0.50    --  -78.00  52.00 -78.58   52
 30  ω    -23.00  11.00   0.50    0.50    --  -78.00  55.00  13.36   68
 31  ω    -78.00 -33.00   0.50    0.50    --  -86.00  55.00 116.24   90
 32  ω   -135.00   3.00   0.50    0.50    --  -86.00  53.00 151.54  276
 33  ω   -147.00-116.00   0.50    0.50    --  -86.00  55.00 116.24   62
 34  ω    -25.00   3.00   0.50    0.50    --  -86.00  54.00 -88.05   56
 35  ω    -22.00   3.00   0.50    0.50    --  -86.00  55.00 116.24   50
 36  ω    -24.00   1.00   0.50    0.50    --  -86.00  53.00 130.23   50
 37  ω    -51.00  -3.00   0.50    0.50    --  -90.00  54.00  81.26   96
 38  ω   -126.00  -6.00   0.50    0.50    --  -90.00  53.00 -42.65  240
 39  ω    -43.00  -2.00   0.50    0.50    --  -90.00  55.00 174.96   82
 40  ω   -162.00-136.00   0.50    0.50    --  -90.00  55.00 174.96   52
 41  ω    -32.00  -3.00   0.50    0.50    --  -90.00  51.00-131.58   58
 42  ω    -40.00  -8.00   0.50    0.50    --  -94.00  53.00 123.38   64
 43  ω   -137.00 -69.00   0.50    0.50    --  -94.00  53.00 123.38  136
 44  ω    -36.00 -11.00   0.50    0.50    --  -95.40  55.00 -96.49   50
 45  ω   -126.00 -48.00   0.50    0.50    --  -95.40  55.00 -96.49  156
 46  ω   -182.00  -7.00   0.50    0.50    --  -95.40  55.00 -58.37  350
 47  ω   -175.00-149.00   0.50    0.50    --  -95.40  55.00 -96.49   52
 48  ω   -134.00 -37.00   0.50    0.50    --  -95.40  53.00 163.19  194
 49  ω   -132.00  -6.00   0.50    0.50    --  -95.40  55.00  -2.05  252
 50  ω   -176.00-139.00   0.50    0.50    --  -95.40  55.00  -2.05   74
 51  ω    -42.00  -6.00   0.50    0.50    --  -95.40  53.00 -25.68   72
 52  ω   -184.00 -66.00   0.50    0.50    --  -95.40  55.00-150.52  236
 53  ω   -183.00  -7.00   0.50    0.50    --  -95.40  55.00  66.98  352
 54  ω   -160.00  -7.00   0.50    0.50    --  -95.40  55.00-109.45  306
 55  ω    -32.00  -6.00   0.50    0.50    --  -95.40  51.00  21.35   52
 56  ω   -105.00  -6.00   0.50    0.50    --  -95.40  54.00-140.30  198
 57  ω    -38.00  -6.00   0.50    0.50    --  -95.40  55.00   8.88   64
 58  ω   -119.00 -45.00   0.50    0.50    --  -95.40  55.00   8.88  148
 59  ω   -126.00  -6.00   0.50    0.50    --  -95.40  55.00 109.14  240
 60  ω   -175.00-140.00   0.50    0.50    --  -95.40  55.00 109.14   70
 61  ω   -137.00  -6.00   0.50    0.50    --  -95.40  54.00  51.05  262
 62  ω    -59.00 -10.00   0.50    0.50    --  -95.40  55.00-150.52   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0848917000
_diffrn_orient_matrix_UB_12      -0.0642460000
_diffrn_orient_matrix_UB_13      -0.0427911000
_diffrn_orient_matrix_UB_21      0.0999032000
_diffrn_orient_matrix_UB_22      0.0057883000
_diffrn_orient_matrix_UB_23      0.1188742000
_diffrn_orient_matrix_UB_31      -0.0669238000
_diffrn_orient_matrix_UB_32      -0.1080356000
_diffrn_orient_matrix_UB_33      0.0222566000
_diffrn_oxdiff_digest_frames     
;
01abefbb46bbf6e9ace5a09866b9b78568000277976
;
_diffrn_oxdiff_digest_hkl        
;
013c9f9f66ccb089a6bf2cad9ff9bffe7760de
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5825
_reflns_number_total             6340
_reflns_odcompleteness_completeness 98.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       0.00309(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         6340
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0271
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0421P)²+0.3530P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0763
_refine_ls_wR_factor_ref         0.0776
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
2. Others
 Sof(H20c)=Sof(H20d)=Sof(C19A)=Sof(H19c)=Sof(H19d)=Sof(Cl)=1-FVAR(1)
 Sof(Cl18)=Sof(H20a)=Sof(H20b)=Sof(C19)=Sof(H19a)=Sof(H19b)=FVAR(1)
 Sof(O1A)=Sof(O23A)=Sof(C22A)=Sof(H22c)=Sof(H22d)=Sof(C27A)=Sof(H27c)=
 Sof(H27d)=Sof(C24A)=Sof(H24c)=Sof(H24d)=Sof(C26A)=Sof(H26c)=Sof(H26d)=Sof(C8A)=
 Sof(H8Aa)=Sof(H8Ab)=Sof(O6A)=Sof(C32A)=Sof(H32c)=Sof(H32d)=Sof(C40A)=Sof(H40c)=
 Sof(H40d)=Sof(O28A)=Sof(C4A)=Sof(H4Aa)=Sof(H4Ab)=Sof(C31A)=Sof(H31c)=Sof(H31d)=
 Sof(O2A)=Sof(C30A)=Sof(H30c)=Sof(H30d)=Sof(C37A)=Sof(H37c)=Sof(H37d)=Sof(O3A)=
 Sof(C1A)=Sof(H1Aa)=Sof(H1Ab)=1-FVAR(2)
 Sof(O23)=Sof(C30)=Sof(H30a)=Sof(H30b)=Sof(C32)=Sof(H32a)=Sof(H32b)=Sof(C22)=
 Sof(H22a)=Sof(H22b)=Sof(C37)=Sof(H37a)=Sof(H37b)=Sof(O28)=Sof(C27)=Sof(H27a)=
 Sof(H27b)=Sof(C40)=Sof(H40a)=Sof(H40b)=Sof(C24)=Sof(H24a)=Sof(H24b)=Sof(C31)=
 Sof(H31a)=Sof(H31b)=Sof(C26)=Sof(H26a)=Sof(H26b)=Sof(O1)=Sof(O2)=Sof(O3)=
 Sof(O6)=Sof(C8)=Sof(H8a)=Sof(H8b)=Sof(C4)=Sof(H4a)=Sof(H4b)=Sof(C1)=Sof(H1a)=
 Sof(H1b)=FVAR(2)
3.a Secondary CH2 refined with riding coordinates:
 C20(H20a,H20b), C20(H20c,H20d), C30(H30a,H30b), C32(H32a,H32b), C22(H22a,
 H22b), C37(H37a,H37b), C19(H19a,H19b), C27(H27a,H27b), C40(H40a,H40b),
 C24(H24a,H24b), C31(H31a,H31b), C26(H26a,H26b), C19A(H19c,H19d), C8(H8a,H8b),
 C4(H4a,H4b), C1(H1a,H1b), C22A(H22c,H22d), C27A(H27c,H27d), C24A(H24c,H24d),
 C26A(H26c,H26d), C8A(H8Aa,H8Ab), C32A(H32c,H32d), C40A(H40c,H40d), C4A(H4Aa,
 H4Ab), C31A(H31c,H31d), C30A(H30c,H30d), C37A(H37c,H37d), C1A(H1Aa,H1Ab)
3.b Idealised Me refined as rotating group:
 N21(H21a,H21b,H21c)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.34531(2) 0.88974(2) 0.51228(2) 0.04381(9) Uani 1 1 d . . . . .
S6 S 0.11402(4) 1.02583(4) 0.72071(4) 0.05329(11) Uani 1 1 d . . . . .
S9 S 0.39889(4) 0.84437(4) 0.68249(3) 0.05532(12) Uani 1 1 d . . . . .
S7 S 0.19215(4) 0.97559(4) 0.52322(3) 0.05375(11) Uani 1 1 d . . . . .
S16 S 0.50566(4) 0.81211(4) 0.50707(3) 0.05401(11) Uani 1 1 d . . . . .
S15 S 0.29048(4) 0.92928(4) 0.34008(3) 0.05440(12) Uani 1 1 d . . . . .
S4 S 0.30193(5) 0.90246(4) 0.86549(3) 0.05774(12) Uani 1 1 d . . . . .
S13 S 0.59933(4) 0.77126(4) 0.31784(4) 0.05919(12) Uani 1 1 d . . . . .
S11 S 0.40780(5) 0.88640(4) 0.16631(4) 0.05900(12) Uani 1 1 d . . . . .
S8 S 0.12628(5) 1.00306(4) 0.95396(4) 0.06677(14) Uani 1 1 d . . . . .
S17 S 0.58959(5) 0.78595(5) 0.08512(4) 0.07288(15) Uani 1 1 d . . . . .
Cl18 Cl 0.6638(3) 0.5466(3) 0.4877(2) 0.0939(8) Uani 0.674(5) 1 d . . P A 1
N21 N 0.83464(14) 0.49799(11) 0.74438(11) 0.0520(3) Uani 1 1 d . . . . .
H21A H 0.813444 0.564761 0.729307 0.062 Uiso 1 1 calc GR . . . .
H21B H 0.910605 0.493517 0.739207 0.062 Uiso 1 1 calc GR . . . .
H21C H 0.838265 0.484527 0.813082 0.062 Uiso 1 1 calc GR . . . .
C3 C 0.29763(15) 0.90787(13) 0.72925(13) 0.0461(3) Uani 1 1 d . . . . .
C2 C 0.20872(15) 0.96527(12) 0.66049(13) 0.0447(3) Uani 1 1 d . . . . .
C12 C 0.53498(17) 0.81304(15) 0.18454(14) 0.0550(4) Uani 1 1 d . . . . .
C10 C 0.40316(15) 0.87699(13) 0.29981(13) 0.0470(3) Uani 1 1 d . . . . .
C5 C 0.17822(16) 0.97869(14) 0.85216(14) 0.0510(4) Uani 1 1 d . . . . .
C14 C 0.49509(15) 0.82464(13) 0.37193(13) 0.0470(3) Uani 1 1 d . . . . .
O23 O 0.8534(5) 0.3446(4) 0.9113(3) 0.0679(10) Uani 0.457(4) 1 d . . P B 1
C20 C 0.7373(2) 0.41652(17) 0.66353(17) 0.0717(5) Uani 1 1 d . . . . .
H20A H 0.653855 0.425247 0.665970 0.086 Uiso 0.674(5) 1 calc R . P A 1
H20B H 0.755540 0.343701 0.685477 0.086 Uiso 0.674(5) 1 calc R . P A 1
H20C H 0.776916 0.377522 0.621032 0.086 Uiso 0.326(5) 1 calc R . P A 2
H20D H 0.701954 0.363882 0.703247 0.086 Uiso 0.326(5) 1 calc R . P A 2
C30 C 0.8528(15) 0.7867(9) 0.6816(11) 0.070(4) Uani 0.457(4) 1 d . . P B 1
H30A H 0.783556 0.762611 0.612113 0.084 Uiso 0.457(4) 1 calc R . P B 1
H30B H 0.893082 0.857633 0.672265 0.084 Uiso 0.457(4) 1 calc R . P B 1
C32 C 0.6795(7) 0.7022(6) 0.8643(6) 0.0726(17) Uani 0.457(4) 1 d . . P B 1
H32A H 0.613251 0.749857 0.842158 0.087 Uiso 0.457(4) 1 calc R . P B 1
H32B H 0.743806 0.732063 0.934458 0.087 Uiso 0.457(4) 1 calc R . P B 1
C22 C 0.6876(10) 0.4220(11) 0.9491(9) 0.080(3) Uani 0.457(4) 1 d . . P B 1
H22A H 0.625539 0.379977 0.884450 0.096 Uiso 0.457(4) 1 calc R . P B 1
H22B H 0.648542 0.429764 1.004535 0.096 Uiso 0.457(4) 1 calc R . P B 1
C37 C 1.1002(13) 0.6334(14) 0.6578(12) 0.085(4) Uani 0.457(4) 1 d . . P B 1
H37A H 1.141721 0.633836 0.603356 0.102 Uiso 0.457(4) 1 calc R . P B 1
H37B H 1.163564 0.661189 0.729193 0.102 Uiso 0.457(4) 1 calc R . P B 1
C19 C 0.7334(4) 0.4272(3) 0.5472(3) 0.0772(11) Uani 0.674(5) 1 d . . P A 1
H19A H 0.684017 0.362575 0.501662 0.093 Uiso 0.674(5) 1 calc R . P A 1
H19B H 0.819621 0.431358 0.546748 0.093 Uiso 0.674(5) 1 calc R . P A 1
O28 O 0.7354(4) 0.6955(3) 0.7818(3) 0.0643(10) Uani 0.457(4) 1 d . . P B 1
C27 C 0.9661(12) 0.2947(8) 0.9538(7) 0.081(3) Uani 0.457(4) 1 d . . P B 1
H27A H 0.949655 0.228438 0.988469 0.097 Uiso 0.457(4) 1 calc R . P B 1
H27B H 1.031946 0.343763 1.009790 0.097 Uiso 0.457(4) 1 calc R . P B 1
C40 C 1.1491(7) 0.3964(8) 0.7632(10) 0.089(2) Uani 0.457(4) 1 d . . P B 1
H40A H 1.228298 0.418322 0.825144 0.107 Uiso 0.457(4) 1 calc R . P B 1
H40B H 1.159519 0.328668 0.729743 0.107 Uiso 0.457(4) 1 calc R . P B 1
C24 C 0.8049(8) 0.3635(5) 0.9960(6) 0.0856(18) Uani 0.457(4) 1 d . . P B 1
H24A H 0.869290 0.407935 1.057464 0.103 Uiso 0.457(4) 1 calc R . P B 1
H24B H 0.782387 0.294684 1.023629 0.103 Uiso 0.457(4) 1 calc R . P B 1
C31 C 0.7998(6) 0.7966(4) 0.7735(5) 0.0761(16) Uani 0.457(4) 1 d . . P B 1
H31A H 0.868874 0.819123 0.843507 0.091 Uiso 0.457(4) 1 calc R . P B 1
H31B H 0.741564 0.851427 0.757254 0.091 Uiso 0.457(4) 1 calc R . P B 1
C26 C 1.0095(7) 0.2684(5) 0.8612(5) 0.0806(16) Uani 0.457(4) 1 d . . P B 1
H26A H 1.083229 0.229067 0.888414 0.097 Uiso 0.457(4) 1 calc R . P B 1
H26B H 0.942013 0.222081 0.803811 0.097 Uiso 0.457(4) 1 calc R . P B 1
C19A C 0.6381(6) 0.4694(6) 0.5903(5) 0.070(2) Uani 0.326(5) 1 d . . P A 2
H19C H 0.618666 0.527042 0.631783 0.084 Uiso 0.326(5) 1 calc R . P A 2
H19D H 0.561690 0.417306 0.558452 0.084 Uiso 0.326(5) 1 calc R . P A 2
Cl Cl 0.6825(8) 0.5255(7) 0.4827(5) 0.107(2) Uani 0.326(5) 1 d . . P A 2
O1 O 0.7250(4) 0.5252(4) 0.9190(3) 0.0678(10) Uani 0.457(4) 1 d . . P B 1
O2 O 1.0483(4) 0.5264(4) 0.6657(3) 0.0751(11) Uani 0.457(4) 1 d . . P B 1
O3 O 0.9402(4) 0.7139(3) 0.7056(3) 0.0670(10) Uani 0.457(4) 1 d . . P B 1
O6 O 1.0423(4) 0.3664(4) 0.8160(4) 0.0665(10) Uani 0.457(4) 1 d . . P B 1
C8 C 0.6235(6) 0.5900(6) 0.8777(5) 0.0840(19) Uani 0.457(4) 1 d . . P B 1
H8A H 0.578615 0.593327 0.929324 0.101 Uiso 0.457(4) 1 calc R . P B 1
H8B H 0.563214 0.558075 0.806525 0.101 Uiso 0.457(4) 1 calc R . P B 1
C4 C 1.1434(8) 0.4560(8) 0.7032(6) 0.090(2) Uani 0.457(4) 1 d . . P B 1
H4A H 1.142427 0.416520 0.636845 0.108 Uiso 0.457(4) 1 calc R . P B 1
H4B H 1.224220 0.503158 0.731253 0.108 Uiso 0.457(4) 1 calc R . P B 1
C1 C 0.9945(7) 0.7047(5) 0.6233(7) 0.0815(19) Uani 0.457(4) 1 d . . P B 1
H1A H 1.028338 0.776798 0.610138 0.098 Uiso 0.457(4) 1 calc R . P B 1
H1B H 0.928955 0.673892 0.554193 0.098 Uiso 0.457(4) 1 calc R . P B 1
O1A O 0.7102(4) 0.5842(3) 0.8837(3) 0.0673(8) Uani 0.543(4) 1 d . . P B 2
O23A O 0.7957(4) 0.3803(3) 0.9205(3) 0.0657(8) Uani 0.543(4) 1 d . . P B 2
C22A C 0.6410(6) 0.4963(5) 0.9166(4) 0.0814(13) Uani 0.543(4) 1 d . . P B 2
H22C H 0.580396 0.453947 0.851459 0.098 Uiso 0.543(4) 1 calc R . P B 2
H22D H 0.594245 0.524349 0.959457 0.098 Uiso 0.543(4) 1 calc R . P B 2
C27A C 0.8953(6) 0.3208(4) 0.9830(5) 0.0800(14) Uani 0.543(4) 1 d . . P B 2
H27C H 0.862305 0.265998 1.022259 0.096 Uiso 0.543(4) 1 calc R . P B 2
H27D H 0.962462 0.369888 1.037658 0.096 Uiso 0.543(4) 1 calc R . P B 2
C24A C 0.7370(9) 0.4250(10) 0.9870(7) 0.079(2) Uani 0.543(4) 1 d . . P B 2
H24C H 0.800535 0.468451 1.049771 0.095 Uiso 0.543(4) 1 calc R . P B 2
H24D H 0.693728 0.367162 1.015550 0.095 Uiso 0.543(4) 1 calc R . P B 2
C26A C 0.9479(9) 0.2672(6) 0.9081(7) 0.077(2) Uani 0.543(4) 1 d . . P B 2
H26C H 1.009625 0.220672 0.949886 0.092 Uiso 0.543(4) 1 calc R . P B 2
H26D H 0.879749 0.221969 0.850137 0.092 Uiso 0.543(4) 1 calc R . P B 2
C8A C 0.6336(5) 0.6619(5) 0.8253(5) 0.0674(13) Uani 0.543(4) 1 d . . P B 2
H8AA H 0.585645 0.687815 0.868174 0.081 Uiso 0.543(4) 1 calc R . P B 2
H8AB H 0.573445 0.629071 0.754514 0.081 Uiso 0.543(4) 1 calc R . P B 2
O6A O 1.0079(3) 0.3482(3) 0.8593(4) 0.0691(9) Uani 0.543(4) 1 d . . P B 2
C32A C 0.7182(4) 0.7541(4) 0.8066(4) 0.0666(12) Uani 0.543(4) 1 d . . P B 2
H32C H 0.668437 0.812136 0.773657 0.080 Uiso 0.543(4) 1 calc R . P B 2
H32D H 0.782485 0.782958 0.877160 0.080 Uiso 0.543(4) 1 calc R . P B 2
C40A C 1.0616(5) 0.3034(5) 0.7868(6) 0.0872(17) Uani 0.543(4) 1 d . . P B 2
H40C H 1.136257 0.272202 0.833283 0.105 Uiso 0.543(4) 1 calc R . P B 2
H40D H 1.000408 0.242799 0.743694 0.105 Uiso 0.543(4) 1 calc R . P B 2
O28A O 0.7783(3) 0.7176(2) 0.7344(3) 0.0579(7) Uani 0.543(4) 1 d . . P B 2
C4A C 1.0900(11) 0.3502(8) 0.7296(7) 0.102(2) Uani 0.543(4) 1 d . . P B 2
H4AA H 1.050587 0.308661 0.658458 0.122 Uiso 0.543(4) 1 calc R . P B 2
H4AB H 1.181117 0.347705 0.751243 0.122 Uiso 0.543(4) 1 calc R . P B 2
C31A C 0.8560(13) 0.8050(10) 0.7116(11) 0.077(3) Uani 0.543(4) 1 d . . P B 2
H31C H 0.923363 0.835213 0.779950 0.092 Uiso 0.543(4) 1 calc R . P B 2
H31D H 0.805228 0.862356 0.678624 0.092 Uiso 0.543(4) 1 calc R . P B 2
O2A O 1.0705(4) 0.4720(3) 0.7035(3) 0.0768(9) Uani 0.543(4) 1 d . . P B 2
C30A C 0.9133(5) 0.7609(3) 0.6315(4) 0.0737(12) Uani 0.543(4) 1 d . . P B 2
H30C H 0.845762 0.728432 0.564233 0.088 Uiso 0.543(4) 1 calc R . P B 2
H30D H 0.963729 0.819713 0.611110 0.088 Uiso 0.543(4) 1 calc R . P B 2
C37A C 1.1483(5) 0.5667(6) 0.6893(5) 0.0862(16) Uani 0.543(4) 1 d . . P B 2
H37C H 1.202700 0.545709 0.650469 0.103 Uiso 0.543(4) 1 calc R . P B 2
H37D H 1.202307 0.601474 0.761381 0.103 Uiso 0.543(4) 1 calc R . P B 2
O3A O 0.9921(3) 0.6805(3) 0.6848(3) 0.0663(8) Uani 0.543(4) 1 d . . P B 2
C1A C 1.0608(11) 0.6455(12) 0.6223(10) 0.077(3) Uani 0.543(4) 1 d . . P B 2
H1AA H 1.110916 0.707535 0.606112 0.092 Uiso 0.543(4) 1 calc R . P B 2
H1AB H 1.002774 0.609336 0.552274 0.092 Uiso 0.543(4) 1 calc R . P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S9 2.1591(5) . ?
Ni1 S7 2.1685(5) . ?
Ni1 S16 2.1598(5) . ?
Ni1 S15 2.1610(5) . ?
S6 C2 1.7433(16) . ?
S6 C5 1.7292(17) . ?
S9 C3 1.7168(16) . ?
S7 C2 1.7175(16) . ?
S16 C14 1.7112(16) . ?
S15 C10 1.7133(16) . ?
S4 C3 1.7386(16) . ?
S4 C5 1.7301(17) . ?
S13 C12 1.7241(19) . ?
S13 C14 1.7415(16) . ?
S11 C12 1.7303(19) . ?
S11 C10 1.7421(16) . ?
S8 C5 1.6472(16) . ?
S17 C12 1.6468(17) . ?
Cl18 C19 1.805(5) . ?
N21 H21A 0.8900 . ?
N21 H21B 0.8900 . ?
N21 H21C 0.8900 . ?
N21 C20 1.484(2) . ?
C3 C2 1.359(2) . ?
C10 C14 1.359(2) . ?
O23 C27 1.412(13) . ?
O23 C24 1.408(8) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 H20C 0.9700 . ?
C20 H20D 0.9700 . ?
C20 C19 1.490(4) . ?
C20 C19A 1.417(6) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 C31 1.510(16) . ?
C30 O3 1.367(14) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 O28 1.417(8) . ?
C32 C8 1.496(10) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C24 1.517(14) . ?
C22 O1 1.403(14) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C37 O2 1.404(17) . ?
C37 C1 1.506(16) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
O28 C31 1.399(8) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 C26 1.482(13) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C40 O6 1.594(11) . ?
C40 C4 1.067(12) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 O6 1.421(8) . ?
C19A H19C 0.9700 . ?
C19A H19D 0.9700 . ?
C19A Cl 1.760(9) . ?
O1 C8 1.423(9) . ?
O2 C4 1.414(11) . ?
O3 C1 1.407(8) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
O1A C22A 1.424(7) . ?
O1A C8A 1.410(7) . ?
O23A C27A 1.421(7) . ?
O23A C24A 1.392(12) . ?
C22A H22C 0.9700 . ?
C22A H22D 0.9700 . ?
C22A C24A 1.524(12) . ?
C27A H27C 0.9700 . ?
C27A H27D 0.9700 . ?
C27A C26A 1.478(11) . ?
C24A H24C 0.9700 . ?
C24A H24D 0.9700 . ?
C26A H26C 0.9700 . ?
C26A H26D 0.9700 . ?
C26A O6A 1.423(10) . ?
C8A H8AA 0.9700 . ?
C8A H8AB 0.9700 . ?
C8A C32A 1.481(8) . ?
O6A C40A 1.412(8) . ?
C32A H32C 0.9700 . ?
C32A H32D 0.9700 . ?
C32A O28A 1.422(6) . ?
C40A H40C 0.9700 . ?
C40A H40D 0.9700 . ?
C40A C4A 1.059(10) . ?
O28A C31A 1.415(13) . ?
C4A H4AA 0.9700 . ?
C4A H4AB 0.9700 . ?
C4A O2A 1.570(9) . ?
C31A H31C 0.9700 . ?
C31A H31D 0.9700 . ?
C31A C30A 1.517(13) . ?
O2A C37A 1.436(8) . ?
C30A H30C 0.9700 . ?
C30A H30D 0.9700 . ?
C30A O3A 1.428(6) . ?
C37A H37C 0.9700 . ?
C37A H37D 0.9700 . ?
C37A C1A 1.520(12) . ?
O3A C1A 1.391(15) . ?
C1A H1AA 0.9700 . ?
C1A H1AB 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S9 Ni1 S7 93.050(17) . . ?
S9 Ni1 S16 86.082(17) . . ?
S9 Ni1 S15 178.03(2) . . ?
S16 Ni1 S7 176.66(2) . . ?
S16 Ni1 S15 93.006(18) . . ?
S15 Ni1 S7 87.958(17) . . ?
C5 S6 C2 97.51(8) . . ?
C3 S9 Ni1 102.30(5) . . ?
C2 S7 Ni1 102.00(5) . . ?
C14 S16 Ni1 102.23(6) . . ?
C10 S15 Ni1 102.31(6) . . ?
C5 S4 C3 97.38(8) . . ?
C12 S13 C14 97.58(8) . . ?
C12 S11 C10 97.38(8) . . ?
H21A N21 H21B 109.5 . . ?
H21A N21 H21C 109.5 . . ?
H21B N21 H21C 109.5 . . ?
C20 N21 H21A 109.5 . . ?
C20 N21 H21B 109.5 . . ?
C20 N21 H21C 109.5 . . ?
S9 C3 S4 122.49(9) . . ?
C2 C3 S9 121.21(12) . . ?
C2 C3 S4 116.31(12) . . ?
S7 C2 S6 123.03(9) . . ?
C3 C2 S6 115.70(12) . . ?
C3 C2 S7 121.27(12) . . ?
S13 C12 S11 113.13(10) . . ?
S17 C12 S13 123.26(11) . . ?
S17 C12 S11 123.61(11) . . ?
S15 C10 S11 123.04(10) . . ?
C14 C10 S15 121.01(12) . . ?
C14 C10 S11 115.95(12) . . ?
S6 C5 S4 113.06(9) . . ?
S8 C5 S6 123.50(10) . . ?
S8 C5 S4 123.44(10) . . ?
S16 C14 S13 122.69(10) . . ?
C10 C14 S16 121.41(12) . . ?
C10 C14 S13 115.90(12) . . ?
C24 O23 C27 110.2(7) . . ?
N21 C20 H20A 109.0 . . ?
N21 C20 H20B 109.0 . . ?
N21 C20 H20C 109.6 . . ?
N21 C20 H20D 109.6 . . ?
N21 C20 C19 112.85(19) . . ?
H20A C20 H20B 107.8 . . ?
H20C C20 H20D 108.2 . . ?
C19 C20 H20A 109.0 . . ?
C19 C20 H20B 109.0 . . ?
C19A C20 N21 110.1(3) . . ?
C19A C20 H20C 109.6 . . ?
C19A C20 H20D 109.6 . . ?
H30A C30 H30B 108.1 . . ?
C31 C30 H30A 109.5 . . ?
C31 C30 H30B 109.5 . . ?
O3 C30 H30A 109.5 . . ?
O3 C30 H30B 109.5 . . ?
O3 C30 C31 110.8(8) . . ?
H32A C32 H32B 108.3 . . ?
O28 C32 H32A 110.0 . . ?
O28 C32 H32B 110.0 . . ?
O28 C32 C8 108.7(5) . . ?
C8 C32 H32A 110.0 . . ?
C8 C32 H32B 110.0 . . ?
H22A C22 H22B 108.3 . . ?
C24 C22 H22A 110.0 . . ?
C24 C22 H22B 110.0 . . ?
O1 C22 H22A 110.0 . . ?
O1 C22 H22B 110.0 . . ?
O1 C22 C24 108.6(8) . . ?
H37A C37 H37B 108.3 . . ?
O2 C37 H37A 109.9 . . ?
O2 C37 H37B 109.9 . . ?
O2 C37 C1 109.1(10) . . ?
C1 C37 H37A 109.9 . . ?
C1 C37 H37B 109.9 . . ?
Cl18 C19 H19A 109.2 . . ?
Cl18 C19 H19B 109.2 . . ?
C20 C19 Cl18 112.1(2) . . ?
C20 C19 H19A 109.2 . . ?
C20 C19 H19B 109.2 . . ?
H19A C19 H19B 107.9 . . ?
C31 O28 C32 111.0(6) . . ?
O23 C27 H27A 109.9 . . ?
O23 C27 H27B 109.9 . . ?
O23 C27 C26 108.9(7) . . ?
H27A C27 H27B 108.3 . . ?
C26 C27 H27A 109.9 . . ?
C26 C27 H27B 109.9 . . ?
H40A C40 H40B 106.4 . . ?
O6 C40 H40A 106.3 . . ?
O6 C40 H40B 106.3 . . ?
C4 C40 H40A 106.3 . . ?
C4 C40 H40B 106.3 . . ?
C4 C40 O6 124.0(7) . . ?
O23 C24 C22 108.9(7) . . ?
O23 C24 H24A 109.9 . . ?
O23 C24 H24B 109.9 . . ?
C22 C24 H24A 109.9 . . ?
C22 C24 H24B 109.9 . . ?
H24A C24 H24B 108.3 . . ?
C30 C31 H31A 109.9 . . ?
C30 C31 H31B 109.9 . . ?
O28 C31 C30 109.1(6) . . ?
O28 C31 H31A 109.9 . . ?
O28 C31 H31B 109.9 . . ?
H31A C31 H31B 108.3 . . ?
C27 C26 H26A 109.7 . . ?
C27 C26 H26B 109.7 . . ?
H26A C26 H26B 108.2 . . ?
O6 C26 C27 109.7(6) . . ?
O6 C26 H26A 109.7 . . ?
O6 C26 H26B 109.7 . . ?
C20 C19A H19C 109.4 . . ?
C20 C19A H19D 109.4 . . ?
C20 C19A Cl 111.1(5) . . ?
H19C C19A H19D 108.0 . . ?
Cl C19A H19C 109.4 . . ?
Cl C19A H19D 109.4 . . ?
C22 O1 C8 114.0(7) . . ?
C37 O2 C4 112.1(7) . . ?
C30 O3 C1 112.5(7) . . ?
C26 O6 C40 130.4(6) . . ?
C32 C8 H8A 110.1 . . ?
C32 C8 H8B 110.1 . . ?
O1 C8 C32 108.2(6) . . ?
O1 C8 H8A 110.1 . . ?
O1 C8 H8B 110.1 . . ?
H8A C8 H8B 108.4 . . ?
C40 C4 O2 126.3(8) . . ?
C40 C4 H4A 105.7 . . ?
C40 C4 H4B 105.7 . . ?
O2 C4 H4A 105.7 . . ?
O2 C4 H4B 105.7 . . ?
H4A C4 H4B 106.2 . . ?
C37 C1 H1A 109.4 . . ?
C37 C1 H1B 109.4 . . ?
O3 C1 C37 111.2(9) . . ?
O3 C1 H1A 109.4 . . ?
O3 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
C8A O1A C22A 113.7(5) . . ?
C24A O23A C27A 111.7(6) . . ?
O1A C22A H22C 110.1 . . ?
O1A C22A H22D 110.1 . . ?
O1A C22A C24A 107.8(6) . . ?
H22C C22A H22D 108.5 . . ?
C24A C22A H22C 110.1 . . ?
C24A C22A H22D 110.1 . . ?
O23A C27A H27C 109.6 . . ?
O23A C27A H27D 109.6 . . ?
O23A C27A C26A 110.1(5) . . ?
H27C C27A H27D 108.2 . . ?
C26A C27A H27C 109.6 . . ?
C26A C27A H27D 109.6 . . ?
O23A C24A C22A 108.4(6) . . ?
O23A C24A H24C 110.0 . . ?
O23A C24A H24D 110.0 . . ?
C22A C24A H24C 110.0 . . ?
C22A C24A H24D 110.0 . . ?
H24C C24A H24D 108.4 . . ?
C27A C26A H26C 109.8 . . ?
C27A C26A H26D 109.8 . . ?
H26C C26A H26D 108.2 . . ?
O6A C26A C27A 109.5(5) . . ?
O6A C26A H26C 109.8 . . ?
O6A C26A H26D 109.8 . . ?
O1A C8A H8AA 110.0 . . ?
O1A C8A H8AB 110.0 . . ?
O1A C8A C32A 108.3(4) . . ?
H8AA C8A H8AB 108.4 . . ?
C32A C8A H8AA 110.0 . . ?
C32A C8A H8AB 110.0 . . ?
C40A O6A C26A 112.9(5) . . ?
C8A C32A H32C 109.7 . . ?
C8A C32A H32D 109.7 . . ?
H32C C32A H32D 108.2 . . ?
O28A C32A C8A 109.6(4) . . ?
O28A C32A H32C 109.7 . . ?
O28A C32A H32D 109.7 . . ?
O6A C40A H40C 106.7 . . ?
O6A C40A H40D 106.7 . . ?
H40C C40A H40D 106.6 . . ?
C4A C40A O6A 122.6(7) . . ?
C4A C40A H40C 106.7 . . ?
C4A C40A H40D 106.7 . . ?
C31A O28A C32A 110.9(6) . . ?
C40A C4A H4AA 105.4 . . ?
C40A C4A H4AB 105.4 . . ?
C40A C4A O2A 127.6(6) . . ?
H4AA C4A H4AB 106.0 . . ?
O2A C4A H4AA 105.4 . . ?
O2A C4A H4AB 105.4 . . ?
O28A C31A H31C 110.1 . . ?
O28A C31A H31D 110.1 . . ?
O28A C31A C30A 107.9(8) . . ?
H31C C31A H31D 108.4 . . ?
C30A C31A H31C 110.1 . . ?
C30A C31A H31D 110.1 . . ?
C37A O2A C4A 135.6(6) . . ?
C31A C30A H30C 110.0 . . ?
C31A C30A H30D 110.0 . . ?
H30C C30A H30D 108.4 . . ?
O3A C30A C31A 108.5(7) . . ?
O3A C30A H30C 110.0 . . ?
O3A C30A H30D 110.0 . . ?
O2A C37A H37C 110.0 . . ?
O2A C37A H37D 110.0 . . ?
O2A C37A C1A 108.4(7) . . ?
H37C C37A H37D 108.4 . . ?
C1A C37A H37C 110.0 . . ?
C1A C37A H37D 110.0 . . ?
C1A O3A C30A 112.2(7) . . ?
C37A C1A H1AA 110.1 . . ?
C37A C1A H1AB 110.1 . . ?
O3A C1A C37A 108.1(9) . . ?
O3A C1A H1AA 110.1 . . ?
O3A C1A H1AB 110.1 . . ?
H1AA C1A H1AB 108.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S9 C3 S4 -178.01(9) . . . . ?
Ni1 S9 C3 C2 2.23(15) . . . . ?
Ni1 S7 C2 S6 177.01(9) . . . . ?
Ni1 S7 C2 C3 -3.34(15) . . . . ?
Ni1 S16 C14 S13 -177.78(9) . . . . ?
Ni1 S16 C14 C10 1.85(15) . . . . ?
Ni1 S15 C10 S11 -179.27(9) . . . . ?
Ni1 S15 C10 C14 0.97(15) . . . . ?
S9 C3 C2 S6 -179.52(9) . . . . ?
S9 C3 C2 S7 0.8(2) . . . . ?
S15 C10 C14 S16 -2.0(2) . . . . ?
S15 C10 C14 S13 177.64(9) . . . . ?
S4 C3 C2 S6 0.70(18) . . . . ?
S4 C3 C2 S7 -178.97(9) . . . . ?
S11 C10 C14 S16 178.21(9) . . . . ?
S11 C10 C14 S13 -2.15(18) . . . . ?
N21 C20 C19 Cl18 -72.4(3) . . . . ?
N21 C20 C19A Cl 81.1(5) . . . . ?
C3 S4 C5 S6 -1.70(11) . . . . ?
C3 S4 C5 S8 177.87(12) . . . . ?
C2 S6 C5 S4 2.00(11) . . . . ?
C2 S6 C5 S8 -177.57(12) . . . . ?
C12 S13 C14 S16 -179.87(11) . . . . ?
C12 S13 C14 C10 0.49(15) . . . . ?
C12 S11 C10 S15 -177.11(11) . . . . ?
C12 S11 C10 C14 2.66(15) . . . . ?
C10 S11 C12 S13 -2.23(11) . . . . ?
C10 S11 C12 S17 177.92(12) . . . . ?
C5 S6 C2 S7 178.02(11) . . . . ?
C5 S6 C2 C3 -1.65(15) . . . . ?
C5 S4 C3 S9 -179.16(11) . . . . ?
C5 S4 C3 C2 0.62(15) . . . . ?
C14 S13 C12 S11 1.32(11) . . . . ?
C14 S13 C12 S17 -178.84(12) . . . . ?
O23 C27 C26 O6 63.7(8) . . . . ?
C30 O3 C1 C37 173.9(9) . . . . ?
C32 O28 C31 C30 -177.6(7) . . . . ?
C22 O1 C8 C32 172.1(6) . . . . ?
C37 O2 C4 C40 137.0(12) . . . . ?
O28 C32 C8 O1 64.4(6) . . . . ?
C27 O23 C24 C22 177.3(7) . . . . ?
C27 C26 O6 C40 146.7(8) . . . . ?
C24 O23 C27 C26 175.9(6) . . . . ?
C24 C22 O1 C8 -177.7(6) . . . . ?
C31 C30 O3 C1 -178.3(7) . . . . ?
O1 C22 C24 O23 -64.8(8) . . . . ?
O2 C37 C1 O3 65.0(11) . . . . ?
O3 C30 C31 O28 -62.6(11) . . . . ?
O6 C40 C4 O2 5.9(16) . . . . ?
C8 C32 O28 C31 -174.4(5) . . . . ?
C4 C40 O6 C26 153.8(9) . . . . ?
C1 C37 O2 C4 -177.1(8) . . . . ?
O1A C22A C24A O23A -63.9(7) . . . . ?
O1A C8A C32A O28A 65.5(5) . . . . ?
O23A C27A C26A O6A 65.3(6) . . . . ?
C22A O1A C8A C32A 174.1(4) . . . . ?
C27A O23A C24A C22A 174.5(5) . . . . ?
C27A C26A O6A C40A 179.6(5) . . . . ?
C24A O23A C27A C26A 175.3(6) . . . . ?
C26A O6A C40A C4A 165.1(10) . . . . ?
C8A O1A C22A C24A -175.1(5) . . . . ?
C8A C32A O28A C31A 177.7(7) . . . . ?
O6A C40A C4A O2A -5.5(17) . . . . ?
C32A O28A C31A C30A -178.1(6) . . . . ?
C40A C4A O2A C37A 135.2(11) . . . . ?
O28A C31A C30A O3A -62.5(9) . . . . ?
C4A O2A C37A C1A 158.0(8) . . . . ?
C31A C30A O3A C1A -172.6(8) . . . . ?
O2A C37A C1A O3A 64.5(9) . . . . ?
C30A O3A C1A C37A 176.1(6) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.736
_oxdiff_exptl_absorpt_empirical_full_min 0.750
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_293k-f2
_database_code_depnum_ccdc_archive 'CCDC 2053400'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-18 downloaded from the CCDC.
;
_audit_creation_date             2020-11-24
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C2 H7 Cl N, C12 H24 O6'
_chemical_formula_sum            'C20 H30 Cl N Ni O6 S10'
_chemical_formula_weight         795.21
_chemical_melting_point          ?
_chemical_oxdiff_formula         C20H30NO6NiS10Cl
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.2892(3)
_cell_length_b                   12.3438(3)
_cell_length_c                   12.8805(3)
_cell_angle_alpha                91.047(2)
_cell_angle_beta                 110.467(2)
_cell_angle_gamma                96.326(2)
_cell_volume                     1668.26(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    14311
_cell_measurement_temperature    293
_cell_measurement_theta_max      28.7160
_cell_measurement_theta_min      1.6880
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.322
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65160
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             820
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.961
_exptl_crystal_size_mid          0.624
_exptl_crystal_size_min          0.371
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.890
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            32304
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.890
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.008
_diffrn_reflns_theta_min         1.941
_diffrn_ambient_temperature      293
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.890
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      4.00  90.00   0.50    0.15    --   21.85  34.00 -63.00  172
  2  ω    -37.00  25.00   0.50    0.15    --   21.85 -19.00 -30.00  124
  3  ω    -68.00  44.00   0.50    0.15    --   21.85 -37.00  60.00  224
  4  ω    -69.00  39.00   0.50    0.15    --   21.85 -34.00 139.00  216
  5  ω    -25.00  99.00   0.50    0.15    --   21.85  19.00  90.00  248
  6  ω     32.00  80.00   0.50    0.15    --   21.85 -99.00 -60.00   96
  7  ω    -14.00  36.00   0.50    0.15    --  -21.77 -99.00-120.00  100
  8  ω    -12.00  13.00   0.50    0.15    --   21.85 -99.00 -60.00   50
  9  ω    -17.00  37.00   0.50    0.15    --  -21.77 -99.00 -60.00  108
 10  ω    -18.00  37.00   0.50    0.15    --  -21.77 -99.00   0.00  110
 11  ω     67.00 104.00   0.50    0.15    --   21.85-178.00 120.00   74
 12  ω    -93.00  20.00   0.50    0.15    --  -21.77 -57.00 120.00  226
 13  ω    -99.00 -10.00   0.50    0.15    --  -21.77 -34.00 139.00  178
 14  ω    -38.00  60.00   0.50    0.15    --  -21.77  34.00 -63.00  196
 15  ω   -123.00 -50.00   0.50    0.15    --  -21.77 178.00 120.00  146
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0544227000
_diffrn_orient_matrix_UB_12      0.0203066000
_diffrn_orient_matrix_UB_13      0.0046622000
_diffrn_orient_matrix_UB_21      0.0346735000
_diffrn_orient_matrix_UB_22      0.0158448000
_diffrn_orient_matrix_UB_23      0.0567181000
_diffrn_orient_matrix_UB_31      0.0201038000
_diffrn_orient_matrix_UB_32      0.0518803000
_diffrn_orient_matrix_UB_33      -0.0151366000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5826
_reflns_number_total             7906
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         7906
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0366
_refine_ls_restrained_S_all      1.015
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0671P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1176
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
2. Others
 Sof(Cl1A)=Sof(H1BC)=Sof(H1BD)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(Cl1)=FVAR(1)
 Sof(H3BC)=Sof(H3BD)=Sof(O5A)=Sof(O4A)=Sof(C10A)=Sof(H10C)=Sof(H10D)=Sof(C9A)=
 Sof(H9AA)=Sof(H9AB)=Sof(H11C)=Sof(H11D)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(O3A)=
 Sof(C12A)=Sof(H12C)=Sof(H12D)=Sof(C13A)=Sof(H13C)=Sof(H13D)=Sof(C6A)=Sof(H6AA)=
 Sof(H6AB)=Sof(O6A)=Sof(O2A)=Sof(C14A)=Sof(H14C)=Sof(H14D)=Sof(C4A)=Sof(H4AA)=
 Sof(H4AB)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(O1A)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=1-
 FVAR(2)
 Sof(O4)=Sof(O1)=Sof(O3)=Sof(O6)=Sof(H3AA)=Sof(H3AB)=Sof(O5)=Sof(O2)=Sof(C9)=
 Sof(H9A)=Sof(H9B)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C13)=Sof(H13A)=Sof(H13B)=
 Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C7)=Sof(H7A)=
 Sof(H7B)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C8)=
 Sof(H8A)=Sof(H8B)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H11A)=Sof(H11B)=FVAR(2)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1BC,H1BD), C1(H1AA,H1AB), C3(H3AA,H3AB), C3(H3BC,H3BD), C9(H9A,H9B),
 C5(H5A,H5B), C13(H13A,H13B), C14(H14A,H14B), C4(H4A,H4B), C7(H7A,H7B), C2(H2A,
 H2B), C12(H12A,H12B), C6(H6A,H6B), C2A(H2AA,H2AB), C8(H8A,H8B), C10(H10A,H10B),
  C10A(H10C,H10D), C9A(H9AA,H9AB), C11(H11A,H11B), C11(H11C,H11D), C8A(H8AA,
 H8AB), C12A(H12C,H12D), C13A(H13C,H13D), C6A(H6AA,H6AB), C14A(H14C,H14D),
 C4A(H4AA,H4AB), C5A(H5AA,H5AB), C7A(H7AA,H7AB)
3.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.84531(2) 0.88971(2) 0.51234(2) 0.04738(10) Uani 1 1 d . . . . .
S6 S 0.69221(6) 0.97528(5) 0.52332(5) 0.05825(15) Uani 1 1 d . . . . .
S2 S 1.00548(5) 0.81224(5) 0.50685(5) 0.05875(15) Uani 1 1 d . . . . .
S1 S 0.79000(6) 0.92833(5) 0.34020(5) 0.05896(15) Uani 1 1 d . . . . .
S7 S 0.89915(6) 0.84503(5) 0.68224(5) 0.06050(16) Uani 1 1 d . . . . .
S8 S 0.61381(6) 1.02522(5) 0.72045(5) 0.05820(15) Uani 1 1 d . . . . .
S9 S 0.80184(6) 0.90271(5) 0.86494(5) 0.06316(17) Uani 1 1 d . . . . .
S4 S 1.09911(6) 0.77153(5) 0.31789(5) 0.06415(16) Uani 1 1 d . . . . .
S3 S 0.90711(6) 0.88540(5) 0.16649(5) 0.06458(16) Uani 1 1 d . . . . .
S10 S 0.62612(7) 1.00286(5) 0.95322(6) 0.07349(19) Uani 1 1 d . . . . .
S5 S 1.08920(7) 0.78573(6) 0.08553(6) 0.0799(2) Uani 1 1 d . . . . .
Cl1A Cl 0.8264(8) 0.4503(4) 0.5242(5) 0.0791(11) Uani 0.336(6) 1 d . . P A 2
N1 N 0.66566(17) 0.50211(12) 0.25596(15) 0.0558(4) Uani 1 1 d . . . . .
H1A H 0.654751 0.520928 0.187154 0.067 Uiso 1 1 calc R U . . .
H1B H 0.592294 0.500834 0.267543 0.067 Uiso 1 1 calc R U . . .
H1C H 0.691413 0.436191 0.264911 0.067 Uiso 1 1 calc R U . . .
C18 C 0.7086(2) 0.96494(15) 0.66035(17) 0.0480(4) Uani 1 1 d . . . . .
C19 C 0.7980(2) 0.90797(16) 0.72903(17) 0.0506(5) Uani 1 1 d . . . . .
C15 C 0.9025(2) 0.87631(15) 0.29995(17) 0.0492(5) Uani 1 1 d . . . . .
C17 C 1.0342(2) 0.81295(18) 0.18453(19) 0.0589(5) Uani 1 1 d . . . . .
C20 C 0.6781(2) 0.97829(16) 0.85177(19) 0.0547(5) Uani 1 1 d . . . . .
C16 C 0.9949(2) 0.82434(16) 0.37184(18) 0.0507(5) Uani 1 1 d . . . . .
O4 O 0.7050(5) 0.6190(4) 0.0795(4) 0.0733(13) Uani 0.540(5) 1 d . . P B 1
O1 O 0.5086(5) 0.3188(4) 0.3167(5) 0.0753(12) Uani 0.540(5) 1 d . . P B 1
O3 O 0.4919(4) 0.6522(4) 0.1418(5) 0.0742(12) Uani 0.540(5) 1 d . . P B 1
O6 O 0.7218(3) 0.2823(3) 0.2642(3) 0.0618(10) Uani 0.540(5) 1 d . . P B 1
C1 C 0.7631(3) 0.5827(2) 0.3364(2) 0.0795(8) Uani 1 1 d . . . . .
H1BC H 0.799292 0.634586 0.296545 0.095 Uiso 0.336(6) 1 calc R U P A 2
H1BD H 0.723377 0.622683 0.378050 0.095 Uiso 0.336(6) 1 calc R U P A 2
H1AA H 0.745383 0.655697 0.314524 0.095 Uiso 0.664(6) 1 calc R U P A 1
H1AB H 0.846100 0.573358 0.333405 0.095 Uiso 0.664(6) 1 calc R U P A 1
C3 C 0.6460(3) 0.2033(2) 0.3031(4) 0.0993(11) Uani 1 1 d . . . . .
H3AA H 0.581273 0.163985 0.238674 0.119 Uiso 0.540(5) 1 calc R U P B 1
H3AB H 0.700521 0.150950 0.343137 0.119 Uiso 0.540(5) 1 calc R U P B 1
H3BC H 0.713336 0.213329 0.375403 0.119 Uiso 0.460(5) 1 calc R U P B 2
H3BD H 0.598270 0.132044 0.299042 0.119 Uiso 0.460(5) 1 calc R U P B 2
O5 O 0.7884(5) 0.4162(4) 0.1167(4) 0.0754(12) Uani 0.540(5) 1 d . . P B 1
O2 O 0.4314(5) 0.5272(5) 0.2982(5) 0.0846(14) Uani 0.540(5) 1 d . . P B 1
C9 C 0.5497(13) 0.7320(8) 0.0924(8) 0.082(3) Uani 0.540(5) 1 d . . P B 1
H9A H 0.617220 0.777985 0.149427 0.098 Uiso 0.540(5) 1 calc R U P B 1
H9B H 0.487344 0.777676 0.050235 0.098 Uiso 0.540(5) 1 calc R U P B 1
C5 C 0.4390(16) 0.3543(16) 0.3766(14) 0.082(4) Uani 0.540(5) 1 d . . P B 1
H5A H 0.496128 0.390451 0.446468 0.099 Uiso 0.540(5) 1 calc R U P B 1
H5B H 0.388914 0.292349 0.392823 0.099 Uiso 0.540(5) 1 calc R U P B 1
C13 C 0.8675(8) 0.3386(8) 0.1740(8) 0.078(2) Uani 0.540(5) 1 d . . P B 1
H13A H 0.927827 0.370947 0.244440 0.093 Uiso 0.540(5) 1 calc R U P B 1
H13B H 0.914736 0.313193 0.130200 0.093 Uiso 0.540(5) 1 calc R U P B 1
C14 C 0.7812(6) 0.2452(6) 0.1926(5) 0.0742(18) Uani 0.540(5) 1 d . . P B 1
H14A H 0.717071 0.216963 0.122287 0.089 Uiso 0.540(5) 1 calc R U P B 1
H14B H 0.830246 0.186766 0.225397 0.089 Uiso 0.540(5) 1 calc R U P B 1
C4 C 0.5877(6) 0.2399(4) 0.3684(6) 0.0816(18) Uani 0.540(5) 1 d . . P B 1
H4A H 0.651122 0.271801 0.437616 0.098 Uiso 0.540(5) 1 calc R U P B 1
H4B H 0.536772 0.179203 0.385627 0.098 Uiso 0.540(5) 1 calc R U P B 1
C7 C 0.3566(10) 0.6072(10) 0.2427(11) 0.098(3) Uani 0.540(5) 1 d . . P B 1
H7A H 0.316900 0.637881 0.290309 0.118 Uiso 0.540(5) 1 calc R U P B 1
H7B H 0.289671 0.574214 0.175941 0.118 Uiso 0.540(5) 1 calc R U P B 1
C2 C 0.7676(5) 0.5725(3) 0.4527(3) 0.0856(17) Uani 0.664(6) 1 d . . P A 1
H2A H 0.681598 0.567851 0.453529 0.103 Uiso 0.664(6) 1 calc R U P A 1
H2B H 0.816014 0.637570 0.497213 0.103 Uiso 0.664(6) 1 calc R U P A 1
C12 C 0.8582(8) 0.5052(6) 0.0837(6) 0.093(2) Uani 0.540(5) 1 d . . P B 1
H12A H 0.923483 0.542211 0.149232 0.112 Uiso 0.540(5) 1 calc R U P B 1
H12B H 0.900164 0.476600 0.036966 0.112 Uiso 0.540(5) 1 calc R U P B 1
C6 C 0.3523(8) 0.4323(8) 0.3108(7) 0.094(2) Uani 0.540(5) 1 d . . P B 1
H6A H 0.299076 0.398351 0.238617 0.113 Uiso 0.540(5) 1 calc R U P B 1
H6B H 0.297481 0.452925 0.349479 0.113 Uiso 0.540(5) 1 calc R U P B 1
C2A C 0.8607(8) 0.5303(7) 0.4101(7) 0.081(3) Uani 0.336(6) 1 d . . P A 2
H2AA H 0.932729 0.585432 0.445737 0.098 Uiso 0.336(6) 1 calc R U P A 2
H2AB H 0.887587 0.480341 0.366164 0.098 Uiso 0.336(6) 1 calc R U P A 2
C8 C 0.4390(7) 0.6959(6) 0.2128(8) 0.093(2) Uani 0.540(5) 1 d . . P B 1
H8A H 0.388240 0.752349 0.176920 0.111 Uiso 0.540(5) 1 calc R U P B 1
H8B H 0.506096 0.728767 0.279500 0.111 Uiso 0.540(5) 1 calc R U P B 1
C10 C 0.6025(8) 0.6786(6) 0.0187(8) 0.0870(19) Uani 0.540(5) 1 d . . P B 1
H10A H 0.535604 0.628931 -0.034901 0.104 Uiso 0.540(5) 1 calc R U P B 1
H10B H 0.633501 0.733445 -0.021780 0.104 Uiso 0.540(5) 1 calc R U P B 1
O5A O 0.7760(5) 0.4747(5) 0.0800(5) 0.0757(14) Uani 0.460(5) 1 d . . P B 2
O4A O 0.6476(7) 0.6532(5) 0.0885(5) 0.0761(16) Uani 0.460(5) 1 d . . P B 2
C10A C 0.6946(11) 0.6351(7) 0.0018(7) 0.106(4) Uani 0.460(5) 1 d . . P B 2
H10C H 0.625468 0.600387 -0.062601 0.128 Uiso 0.460(5) 1 calc R U P B 2
H10D H 0.725257 0.704881 -0.019072 0.128 Uiso 0.460(5) 1 calc R U P B 2
C9A C 0.5364(16) 0.7052(10) 0.0467(9) 0.083(3) Uani 0.460(5) 1 d . . P B 2
H9AA H 0.470552 0.657533 -0.010035 0.099 Uiso 0.460(5) 1 calc R U P B 2
H9AB H 0.554605 0.771773 0.013309 0.099 Uiso 0.460(5) 1 calc R U P B 2
C11 C 0.7835(6) 0.5761(3) 0.0293(4) 0.1303(17) Uani 1 1 d . . . . .
H11A H 0.729228 0.541232 -0.042202 0.156 Uiso 0.540(5) 1 calc R U P B 1
H11B H 0.836975 0.636731 0.015043 0.156 Uiso 0.540(5) 1 calc R U P B 1
H11C H 0.858202 0.621352 0.079242 0.156 Uiso 0.460(5) 1 calc R U P B 2
H11D H 0.801497 0.560105 -0.037368 0.156 Uiso 0.460(5) 1 calc R U P B 2
C8A C 0.4900(9) 0.7319(7) 0.1402(8) 0.089(2) Uani 0.460(5) 1 d . . P B 2
H8AA H 0.556224 0.778282 0.197905 0.106 Uiso 0.460(5) 1 calc R U P B 2
H8AB H 0.415864 0.770590 0.112456 0.106 Uiso 0.460(5) 1 calc R U P B 2
O3A O 0.4579(6) 0.6323(4) 0.1841(5) 0.0701(13) Uani 0.460(5) 1 d . . P B 2
C12A C 0.8727(10) 0.4096(8) 0.1215(7) 0.094(3) Uani 0.460(5) 1 d . . P B 2
H12C H 0.932807 0.442213 0.191904 0.113 Uiso 0.460(5) 1 calc R U P B 2
H12D H 0.918095 0.405154 0.070280 0.113 Uiso 0.460(5) 1 calc R U P B 2
C13A C 0.8201(10) 0.2989(9) 0.1372(10) 0.079(3) Uani 0.460(5) 1 d . . P B 2
H13C H 0.756929 0.267373 0.067736 0.095 Uiso 0.460(5) 1 calc R U P B 2
H13D H 0.887626 0.252519 0.160384 0.095 Uiso 0.460(5) 1 calc R U P B 2
C6A C 0.3578(11) 0.5428(11) 0.2984(8) 0.101(3) Uani 0.460(5) 1 d . . P B 2
H6AA H 0.322814 0.554191 0.356066 0.121 Uiso 0.460(5) 1 calc R U P B 2
H6AB H 0.289063 0.509744 0.232789 0.121 Uiso 0.460(5) 1 calc R U P B 2
O6A O 0.7646(5) 0.3046(4) 0.2173(4) 0.0704(13) Uani 0.460(5) 1 d . . P B 2
O2A O 0.4522(6) 0.4721(5) 0.3342(5) 0.0823(16) Uani 0.460(5) 1 d . . P B 2
C14A C 0.6987(8) 0.2032(5) 0.2269(6) 0.080(2) Uani 0.460(5) 1 d . . P B 2
H14C H 0.632632 0.180755 0.155688 0.096 Uiso 0.460(5) 1 calc R U P B 2
H14D H 0.757808 0.149119 0.243481 0.096 Uiso 0.460(5) 1 calc R U P B 2
C4A C 0.5055(10) 0.2969(7) 0.3784(9) 0.089(3) Uani 0.460(5) 1 d . . P B 2
H4AA H 0.570451 0.329007 0.446671 0.106 Uiso 0.460(5) 1 calc R U P B 2
H4AB H 0.472526 0.225115 0.392922 0.106 Uiso 0.460(5) 1 calc R U P B 2
C5A C 0.400(2) 0.367(2) 0.3419(19) 0.105(8) Uani 0.460(5) 1 d . . P B 2
H5AA H 0.338704 0.338553 0.270414 0.126 Uiso 0.460(5) 1 calc R U P B 2
H5AB H 0.357234 0.366515 0.395190 0.126 Uiso 0.460(5) 1 calc R U P B 2
O1A O 0.5603(6) 0.2866(4) 0.2956(4) 0.0726(14) Uani 0.460(5) 1 d . . P B 2
C7A C 0.4143(13) 0.6533(11) 0.2714(11) 0.095(3) Uani 0.460(5) 1 d . . P B 2
H7AA H 0.349772 0.702587 0.249188 0.114 Uiso 0.460(5) 1 calc R U P B 2
H7AB H 0.484180 0.686490 0.336042 0.114 Uiso 0.460(5) 1 calc R U P B 2
Cl1 Cl 0.8312(5) 0.4666(3) 0.5078(3) 0.1271(14) Uani 0.664(6) 1 d . . P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S6 2.1658(6) . ?
Ni1 S2 2.1580(6) . ?
Ni1 S1 2.1608(6) . ?
Ni1 S7 2.1565(6) . ?
S6 C18 1.718(2) . ?
S2 C16 1.711(2) . ?
S1 C15 1.709(2) . ?
S7 C19 1.712(2) . ?
S8 C18 1.741(2) . ?
S8 C20 1.730(2) . ?
S9 C19 1.739(2) . ?
S9 C20 1.725(2) . ?
S4 C17 1.727(2) . ?
S4 C16 1.737(2) . ?
S3 C15 1.743(2) . ?
S3 C17 1.723(2) . ?
S10 C20 1.645(2) . ?
S5 C17 1.646(2) . ?
Cl1A C2A 1.911(10) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.482(3) . ?
C18 C19 1.360(3) . ?
C15 C16 1.360(3) . ?
O4 C10 1.438(10) . ?
O4 C11 1.407(7) . ?
O1 C5 1.38(2) . ?
O1 C4 1.410(8) . ?
O3 C9 1.404(13) . ?
O3 C8 1.386(10) . ?
O6 C3 1.437(5) . ?
O6 C14 1.412(8) . ?
C1 H1BC 0.9700 . ?
C1 H1BD 0.9700 . ?
C1 H1AA 0.9700 . ?
C1 H1AB 0.9700 . ?
C1 C2 1.490(5) . ?
C1 C2A 1.408(8) . ?
C3 H3AA 0.9700 . ?
C3 H3AB 0.9700 . ?
C3 H3BC 0.9700 . ?
C3 H3BD 0.9700 . ?
C3 C4 1.336(8) . ?
C3 C14A 1.314(9) . ?
C3 O1A 1.469(7) . ?
O5 C13 1.419(11) . ?
O5 C12 1.438(9) . ?
O2 C7 1.410(12) . ?
O2 C6 1.440(10) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.466(13) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.505(19) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.504(11) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.502(13) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 Cl1 1.616(6) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C11 1.318(9) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
O5A C11 1.430(8) . ?
O5A C12A 1.388(12) . ?
O4A C10A 1.418(12) . ?
O4A C9A 1.412(17) . ?
C10A H10C 0.9700 . ?
C10A H10D 0.9700 . ?
C10A C11 1.260(12) . ?
C9A H9AA 0.9700 . ?
C9A H9AB 0.9700 . ?
C9A C8A 1.515(15) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 H11C 0.9700 . ?
C11 H11D 0.9700 . ?
C8A H8AA 0.9700 . ?
C8A H8AB 0.9700 . ?
C8A O3A 1.426(10) . ?
O3A C7A 1.407(13) . ?
C12A H12C 0.9700 . ?
C12A H12D 0.9700 . ?
C12A C13A 1.476(14) . ?
C13A H13C 0.9700 . ?
C13A H13D 0.9700 . ?
C13A O6A 1.385(12) . ?
C6A H6AA 0.9700 . ?
C6A H6AB 0.9700 . ?
C6A O2A 1.409(14) . ?
C6A C7A 1.539(16) . ?
O6A C14A 1.415(9) . ?
O2A C5A 1.39(2) . ?
C14A H14C 0.9700 . ?
C14A H14D 0.9700 . ?
C4A H4AA 0.9700 . ?
C4A H4AB 0.9700 . ?
C4A C5A 1.49(2) . ?
C4A O1A 1.416(11) . ?
C5A H5AA 0.9700 . ?
C5A H5AB 0.9700 . ?
C7A H7AA 0.9700 . ?
C7A H7AB 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S2 Ni1 S6 176.72(2) . . ?
S2 Ni1 S1 92.96(2) . . ?
S1 Ni1 S6 87.98(2) . . ?
S7 Ni1 S6 93.04(2) . . ?
S7 Ni1 S2 86.12(2) . . ?
S7 Ni1 S1 177.94(2) . . ?
C18 S6 Ni1 101.99(7) . . ?
C16 S2 Ni1 102.32(8) . . ?
C15 S1 Ni1 102.34(7) . . ?
C19 S7 Ni1 102.45(7) . . ?
C20 S8 C18 97.53(10) . . ?
C20 S9 C19 97.56(10) . . ?
C17 S4 C16 97.55(11) . . ?
C17 S3 C15 97.49(11) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
S6 C18 S8 123.05(12) . . ?
C19 C18 S6 121.22(16) . . ?
C19 C18 S8 115.73(16) . . ?
S7 C19 S9 122.72(12) . . ?
C18 C19 S7 121.15(16) . . ?
C18 C19 S9 116.12(16) . . ?
S1 C15 S3 123.09(13) . . ?
C16 C15 S1 121.15(16) . . ?
C16 C15 S3 115.76(16) . . ?
S3 C17 S4 113.15(12) . . ?
S5 C17 S4 123.01(15) . . ?
S5 C17 S3 123.84(15) . . ?
S9 C20 S8 113.01(12) . . ?
S10 C20 S8 123.39(13) . . ?
S10 C20 S9 123.59(14) . . ?
S2 C16 S4 122.81(13) . . ?
C15 C16 S2 121.20(16) . . ?
C15 C16 S4 115.99(16) . . ?
C11 O4 C10 121.8(6) . . ?
C5 O1 C4 114.0(10) . . ?
C8 O3 C9 113.2(7) . . ?
C14 O6 C3 118.4(5) . . ?
N1 C1 H1BC 109.5 . . ?
N1 C1 H1BD 109.5 . . ?
N1 C1 H1AA 108.9 . . ?
N1 C1 H1AB 108.9 . . ?
N1 C1 C2 113.3(2) . . ?
H1BC C1 H1BD 108.1 . . ?
H1AA C1 H1AB 107.7 . . ?
C2 C1 H1AA 108.9 . . ?
C2 C1 H1AB 108.9 . . ?
C2A C1 N1 110.8(4) . . ?
C2A C1 H1BC 109.5 . . ?
C2A C1 H1BD 109.5 . . ?
O6 C3 H3AA 107.9 . . ?
O6 C3 H3AB 107.9 . . ?
H3AA C3 H3AB 107.2 . . ?
H3BC C3 H3BD 107.4 . . ?
C4 C3 O6 117.8(3) . . ?
C4 C3 H3AA 107.9 . . ?
C4 C3 H3AB 107.9 . . ?
C14A C3 H3BC 108.3 . . ?
C14A C3 H3BD 108.3 . . ?
C14A C3 O1A 115.9(4) . . ?
O1A C3 H3BC 108.3 . . ?
O1A C3 H3BD 108.3 . . ?
C13 O5 C12 112.5(7) . . ?
C7 O2 C6 110.8(8) . . ?
O3 C9 H9A 109.8 . . ?
O3 C9 H9B 109.8 . . ?
O3 C9 C10 109.5(8) . . ?
H9A C9 H9B 108.2 . . ?
C10 C9 H9A 109.8 . . ?
C10 C9 H9B 109.8 . . ?
O1 C5 H5A 109.8 . . ?
O1 C5 H5B 109.8 . . ?
O1 C5 C6 109.5(13) . . ?
H5A C5 H5B 108.2 . . ?
C6 C5 H5A 109.8 . . ?
C6 C5 H5B 109.8 . . ?
O5 C13 H13A 110.4 . . ?
O5 C13 H13B 110.4 . . ?
O5 C13 C14 106.8(6) . . ?
H13A C13 H13B 108.6 . . ?
C14 C13 H13A 110.4 . . ?
C14 C13 H13B 110.4 . . ?
O6 C14 C13 109.3(6) . . ?
O6 C14 H14A 109.8 . . ?
O6 C14 H14B 109.8 . . ?
C13 C14 H14A 109.8 . . ?
C13 C14 H14B 109.8 . . ?
H14A C14 H14B 108.3 . . ?
O1 C4 H4A 109.4 . . ?
O1 C4 H4B 109.4 . . ?
C3 C4 O1 111.2(6) . . ?
C3 C4 H4A 109.4 . . ?
C3 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
O2 C7 H7A 109.7 . . ?
O2 C7 H7B 109.7 . . ?
O2 C7 C8 109.6(8) . . ?
H7A C7 H7B 108.2 . . ?
C8 C7 H7A 109.7 . . ?
C8 C7 H7B 109.7 . . ?
C1 C2 H2A 109.0 . . ?
C1 C2 H2B 109.0 . . ?
C1 C2 Cl1 112.8(3) . . ?
H2A C2 H2B 107.8 . . ?
Cl1 C2 H2A 109.0 . . ?
Cl1 C2 H2B 109.0 . . ?
O5 C12 H12A 109.2 . . ?
O5 C12 H12B 109.2 . . ?
H12A C12 H12B 107.9 . . ?
C11 C12 O5 112.0(8) . . ?
C11 C12 H12A 109.2 . . ?
C11 C12 H12B 109.2 . . ?
O2 C6 C5 107.5(10) . . ?
O2 C6 H6A 110.2 . . ?
O2 C6 H6B 110.2 . . ?
C5 C6 H6A 110.2 . . ?
C5 C6 H6B 110.2 . . ?
H6A C6 H6B 108.5 . . ?
Cl1A C2A H2AA 107.6 . . ?
Cl1A C2A H2AB 107.6 . . ?
C1 C2A Cl1A 118.8(6) . . ?
C1 C2A H2AA 107.6 . . ?
C1 C2A H2AB 107.6 . . ?
H2AA C2A H2AB 107.0 . . ?
O3 C8 C7 109.4(7) . . ?
O3 C8 H8A 109.8 . . ?
O3 C8 H8B 109.8 . . ?
C7 C8 H8A 109.8 . . ?
C7 C8 H8B 109.8 . . ?
H8A C8 H8B 108.2 . . ?
O4 C10 C9 111.7(8) . . ?
O4 C10 H10A 109.3 . . ?
O4 C10 H10B 109.3 . . ?
C9 C10 H10A 109.3 . . ?
C9 C10 H10B 109.3 . . ?
H10A C10 H10B 107.9 . . ?
C12A O5A C11 127.0(8) . . ?
C9A O4A C10A 109.2(9) . . ?
O4A C10A H10C 109.1 . . ?
O4A C10A H10D 109.1 . . ?
H10C C10A H10D 107.9 . . ?
C11 C10A O4A 112.4(9) . . ?
C11 C10A H10C 109.1 . . ?
C11 C10A H10D 109.1 . . ?
O4A C9A H9AA 109.7 . . ?
O4A C9A H9AB 109.7 . . ?
O4A C9A C8A 109.8(8) . . ?
H9AA C9A H9AB 108.2 . . ?
C8A C9A H9AA 109.7 . . ?
C8A C9A H9AB 109.7 . . ?
O4 C11 H11A 107.9 . . ?
O4 C11 H11B 107.9 . . ?
C12 C11 O4 117.7(5) . . ?
C12 C11 H11A 107.9 . . ?
C12 C11 H11B 107.9 . . ?
O5A C11 H11C 106.5 . . ?
O5A C11 H11D 106.5 . . ?
C10A C11 O5A 123.2(5) . . ?
C10A C11 H11C 106.5 . . ?
C10A C11 H11D 106.5 . . ?
H11A C11 H11B 107.2 . . ?
H11C C11 H11D 106.5 . . ?
C9A C8A H8AA 110.0 . . ?
C9A C8A H8AB 110.0 . . ?
H8AA C8A H8AB 108.4 . . ?
O3A C8A C9A 108.5(8) . . ?
O3A C8A H8AA 110.0 . . ?
O3A C8A H8AB 110.0 . . ?
C7A O3A C8A 110.5(9) . . ?
O5A C12A H12C 109.5 . . ?
O5A C12A H12D 109.5 . . ?
O5A C12A C13A 110.6(9) . . ?
H12C C12A H12D 108.1 . . ?
C13A C12A H12C 109.5 . . ?
C13A C12A H12D 109.5 . . ?
C12A C13A H13C 109.8 . . ?
C12A C13A H13D 109.8 . . ?
H13C C13A H13D 108.2 . . ?
O6A C13A C12A 109.4(8) . . ?
O6A C13A H13C 109.8 . . ?
O6A C13A H13D 109.8 . . ?
H6AA C6A H6AB 108.1 . . ?
O2A C6A H6AA 109.6 . . ?
O2A C6A H6AB 109.6 . . ?
O2A C6A C7A 110.5(9) . . ?
C7A C6A H6AA 109.6 . . ?
C7A C6A H6AB 109.6 . . ?
C13A O6A C14A 112.3(8) . . ?
C5A O2A C6A 111.7(11) . . ?
C3 C14A O6A 115.0(7) . . ?
C3 C14A H14C 108.5 . . ?
C3 C14A H14D 108.5 . . ?
O6A C14A H14C 108.5 . . ?
O6A C14A H14D 108.5 . . ?
H14C C14A H14D 107.5 . . ?
H4AA C4A H4AB 108.1 . . ?
C5A C4A H4AA 109.5 . . ?
C5A C4A H4AB 109.5 . . ?
O1A C4A H4AA 109.5 . . ?
O1A C4A H4AB 109.5 . . ?
O1A C4A C5A 110.6(13) . . ?
O2A C5A C4A 108.5(16) . . ?
O2A C5A H5AA 110.0 . . ?
O2A C5A H5AB 110.0 . . ?
C4A C5A H5AA 110.0 . . ?
C4A C5A H5AB 110.0 . . ?
H5AA C5A H5AB 108.4 . . ?
C4A O1A C3 119.6(6) . . ?
O3A C7A C6A 107.0(8) . . ?
O3A C7A H7AA 110.3 . . ?
O3A C7A H7AB 110.3 . . ?
C6A C7A H7AA 110.3 . . ?
C6A C7A H7AB 110.3 . . ?
H7AA C7A H7AB 108.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S6 C18 S8 177.05(11) . . . . ?
Ni1 S6 C18 C19 -3.05(19) . . . . ?
Ni1 S2 C16 S4 -178.03(11) . . . . ?
Ni1 S2 C16 C15 1.69(19) . . . . ?
Ni1 S1 C15 S3 -179.11(10) . . . . ?
Ni1 S1 C15 C16 1.04(18) . . . . ?
Ni1 S7 C19 S9 -178.21(11) . . . . ?
Ni1 S7 C19 C18 2.23(19) . . . . ?
S6 C18 C19 S7 0.6(3) . . . . ?
S6 C18 C19 S9 -178.99(11) . . . . ?
S1 C15 C16 S2 -2.0(3) . . . . ?
S1 C15 C16 S4 177.79(10) . . . . ?
S8 C18 C19 S7 -179.49(11) . . . . ?
S8 C18 C19 S9 0.9(2) . . . . ?
S3 C15 C16 S2 178.20(10) . . . . ?
S3 C15 C16 S4 -2.1(2) . . . . ?
N1 C1 C2 Cl1 73.4(4) . . . . ?
N1 C1 C2A Cl1A -73.9(7) . . . . ?
C18 S8 C20 S9 2.07(14) . . . . ?
C18 S8 C20 S10 -177.68(14) . . . . ?
C19 S9 C20 S8 -1.68(14) . . . . ?
C19 S9 C20 S10 178.07(15) . . . . ?
C15 S3 C17 S4 -2.22(14) . . . . ?
C15 S3 C17 S5 177.92(15) . . . . ?
C17 S4 C16 S2 -179.83(14) . . . . ?
C17 S4 C16 C15 0.44(19) . . . . ?
C17 S3 C15 S1 -177.25(13) . . . . ?
C17 S3 C15 C16 2.61(18) . . . . ?
C20 S8 C18 S6 178.09(13) . . . . ?
C20 S8 C18 C19 -1.82(18) . . . . ?
C20 S9 C19 S7 -179.11(14) . . . . ?
C20 S9 C19 C18 0.48(19) . . . . ?
C16 S4 C17 S3 1.33(14) . . . . ?
C16 S4 C17 S5 -178.81(15) . . . . ?
O1 C5 C6 O2 -64.8(12) . . . . ?
O3 C9 C10 O4 -65.5(9) . . . . ?
O6 C3 C4 O1 56.3(6) . . . . ?
C3 O6 C14 C13 -173.1(5) . . . . ?
O5 C13 C14 O6 -64.9(7) . . . . ?
O5 C12 C11 O4 53.0(7) . . . . ?
O2 C7 C8 O3 61.4(9) . . . . ?
C9 O3 C8 C7 168.2(8) . . . . ?
C5 O1 C4 C3 175.8(9) . . . . ?
C13 O5 C12 C11 179.2(6) . . . . ?
C14 O6 C3 C4 -178.3(5) . . . . ?
C4 O1 C5 C6 -176.4(8) . . . . ?
C7 O2 C6 C5 -176.5(10) . . . . ?
C12 O5 C13 C14 -174.2(6) . . . . ?
C6 O2 C7 C8 -170.0(8) . . . . ?
C8 O3 C9 C10 -179.8(7) . . . . ?
C10 O4 C11 C12 -167.0(6) . . . . ?
O5A C12A C13A O6A -64.1(9) . . . . ?
O4A C10A C11 O5A 49.2(9) . . . . ?
O4A C9A C8A O3A -62.2(10) . . . . ?
C10A O4A C9A C8A -176.2(7) . . . . ?
C9A O4A C10A C11 -171.0(8) . . . . ?
C9A C8A O3A C7A 180.0(9) . . . . ?
C11 O4 C10 C9 -169.6(6) . . . . ?
C11 O5A C12A C13A -163.7(7) . . . . ?
C8A O3A C7A C6A 169.2(9) . . . . ?
C12A O5A C11 C10A -174.0(7) . . . . ?
C12A C13A O6A C14A 172.8(8) . . . . ?
C13A O6A C14A C3 178.8(6) . . . . ?
C6A O2A C5A C4A 179.1(12) . . . . ?
O2A C6A C7A O3A 61.9(10) . . . . ?
C14A C3 O1A C4A -176.2(6) . . . . ?
C5A C4A O1A C3 -166.9(10) . . . . ?
O1A C3 C14A O6A 53.9(7) . . . . ?
O1A C4A C5A O2A -66.1(17) . . . . ?
C7A C6A O2A C5A -170.3(13) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.230
_oxdiff_exptl_absorpt_empirical_full_min 0.554
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_193k-f
_database_code_depnum_ccdc_archive 'CCDC 2053396'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2020-12-31 deposited with the CCDC.	2021-03-18 downloaded from the CCDC.
;
_audit_creation_date             2020-11-24
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 Ni S10, C2 H7 Cl N, C12 H24 O6'
_chemical_formula_sum            'C20 H31 Cl N Ni O6 S10'
_chemical_formula_weight         796.22
_chemical_melting_point          ?
_chemical_oxdiff_formula         C20H30NO6NiS10Cl
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.25474(18)
_cell_length_b                   12.34881(18)
_cell_length_c                   12.82304(17)
_cell_angle_alpha                91.7415(11)
_cell_angle_beta                 111.2915(14)
_cell_angle_gamma                96.3016(12)
_cell_volume                     1645.75(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    17001
_cell_measurement_temperature    193
_cell_measurement_theta_max      28.9230
_cell_measurement_theta_min      2.0720
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.341
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72613
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             822
_exptl_crystal_size_max          0.961
_exptl_crystal_size_mid          0.624
_exptl_crystal_size_min          0.371
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0601
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.881
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            33190
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.881
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.126
_diffrn_reflns_theta_min         1.959
_diffrn_ambient_temperature      193
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -21.00 103.00   0.50    0.13    --   21.85  57.00 -90.00  248
  2  ω     64.00  90.00   0.50    0.13    --   21.85  34.00 -63.00   52
  3  ω    -25.00 104.00   0.50    0.13    --   21.85  19.00  90.00  258
  4  ω    -38.00  56.00   0.50    0.13    --  -21.77  34.00 -63.00  188
  5  ω    -78.00 -50.00   0.50    0.13    --  -21.77 178.00 120.00   56
  6  ω   -123.00 -89.00   0.50    0.13    --  -21.77 178.00 120.00   68
  7  ω    -25.00  60.00   0.50    0.13    --  -21.77  19.00  30.00  170
  8  ω    -69.00  40.00   0.50    0.13    --   21.85 -34.00 138.00  218
  9  ω    -68.00  44.00   0.50    0.13    --   21.85 -37.00  60.00  224
 10  ω    -15.00  11.00   0.50    0.13    --   21.85 -99.00 -60.00   52
 11  ω     31.00  81.00   0.50    0.13    --   21.85 -99.00 -60.00  100
 12  ω     62.00 103.00   0.50    0.13    --   21.85-178.00 120.00   82
 13  ω    -18.00  37.00   0.50    0.13    --  -21.77 -99.00  60.00  110
 14  ω   -103.00  12.00   0.50    0.13    --  -21.77 -34.00 138.00  230
 15  ω    -16.00  36.00   0.50    0.13    --  -21.77 -99.00   0.00  104
 16  ω    -17.00  37.00   0.50    0.13    --  -21.77 -99.00 -60.00  108
 17  ω    -18.00  37.00   0.50    0.13    --  -21.77 -99.00-120.00  110
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0549913000
_diffrn_orient_matrix_UB_12      0.0200007000
_diffrn_orient_matrix_UB_13      0.0040841000
_diffrn_orient_matrix_UB_21      0.0347358000
_diffrn_orient_matrix_UB_22      0.0155792000
_diffrn_orient_matrix_UB_23      0.0577690000
_diffrn_orient_matrix_UB_31      0.0205598000
_diffrn_orient_matrix_UB_32      0.0521155000
_diffrn_orient_matrix_UB_33      -0.0138147000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6275
_reflns_number_total             7803
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS n/a (Sheldrick, 2008)'
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         7803
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0347
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0464P)²+0.0253P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.0965
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
2. Others
 Sof(Cl1A)=Sof(H1BC)=Sof(H1BD)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(Cl1)=FVAR(1)
 Sof(H3BC)=Sof(H3BD)=Sof(O5A)=Sof(O4A)=Sof(C10A)=Sof(H10C)=Sof(H10D)=Sof(C9A)=
 Sof(H9AA)=Sof(H9AB)=Sof(H11C)=Sof(H11D)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(O3A)=
 Sof(C12A)=Sof(H12C)=Sof(H12D)=Sof(C13A)=Sof(H13C)=Sof(H13D)=Sof(C6A)=Sof(H6AA)=
 Sof(H6AB)=Sof(O6A)=Sof(O2A)=Sof(C14A)=Sof(H14C)=Sof(H14D)=Sof(C4A)=Sof(H4AA)=
 Sof(H4AB)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(O1A)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=1-
 FVAR(2)
 Sof(O4)=Sof(O1)=Sof(O3)=Sof(O6)=Sof(H3AA)=Sof(H3AB)=Sof(O5)=Sof(O2)=Sof(C9)=
 Sof(H9A)=Sof(H9B)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C13)=Sof(H13A)=Sof(H13B)=
 Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C7)=Sof(H7A)=
 Sof(H7B)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C8)=
 Sof(H8A)=Sof(H8B)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H11A)=Sof(H11B)=FVAR(2)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1AA,H1AB), C1(H1BC,H1BD), C3(H3AA,H3AB), C3(H3BC,H3BD), C9(H9A,H9B),
 C5(H5A,H5B), C13(H13A,H13B), C14(H14A,H14B), C4(H4A,H4B), C7(H7A,H7B), C2(H2A,
 H2B), C12(H12A,H12B), C6(H6A,H6B), C2A(H2AA,H2AB), C8(H8A,H8B), C10(H10A,H10B),
  C10A(H10C,H10D), C9A(H9AA,H9AB), C11(H11C,H11D), C11(H11A,H11B), C8A(H8AA,
 H8AB), C12A(H12C,H12D), C13A(H13C,H13D), C6A(H6AA,H6AB), C14A(H14C,H14D),
 C4A(H4AA,H4AB), C5A(H5AA,H5AB), C7A(H7AA,H7AB)
3.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.84534(2) 0.89023(2) 0.51234(2) 0.03214(8) Uani 1 1 d . . . . .
S6 S 0.69185(5) 0.97673(4) 0.52284(4) 0.04065(12) Uani 1 1 d . . . . .
S2 S 1.00582(5) 0.81152(4) 0.50749(4) 0.03935(12) Uani 1 1 d . . . . .
S1 S 0.79262(5) 0.93284(4) 0.34051(4) 0.04025(12) Uani 1 1 d . . . . .
S7 S 0.89824(5) 0.84338(4) 0.68266(4) 0.04009(12) Uani 1 1 d . . . . .
S8 S 0.61372(5) 1.02695(4) 0.72123(4) 0.03966(12) Uani 1 1 d . . . . .
S9 S 0.80158(5) 0.90195(4) 0.86655(4) 0.04169(13) Uani 1 1 d . . . . .
S4 S 1.09999(5) 0.77090(4) 0.31797(4) 0.04445(13) Uani 1 1 d . . . . .
S3 S 0.90987(5) 0.88955(4) 0.16623(4) 0.04352(13) Uani 1 1 d . . . . .
S10 S 0.62590(6) 1.00331(4) 0.95530(5) 0.04938(14) Uani 1 1 d . . . . .
S5 S 1.09076(6) 0.78731(5) 0.08436(5) 0.05463(15) Uani 1 1 d . . . . .
Cl1A Cl 0.8396(8) 0.4491(5) 0.5300(6) 0.0467(10) Uani 0.236(5) 1 d . . P A 2
N1 N 0.66652(15) 0.50243(11) 0.25488(13) 0.0377(4) Uani 1 1 d . . . . .
H1A H 0.661187 0.518226 0.186192 0.045 Uiso 1 1 calc R U . . .
H1B H 0.590284 0.504095 0.260667 0.045 Uiso 1 1 calc R U . . .
H1C H 0.689955 0.436052 0.267475 0.045 Uiso 1 1 calc R U . . .
C18 C 0.70884(18) 0.96599(14) 0.66109(15) 0.0336(4) Uani 1 1 d . . . . .
C19 C 0.79728(18) 0.90760(14) 0.72966(15) 0.0341(4) Uani 1 1 d . . . . .
C15 C 0.90457(18) 0.87946(14) 0.30019(15) 0.0353(4) Uani 1 1 d . . . . .
C17 C 1.03645(19) 0.81487(16) 0.18422(16) 0.0411(4) Uani 1 1 d . . . . .
C20 C 0.67794(19) 0.97873(14) 0.85331(16) 0.0372(4) Uani 1 1 d . . . . .
C16 C 0.99639(18) 0.82519(14) 0.37229(15) 0.0350(4) Uani 1 1 d . . . . .
O4 O 0.7103(4) 0.6187(3) 0.0810(3) 0.0462(8) Uani 0.515(3) 1 d . . P B 1
O1 O 0.5036(3) 0.3216(3) 0.3108(3) 0.0489(8) Uani 0.515(3) 1 d . . P B 1
O3 O 0.4950(3) 0.6537(3) 0.1366(3) 0.0512(9) Uani 0.515(3) 1 d . . P B 1
O6 O 0.7204(3) 0.2826(2) 0.2648(3) 0.0422(8) Uani 0.515(3) 1 d . . P B 1
C1 C 0.7637(2) 0.58418(16) 0.33896(18) 0.0511(5) Uani 1 1 d . . . . .
H1AA H 0.743550 0.656929 0.318918 0.061 Uiso 0.764(5) 1 calc R U P A 1
H1AB H 0.847683 0.577684 0.336376 0.061 Uiso 0.764(5) 1 calc R U P A 1
H1BC H 0.797451 0.638998 0.300811 0.061 Uiso 0.236(5) 1 calc R U P A 2
H1BD H 0.723591 0.620505 0.383179 0.061 Uiso 0.236(5) 1 calc R U P A 2
C3 C 0.6451(3) 0.20393(18) 0.3021(3) 0.0704(8) Uani 1 1 d . . . . .
H3AA H 0.582046 0.161926 0.236450 0.085 Uiso 0.515(3) 1 calc R U P B 1
H3AB H 0.701312 0.153897 0.345335 0.085 Uiso 0.515(3) 1 calc R U P B 1
H3BC H 0.713633 0.215925 0.375485 0.085 Uiso 0.485(3) 1 calc R U P B 2
H3BD H 0.597849 0.132414 0.298399 0.085 Uiso 0.485(3) 1 calc R U P B 2
O5 O 0.7924(4) 0.4141(3) 0.1169(3) 0.0481(8) Uani 0.515(3) 1 d . . P B 1
O2 O 0.4279(4) 0.5303(3) 0.2915(3) 0.0542(9) Uani 0.515(3) 1 d . . P B 1
C9 C 0.5582(9) 0.7336(7) 0.0911(6) 0.0540(18) Uani 0.515(3) 1 d . . P B 1
H9A H 0.626870 0.777870 0.151262 0.065 Uiso 0.515(3) 1 calc R U P B 1
H9B H 0.497782 0.781148 0.048749 0.065 Uiso 0.515(3) 1 calc R U P B 1
C5 C 0.4329(17) 0.3570(15) 0.3717(14) 0.056(3) Uani 0.515(3) 1 d . . P B 1
H5A H 0.490550 0.391566 0.443954 0.068 Uiso 0.515(3) 1 calc R U P B 1
H5B H 0.380023 0.295253 0.384416 0.068 Uiso 0.515(3) 1 calc R U P B 1
C13 C 0.8700(6) 0.3369(5) 0.1789(5) 0.0518(14) Uani 0.515(3) 1 d . . P B 1
H13A H 0.928371 0.370669 0.251318 0.062 Uiso 0.515(3) 1 calc R U P B 1
H13B H 0.920458 0.310650 0.138461 0.062 Uiso 0.515(3) 1 calc R U P B 1
C14 C 0.7818(4) 0.2440(4) 0.1943(4) 0.0480(12) Uani 0.515(3) 1 d . . P B 1
H14A H 0.717808 0.215487 0.122039 0.058 Uiso 0.515(3) 1 calc R U P B 1
H14B H 0.830471 0.185680 0.228094 0.058 Uiso 0.515(3) 1 calc R U P B 1
C4 C 0.5820(5) 0.2411(3) 0.3649(5) 0.0569(13) Uani 0.515(3) 1 d . . P B 1
H4A H 0.644007 0.272543 0.436890 0.068 Uiso 0.515(3) 1 calc R U P B 1
H4B H 0.528475 0.180436 0.378485 0.068 Uiso 0.515(3) 1 calc R U P B 1
C7 C 0.3533(6) 0.6115(5) 0.2327(6) 0.0663(16) Uani 0.515(3) 1 d . . P B 1
H7A H 0.311815 0.643212 0.278494 0.080 Uiso 0.515(3) 1 calc R U P B 1
H7B H 0.287063 0.578407 0.163535 0.080 Uiso 0.515(3) 1 calc R U P B 1
C2 C 0.7692(3) 0.5708(2) 0.4564(2) 0.0586(10) Uani 0.764(5) 1 d . . P A 1
H2A H 0.682938 0.566975 0.456948 0.070 Uiso 0.764(5) 1 calc R U P A 1
H2B H 0.820182 0.634599 0.504182 0.070 Uiso 0.764(5) 1 calc R U P A 1
C12 C 0.8634(6) 0.5011(4) 0.0854(4) 0.0594(13) Uani 0.515(3) 1 d . . P B 1
H12A H 0.932690 0.535611 0.152052 0.071 Uiso 0.515(3) 1 calc R U P B 1
H12B H 0.901710 0.471353 0.035991 0.071 Uiso 0.515(3) 1 calc R U P B 1
C6 C 0.3479(5) 0.4386(5) 0.3045(4) 0.0599(13) Uani 0.515(3) 1 d . . P B 1
H6A H 0.292045 0.404459 0.231385 0.072 Uiso 0.515(3) 1 calc R U P B 1
H6B H 0.294580 0.461721 0.343543 0.072 Uiso 0.515(3) 1 calc R U P B 1
C2A C 0.8636(9) 0.5323(7) 0.4092(7) 0.051(3) Uani 0.236(5) 1 d . . P A 2
H2AA H 0.937069 0.587811 0.443736 0.061 Uiso 0.236(5) 1 calc R U P A 2
H2AB H 0.886988 0.482761 0.361903 0.061 Uiso 0.236(5) 1 calc R U P A 2
C8 C 0.4398(5) 0.6984(5) 0.2072(5) 0.0615(14) Uani 0.515(3) 1 d . . P B 1
H8A H 0.390912 0.755748 0.170900 0.074 Uiso 0.515(3) 1 calc R U P B 1
H8B H 0.506979 0.730232 0.276398 0.074 Uiso 0.515(3) 1 calc R U P B 1
C10 C 0.6117(6) 0.6797(4) 0.0169(5) 0.0582(13) Uani 0.515(3) 1 d . . P B 1
H10A H 0.543968 0.631317 -0.040077 0.070 Uiso 0.515(3) 1 calc R U P B 1
H10B H 0.646835 0.734354 -0.020537 0.070 Uiso 0.515(3) 1 calc R U P B 1
O5A O 0.7752(3) 0.4773(3) 0.0808(3) 0.0486(9) Uani 0.485(3) 1 d . . P B 2
O4A O 0.6469(4) 0.6575(3) 0.0907(3) 0.0483(9) Uani 0.485(3) 1 d . . P B 2
C10A C 0.6958(6) 0.6376(4) 0.0056(5) 0.0602(15) Uani 0.485(3) 1 d . . P B 2
H10C H 0.626033 0.601851 -0.060021 0.072 Uiso 0.485(3) 1 calc R U P B 2
H10D H 0.725831 0.707189 -0.015237 0.072 Uiso 0.485(3) 1 calc R U P B 2
C9A C 0.5314(10) 0.7070(7) 0.0474(6) 0.058(2) Uani 0.485(3) 1 d . . P B 2
H9AA H 0.464909 0.657412 -0.009364 0.069 Uiso 0.485(3) 1 calc R U P B 2
H9AB H 0.546758 0.773375 0.013109 0.069 Uiso 0.485(3) 1 calc R U P B 2
C11 C 0.7911(4) 0.5766(2) 0.0336(3) 0.0923(11) Uani 1 1 d . . . . .
H11C H 0.867077 0.620680 0.086400 0.111 Uiso 0.485(3) 1 calc R U P B 2
H11D H 0.809035 0.560297 -0.033309 0.111 Uiso 0.485(3) 1 calc R U P B 2
H11A H 0.737959 0.545683 -0.041554 0.111 Uiso 0.515(3) 1 calc R U P B 1
H11B H 0.848521 0.637603 0.025682 0.111 Uiso 0.515(3) 1 calc R U P B 1
C8A C 0.4894(6) 0.7327(4) 0.1415(5) 0.0599(15) Uani 0.485(3) 1 d . . P B 2
H8AA H 0.557616 0.779561 0.199716 0.072 Uiso 0.485(3) 1 calc R U P B 2
H8AB H 0.414543 0.771222 0.114942 0.072 Uiso 0.485(3) 1 calc R U P B 2
O3A O 0.4585(4) 0.6334(3) 0.1864(3) 0.0469(8) Uani 0.485(3) 1 d . . P B 2
C12A C 0.8759(6) 0.4127(5) 0.1218(4) 0.0582(14) Uani 0.485(3) 1 d . . P B 2
H12C H 0.936748 0.444654 0.194078 0.070 Uiso 0.485(3) 1 calc R U P B 2
H12D H 0.920944 0.409764 0.070322 0.070 Uiso 0.485(3) 1 calc R U P B 2
C13A C 0.8213(7) 0.3008(6) 0.1336(6) 0.0550(15) Uani 0.485(3) 1 d . . P B 2
H13C H 0.755833 0.270853 0.062601 0.066 Uiso 0.485(3) 1 calc R U P B 2
H13D H 0.888366 0.253673 0.154911 0.066 Uiso 0.485(3) 1 calc R U P B 2
C6A C 0.3587(6) 0.5448(5) 0.3007(5) 0.0634(16) Uani 0.485(3) 1 d . . P B 2
H6AA H 0.324674 0.555884 0.359187 0.076 Uiso 0.485(3) 1 calc R U P B 2
H6AB H 0.288495 0.512278 0.233690 0.076 Uiso 0.485(3) 1 calc R U P B 2
O6A O 0.7666(3) 0.3062(3) 0.2171(3) 0.0478(9) Uani 0.485(3) 1 d . . P B 2
O2A O 0.4539(4) 0.4741(3) 0.3354(3) 0.0516(9) Uani 0.485(3) 1 d . . P B 2
C14A C 0.6987(5) 0.2028(4) 0.2232(4) 0.0528(12) Uani 0.485(3) 1 d . . P B 2
H14C H 0.631563 0.180901 0.150566 0.063 Uiso 0.485(3) 1 calc R U P B 2
H14D H 0.757847 0.148537 0.239403 0.063 Uiso 0.485(3) 1 calc R U P B 2
C4A C 0.5067(6) 0.2950(5) 0.3768(6) 0.0604(16) Uani 0.485(3) 1 d . . P B 2
H4AA H 0.573990 0.324986 0.446777 0.072 Uiso 0.485(3) 1 calc R U P B 2
H4AB H 0.471269 0.223281 0.388677 0.072 Uiso 0.485(3) 1 calc R U P B 2
C5A C 0.4022(18) 0.3686(15) 0.3423(15) 0.065(4) Uani 0.485(3) 1 d . . P B 2
H5AA H 0.337553 0.340999 0.270071 0.078 Uiso 0.485(3) 1 calc R U P B 2
H5AB H 0.360979 0.368958 0.396881 0.078 Uiso 0.485(3) 1 calc R U P B 2
O1A O 0.5589(4) 0.2854(3) 0.2929(3) 0.0482(9) Uani 0.485(3) 1 d . . P B 2
C7A C 0.4158(7) 0.6537(5) 0.2767(6) 0.0626(17) Uani 0.485(3) 1 d . . P B 2
H7AA H 0.351675 0.703589 0.255754 0.075 Uiso 0.485(3) 1 calc R U P B 2
H7AB H 0.487552 0.685975 0.342758 0.075 Uiso 0.485(3) 1 calc R U P B 2
Cl1 Cl 0.8323(3) 0.4598(2) 0.5088(2) 0.0914(8) Uani 0.764(5) 1 d . . P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S6 2.1698(5) . ?
Ni1 S2 2.1620(5) . ?
Ni1 S1 2.1618(5) . ?
Ni1 S7 2.1603(5) . ?
S6 C18 1.7235(18) . ?
S2 C16 1.7127(18) . ?
S1 C15 1.7098(19) . ?
S7 C19 1.7173(18) . ?
S8 C18 1.7461(18) . ?
S8 C20 1.7355(19) . ?
S9 C19 1.7421(18) . ?
S9 C20 1.7298(19) . ?
S4 C17 1.732(2) . ?
S4 C16 1.7400(19) . ?
S3 C15 1.7481(18) . ?
S3 C17 1.731(2) . ?
S10 C20 1.6483(19) . ?
S5 C17 1.6482(19) . ?
Cl1A C2A 1.967(11) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.487(2) . ?
C18 C19 1.358(3) . ?
C15 C16 1.367(3) . ?
O4 C10 1.427(6) . ?
O4 C11 1.397(5) . ?
O1 C5 1.392(19) . ?
O1 C4 1.428(6) . ?
O3 C9 1.415(10) . ?
O3 C8 1.401(7) . ?
O6 C3 1.426(4) . ?
O6 C14 1.421(6) . ?
C1 H1AA 0.9700 . ?
C1 H1AB 0.9700 . ?
C1 H1BC 0.9700 . ?
C1 H1BD 0.9700 . ?
C1 C2 1.499(3) . ?
C1 C2A 1.394(8) . ?
C3 H3AA 0.9700 . ?
C3 H3AB 0.9700 . ?
C3 H3BC 0.9700 . ?
C3 H3BD 0.9700 . ?
C3 C4 1.351(6) . ?
C3 C14A 1.354(6) . ?
C3 O1A 1.451(5) . ?
O5 C13 1.424(7) . ?
O5 C12 1.425(6) . ?
O2 C7 1.432(7) . ?
O2 C6 1.420(6) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.475(11) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.529(15) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.498(8) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.493(8) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 Cl1 1.661(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C11 1.335(6) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
O5A C11 1.406(5) . ?
O5A C12A 1.409(7) . ?
O4A C10A 1.416(7) . ?
O4A C9A 1.430(12) . ?
C10A H10C 0.9700 . ?
C10A H10D 0.9700 . ?
C10A C11 1.327(7) . ?
C9A H9AA 0.9700 . ?
C9A H9AB 0.9700 . ?
C9A C8A 1.485(11) . ?
C11 H11C 0.9700 . ?
C11 H11D 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C8A H8AA 0.9700 . ?
C8A H8AB 0.9700 . ?
C8A O3A 1.431(6) . ?
O3A C7A 1.430(7) . ?
C12A H12C 0.9700 . ?
C12A H12D 0.9700 . ?
C12A C13A 1.484(9) . ?
C13A H13C 0.9700 . ?
C13A H13D 0.9700 . ?
C13A O6A 1.419(7) . ?
C6A H6AA 0.9700 . ?
C6A H6AB 0.9700 . ?
C6A O2A 1.411(7) . ?
C6A C7A 1.515(9) . ?
O6A C14A 1.433(6) . ?
O2A C5A 1.386(19) . ?
C14A H14C 0.9700 . ?
C14A H14D 0.9700 . ?
C4A H4AA 0.9700 . ?
C4A H4AB 0.9700 . ?
C4A C5A 1.513(17) . ?
C4A O1A 1.409(7) . ?
C5A H5AA 0.9700 . ?
C5A H5AB 0.9700 . ?
C7A H7AA 0.9700 . ?
C7A H7AB 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S2 Ni1 S6 176.82(2) . . ?
S1 Ni1 S6 87.853(19) . . ?
S1 Ni1 S2 93.015(19) . . ?
S7 Ni1 S6 93.176(19) . . ?
S7 Ni1 S2 86.014(18) . . ?
S7 Ni1 S1 178.52(2) . . ?
C18 S6 Ni1 101.80(6) . . ?
C16 S2 Ni1 102.33(7) . . ?
C15 S1 Ni1 102.34(6) . . ?
C19 S7 Ni1 102.23(6) . . ?
C20 S8 C18 97.31(9) . . ?
C20 S9 C19 97.47(9) . . ?
C17 S4 C16 97.56(9) . . ?
C17 S3 C15 97.50(9) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
S6 C18 S8 122.78(11) . . ?
C19 C18 S6 121.27(14) . . ?
C19 C18 S8 115.94(14) . . ?
S7 C19 S9 122.50(11) . . ?
C18 C19 S7 121.32(14) . . ?
C18 C19 S9 116.18(14) . . ?
S1 C15 S3 123.11(11) . . ?
C16 C15 S1 121.25(14) . . ?
C16 C15 S3 115.64(14) . . ?
S3 C17 S4 113.12(11) . . ?
S5 C17 S4 123.20(12) . . ?
S5 C17 S3 123.68(12) . . ?
S9 C20 S8 113.05(10) . . ?
S10 C20 S8 123.37(11) . . ?
S10 C20 S9 123.57(11) . . ?
S2 C16 S4 122.86(11) . . ?
C15 C16 S2 121.03(14) . . ?
C15 C16 S4 116.11(14) . . ?
C11 O4 C10 120.6(4) . . ?
C5 O1 C4 112.5(8) . . ?
C8 O3 C9 113.3(5) . . ?
C14 O6 C3 117.8(3) . . ?
N1 C1 H1AA 109.0 . . ?
N1 C1 H1AB 109.0 . . ?
N1 C1 H1BC 109.7 . . ?
N1 C1 H1BD 109.7 . . ?
N1 C1 C2 113.11(18) . . ?
H1AA C1 H1AB 107.8 . . ?
H1BC C1 H1BD 108.2 . . ?
C2 C1 H1AA 109.0 . . ?
C2 C1 H1AB 109.0 . . ?
C2A C1 N1 109.8(4) . . ?
C2A C1 H1BC 109.7 . . ?
C2A C1 H1BD 109.7 . . ?
O6 C3 H3AA 107.9 . . ?
O6 C3 H3AB 107.9 . . ?
H3AA C3 H3AB 107.2 . . ?
H3BC C3 H3BD 107.5 . . ?
C4 C3 O6 117.7(3) . . ?
C4 C3 H3AA 107.9 . . ?
C4 C3 H3AB 107.9 . . ?
C14A C3 H3BC 108.4 . . ?
C14A C3 H3BD 108.4 . . ?
C14A C3 O1A 115.5(3) . . ?
O1A C3 H3BC 108.4 . . ?
O1A C3 H3BD 108.4 . . ?
C13 O5 C12 113.4(5) . . ?
C6 O2 C7 111.3(5) . . ?
O3 C9 H9A 109.7 . . ?
O3 C9 H9B 109.7 . . ?
O3 C9 C10 109.7(6) . . ?
H9A C9 H9B 108.2 . . ?
C10 C9 H9A 109.7 . . ?
C10 C9 H9B 109.7 . . ?
O1 C5 H5A 110.0 . . ?
O1 C5 H5B 110.0 . . ?
O1 C5 C6 108.4(12) . . ?
H5A C5 H5B 108.4 . . ?
C6 C5 H5A 110.0 . . ?
C6 C5 H5B 110.0 . . ?
O5 C13 H13A 110.2 . . ?
O5 C13 H13B 110.2 . . ?
O5 C13 C14 107.6(4) . . ?
H13A C13 H13B 108.5 . . ?
C14 C13 H13A 110.2 . . ?
C14 C13 H13B 110.2 . . ?
O6 C14 C13 108.8(5) . . ?
O6 C14 H14A 109.9 . . ?
O6 C14 H14B 109.9 . . ?
C13 C14 H14A 109.9 . . ?
C13 C14 H14B 109.9 . . ?
H14A C14 H14B 108.3 . . ?
O1 C4 H4A 109.3 . . ?
O1 C4 H4B 109.3 . . ?
C3 C4 O1 111.7(5) . . ?
C3 C4 H4A 109.3 . . ?
C3 C4 H4B 109.3 . . ?
H4A C4 H4B 107.9 . . ?
O2 C7 H7A 109.9 . . ?
O2 C7 H7B 109.9 . . ?
O2 C7 C8 109.1(5) . . ?
H7A C7 H7B 108.3 . . ?
C8 C7 H7A 109.9 . . ?
C8 C7 H7B 109.9 . . ?
C1 C2 H2A 109.0 . . ?
C1 C2 H2B 109.0 . . ?
C1 C2 Cl1 112.9(2) . . ?
H2A C2 H2B 107.8 . . ?
Cl1 C2 H2A 109.0 . . ?
Cl1 C2 H2B 109.0 . . ?
O5 C12 H12A 109.0 . . ?
O5 C12 H12B 109.0 . . ?
H12A C12 H12B 107.8 . . ?
C11 C12 O5 112.9(5) . . ?
C11 C12 H12A 109.0 . . ?
C11 C12 H12B 109.0 . . ?
O2 C6 C5 108.8(9) . . ?
O2 C6 H6A 109.9 . . ?
O2 C6 H6B 109.9 . . ?
C5 C6 H6A 109.9 . . ?
C5 C6 H6B 109.9 . . ?
H6A C6 H6B 108.3 . . ?
Cl1A C2A H2AA 107.3 . . ?
Cl1A C2A H2AB 107.3 . . ?
C1 C2A Cl1A 120.0(6) . . ?
C1 C2A H2AA 107.3 . . ?
C1 C2A H2AB 107.3 . . ?
H2AA C2A H2AB 106.9 . . ?
O3 C8 C7 110.0(6) . . ?
O3 C8 H8A 109.7 . . ?
O3 C8 H8B 109.7 . . ?
C7 C8 H8A 109.7 . . ?
C7 C8 H8B 109.7 . . ?
H8A C8 H8B 108.2 . . ?
O4 C10 C9 110.0(6) . . ?
O4 C10 H10A 109.7 . . ?
O4 C10 H10B 109.7 . . ?
C9 C10 H10A 109.7 . . ?
C9 C10 H10B 109.7 . . ?
H10A C10 H10B 108.2 . . ?
C11 O5A C12A 122.0(4) . . ?
C10A O4A C9A 110.8(6) . . ?
O4A C10A H10C 108.5 . . ?
O4A C10A H10D 108.5 . . ?
H10C C10A H10D 107.5 . . ?
C11 C10A O4A 114.9(5) . . ?
C11 C10A H10C 108.5 . . ?
C11 C10A H10D 108.5 . . ?
O4A C9A H9AA 110.0 . . ?
O4A C9A H9AB 110.0 . . ?
O4A C9A C8A 108.5(6) . . ?
H9AA C9A H9AB 108.4 . . ?
C8A C9A H9AA 110.0 . . ?
C8A C9A H9AB 110.0 . . ?
O4 C11 H11A 107.5 . . ?
O4 C11 H11B 107.5 . . ?
C12 C11 O4 119.3(3) . . ?
C12 C11 H11A 107.5 . . ?
C12 C11 H11B 107.5 . . ?
O5A C11 H11C 107.7 . . ?
O5A C11 H11D 107.7 . . ?
C10A C11 O5A 118.6(3) . . ?
C10A C11 H11C 107.7 . . ?
C10A C11 H11D 107.7 . . ?
H11C C11 H11D 107.1 . . ?
H11A C11 H11B 107.0 . . ?
C9A C8A H8AA 109.8 . . ?
C9A C8A H8AB 109.8 . . ?
H8AA C8A H8AB 108.2 . . ?
O3A C8A C9A 109.4(6) . . ?
O3A C8A H8AA 109.8 . . ?
O3A C8A H8AB 109.8 . . ?
C8A O3A C7A 111.7(5) . . ?
O5A C12A H12C 109.9 . . ?
O5A C12A H12D 109.9 . . ?
O5A C12A C13A 109.1(6) . . ?
H12C C12A H12D 108.3 . . ?
C13A C12A H12C 109.9 . . ?
C13A C12A H12D 109.9 . . ?
C12A C13A H13C 109.9 . . ?
C12A C13A H13D 109.9 . . ?
H13C C13A H13D 108.3 . . ?
O6A C13A C12A 108.8(5) . . ?
O6A C13A H13C 109.9 . . ?
O6A C13A H13D 109.9 . . ?
H6AA C6A H6AB 108.2 . . ?
O2A C6A H6AA 109.7 . . ?
O2A C6A H6AB 109.7 . . ?
O2A C6A C7A 109.9(5) . . ?
C7A C6A H6AA 109.7 . . ?
C7A C6A H6AB 109.7 . . ?
C13A O6A C14A 111.5(5) . . ?
C5A O2A C6A 112.0(8) . . ?
C3 C14A O6A 113.6(4) . . ?
C3 C14A H14C 108.9 . . ?
C3 C14A H14D 108.9 . . ?
O6A C14A H14C 108.9 . . ?
O6A C14A H14D 108.9 . . ?
H14C C14A H14D 107.7 . . ?
H4AA C4A H4AB 108.1 . . ?
C5A C4A H4AA 109.6 . . ?
C5A C4A H4AB 109.6 . . ?
O1A C4A H4AA 109.6 . . ?
O1A C4A H4AB 109.6 . . ?
O1A C4A C5A 110.2(9) . . ?
O2A C5A C4A 110.3(13) . . ?
O2A C5A H5AA 109.6 . . ?
O2A C5A H5AB 109.6 . . ?
C4A C5A H5AA 109.6 . . ?
C4A C5A H5AB 109.6 . . ?
H5AA C5A H5AB 108.1 . . ?
C4A O1A C3 118.0(4) . . ?
O3A C7A C6A 107.4(5) . . ?
O3A C7A H7AA 110.2 . . ?
O3A C7A H7AB 110.2 . . ?
C6A C7A H7AA 110.2 . . ?
C6A C7A H7AB 110.2 . . ?
H7AA C7A H7AB 108.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S6 C18 S8 177.07(9) . . . . ?
Ni1 S6 C18 C19 -3.76(17) . . . . ?
Ni1 S2 C16 S4 -177.33(10) . . . . ?
Ni1 S2 C16 C15 2.06(17) . . . . ?
Ni1 S1 C15 S3 -179.80(10) . . . . ?
Ni1 S1 C15 C16 0.41(17) . . . . ?
Ni1 S7 C19 S9 -177.74(10) . . . . ?
Ni1 S7 C19 C18 2.34(17) . . . . ?
S6 C18 C19 S7 1.0(2) . . . . ?
S6 C18 C19 S9 -178.90(10) . . . . ?
S1 C15 C16 S2 -1.8(2) . . . . ?
S1 C15 C16 S4 177.65(9) . . . . ?
S8 C18 C19 S7 -179.75(9) . . . . ?
S8 C18 C19 S9 0.3(2) . . . . ?
S3 C15 C16 S2 178.43(9) . . . . ?
S3 C15 C16 S4 -2.1(2) . . . . ?
N1 C1 C2 Cl1 70.6(3) . . . . ?
N1 C1 C2A Cl1A -77.2(7) . . . . ?
C18 S8 C20 S9 2.01(12) . . . . ?
C18 S8 C20 S10 -177.77(13) . . . . ?
C19 S9 C20 S8 -1.87(12) . . . . ?
C19 S9 C20 S10 177.91(13) . . . . ?
C15 S3 C17 S4 -1.94(12) . . . . ?
C15 S3 C17 S5 177.63(13) . . . . ?
C17 S4 C16 S2 -179.91(12) . . . . ?
C17 S4 C16 C15 0.68(17) . . . . ?
C17 S3 C15 S1 -177.32(12) . . . . ?
C17 S3 C15 C16 2.48(16) . . . . ?
C20 S8 C18 S6 177.78(12) . . . . ?
C20 S8 C18 C19 -1.43(16) . . . . ?
C20 S9 C19 S7 -178.98(12) . . . . ?
C20 S9 C19 C18 0.95(16) . . . . ?
C16 S4 C17 S3 1.02(12) . . . . ?
C16 S4 C17 S5 -178.55(13) . . . . ?
O1 C5 C6 O2 -62.3(12) . . . . ?
O3 C9 C10 O4 -65.4(6) . . . . ?
O6 C3 C4 O1 53.6(5) . . . . ?
C3 O6 C14 C13 -171.9(3) . . . . ?
O5 C13 C14 O6 -66.6(5) . . . . ?
O5 C12 C11 O4 48.7(5) . . . . ?
O2 C7 C8 O3 62.4(6) . . . . ?
C9 O3 C8 C7 168.5(5) . . . . ?
C5 O1 C4 C3 177.0(9) . . . . ?
C13 O5 C12 C11 -176.0(4) . . . . ?
C14 O6 C3 C4 -177.0(4) . . . . ?
C4 O1 C5 C6 -177.4(8) . . . . ?
C7 O2 C6 C5 -177.8(8) . . . . ?
C12 O5 C13 C14 -173.4(4) . . . . ?
C6 O2 C7 C8 -172.1(5) . . . . ?
C8 O3 C9 C10 -179.2(5) . . . . ?
C10 O4 C11 C12 -165.8(4) . . . . ?
O5A C12A C13A O6A -65.0(6) . . . . ?
O4A C10A C11 O5A 50.2(6) . . . . ?
O4A C9A C8A O3A -63.6(7) . . . . ?
C10A O4A C9A C8A -176.3(5) . . . . ?
C9A O4A C10A C11 -169.9(5) . . . . ?
C9A C8A O3A C7A -179.2(6) . . . . ?
C11 O4 C10 C9 -168.4(4) . . . . ?
C11 O5A C12A C13A -163.0(4) . . . . ?
C8A O3A C7A C6A 167.8(5) . . . . ?
C12A O5A C11 C10A -174.2(4) . . . . ?
C12A C13A O6A C14A 173.1(5) . . . . ?
C13A O6A C14A C3 179.9(4) . . . . ?
C6A O2A C5A C4A 178.6(8) . . . . ?
O2A C6A C7A O3A 62.2(6) . . . . ?
C14A C3 O1A C4A -176.1(4) . . . . ?
C5A C4A O1A C3 -169.9(8) . . . . ?
O1A C3 C14A O6A 55.5(5) . . . . ?
O1A C4A C5A O2A -64.9(13) . . . . ?
C7A C6A O2A C5A -171.1(9) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.751
_oxdiff_exptl_absorpt_empirical_full_min 0.573
