# Supplementary Information (SI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_18c6_nc2oc2n_lt_02_113_00_autored
_database_code_depnum_ccdc_archive 'CCDC 2384649'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2024-09-17 deposited with the CCDC.	2024-11-08 downloaded from the CCDC.
;
_audit_creation_date             2023-12-22
_audit_creation_method           
;
Olex2 1.5-ac5-023
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C6 Ni S10), C4 H14 N2 O, 2(C12 H24 O6)'
_chemical_formula_sum            'C40 H62 N2 Ni2 O13 S20'
_chemical_formula_weight         1537.53
_chemical_melting_point          ?
_chemical_oxdiff_formula         C40H62N2Ni2O13S20
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                   13.0860(3)
_cell_length_b                   14.4188(3)
_cell_length_c                   18.1738(4)
_cell_angle_alpha                90.798(2)
_cell_angle_beta                 100.154(2)
_cell_angle_gamma                104.883(2)
_cell_volume                     3255.84(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    17613
_cell_measurement_temperature    112.95(10)
_cell_measurement_theta_max      30.7950
_cell_measurement_theta_min      2.0230
_shelx_estimated_absorpt_T_max   0.916
_shelx_estimated_absorpt_T_min   0.487
_exptl_absorpt_coefficient_mu    1.274
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31252
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.67a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark black'
_exptl_crystal_colour_modifier   dark
_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             1592
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-18 0 1 0.2125
0 17 12 0.2014
18 0 -2 0.3233
1 -17 -12 0.2287
-1 2 -25 0.0403
0 -1 25 0.0097

_exptl_crystal_size_max          0.658
_exptl_crystal_size_mid          0.505
_exptl_crystal_size_min          0.075
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-17.6348 -0.1477 1.3584 0.2210 0.6259 0.7480
-0.4112 17.0281 11.5476 -0.3009 -0.8485 0.4353
17.7609 -0.2807 -1.6585 -0.2149 -0.6086 -0.7639
1.0369 -17.1764 -11.6996 0.2958 0.8341 -0.4657
-0.8548 1.9994 -24.9750 0.9856 0.0777 -0.1502
-0.0950 -1.3272 25.2432 -0.9758 -0.0769 0.2048

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_unetI/netI     0.0542
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.792
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            43040
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.792
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.896
_diffrn_reflns_theta_min         2.164
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      112.95(10)
_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 0.792
_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    1.46    --   -5.80 -99.00   0.00   90
  2  ω    -77.00   4.00   0.50    1.46    --   -5.80 -37.00 -90.00  162
  3  ω    -75.00 -43.00   0.50    1.46    --   -5.80 -57.00  30.00   64
  4  ω    -38.00   3.00   0.50    1.46    --   -5.80 -57.00  30.00   82
  5  ω    -15.00  68.00   0.50    1.46    --   -5.80  37.00-150.00  166
  6  ω    -67.00   7.00   0.50    1.46    --   -5.80 -37.00  30.00  148
  7  ω    -11.00  35.00   0.50    1.46    --    6.03 -99.00-150.00   92
;
_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      -0.0155484000
_diffrn_orient_matrix_UB_12      0.0079269000
_diffrn_orient_matrix_UB_13      -0.0382968000
_diffrn_orient_matrix_UB_21      -0.0355325000
_diffrn_orient_matrix_UB_22      -0.0468596000
_diffrn_orient_matrix_UB_23      -0.0056447000
_diffrn_orient_matrix_UB_31      -0.0418814000
_diffrn_orient_matrix_UB_32      0.0185006000
_diffrn_orient_matrix_UB_33      0.0089279000
_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                11146
_reflns_number_total             16286
_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 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.054
_refine_diff_density_min         -1.239
_refine_diff_density_rms         0.099
_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     862
_refine_ls_number_reflns         16286
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0871
_refine_ls_R_factor_gt           0.0508
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0574P)²+5.3728P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1193
_refine_ls_wR_factor_ref         0.1378
_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. Others
 Sof(C29A)=Sof(H29C)=Sof(H29D)=Sof(O12A)=Sof(C37A)=Sof(H37C)=Sof(H37D)=
 Sof(C36A)=Sof(H36C)=Sof(H36D)=Sof(C38A)=Sof(H38C)=Sof(H38D)=Sof(C35A)=
 Sof(H35C)=Sof(H35D)=Sof(O13A)=Sof(O11A)=Sof(C39A)=Sof(H39C)=Sof(H39D)=
 Sof(C34A)=Sof(H34C)=Sof(H34D)=Sof(C40A)=Sof(H40C)=Sof(H40D)=Sof(O8A)=Sof(O10A)=
 Sof(C30A)=Sof(H30C)=Sof(H30D)=Sof(C32A)=Sof(H32C)=Sof(H32D)=Sof(O9A)=Sof(C31A)=
 Sof(H31C)=Sof(H31D)=Sof(C33A)=Sof(H33C)=Sof(H33D)=1-FVAR(1)
 Sof(O12)=Sof(O8)=Sof(O13)=Sof(O10)=Sof(O11)=Sof(C38)=Sof(H38A)=Sof(H38B)=
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C40)=Sof(H40A)=
 Sof(H40B)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(O9)=Sof(C32)=Sof(H32A)=Sof(H32B)=
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(C29)=Sof(H29A)=
 Sof(H29B)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C31)=
 Sof(H31A)=Sof(H31B)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C27(H27A,H27B), C25(H25A,H25B), C28(H28A,H28B), C13(H13A,
 H13B), C21(H21A,H21B), C14(H14A,H14B), C16(H16A,H16B), C22(H22A,H22B),
 C24(H24A,H24B), C23(H23A,H23B), C18(H18A,H18B), C17(H17A,H17B), C15(H15A,H15B),
  C20(H20A,H20B), C19(H19A,H19B), C38(H38A,H38B), C39(H39A,H39B), C37(H37A,
 H37B), C40(H40A,H40B), C35(H35A,H35B), C32(H32A,H32B), C36(H36A,H36B),
 C34(H34A,H34B), C29(H29A,H29B), C30(H30A,H30B), C29A(H29C,H29D), C37A(H37C,
 H37D), C36A(H36C,H36D), C38A(H38C,H38D), C35A(H35C,H35D), C39A(H39C,H39D),
 C34A(H34C,H34D), C40A(H40C,H40D), C30A(H30C,H30D), C32A(H32C,H32D), C33(H33A,
 H33B), C31(H31A,H31B), C31A(H31C,H31D), C33A(H33C,H33D)
3.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(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 0.70143(3) 0.92142(3) 0.98416(3) 0.02605(11) Uani 1 1 d . . . . .
Ni2 Ni 0.500000 0.500000 1.000000 0.02856(14) Uani 1 2 d S . P . .
Ni3 Ni 0.500000 0.500000 0.500000 0.03238(15) Uani 1 2 d S . P . .
S4 S 0.53004(7) 0.90272(6) 0.95900(5) 0.02839(18) Uani 1 1 d . . . . .
S6 S 0.69767(7) 1.00133(7) 1.08479(5) 0.0323(2) Uani 1 1 d . . . . .
S5 S 0.70101(7) 0.83514(6) 0.88519(6) 0.0320(2) Uani 1 1 d . . . . .
S7 S 0.87316(7) 0.94057(6) 1.01210(5) 0.03154(19) Uani 1 1 d . . . . .
S15 S 0.59551(7) 0.64758(7) 1.00914(5) 0.0332(2) Uani 1 1 d . . . . .
S14 S 0.57653(7) 0.47000(7) 1.10952(5) 0.0331(2) Uani 1 1 d . . . . .
S13 S 0.76759(8) 0.76236(7) 1.13593(6) 0.0379(2) Uani 1 1 d . . . . .
S2 S 0.35908(7) 0.78920(6) 0.83304(6) 0.0339(2) Uani 1 1 d . . . . .
S9 S 1.03417(8) 1.02705(7) 1.15452(6) 0.0401(2) Uani 1 1 d . . . . .
S20 S 0.59410(8) 0.49506(8) 0.41423(6) 0.0400(2) Uani 1 1 d . . . . .
S19 S 0.63888(8) 0.56953(7) 0.58358(6) 0.0382(2) Uani 1 1 d . . . . .
S17 S 0.87664(8) 0.62675(7) 0.57628(6) 0.0412(2) Uani 1 1 d . . . . .
S12 S 0.75015(8) 0.59901(7) 1.22839(6) 0.0387(2) Uani 1 1 d . . . . .
S8 S 0.87062(9) 1.07967(7) 1.22158(6) 0.0424(2) Uani 1 1 d . . . . .
S11 S 0.91600(8) 0.78250(8) 1.28291(7) 0.0496(3) Uani 1 1 d . . . . .
S3 S 0.51403(8) 0.71916(7) 0.76809(6) 0.0428(2) Uani 1 1 d . . . . .
S18 S 0.83585(9) 0.55909(9) 0.42031(6) 0.0498(3) Uani 1 1 d . . . . .
S10 S 1.09162(11) 1.11732(8) 1.31068(7) 0.0578(3) Uani 1 1 d . . . . .
S1 S 0.28025(9) 0.65370(11) 0.69917(9) 0.0700(4) Uani 1 1 d . . . . .
S16 S 1.06107(11) 0.64345(12) 0.49828(8) 0.0731(4) Uani 1 1 d . . . . .
O7 O 0.24290(19) 0.67578(17) 0.30619(14) 0.0312(5) Uani 1 1 d . . . . .
O5 O 0.0811(2) 0.71850(17) 0.02878(15) 0.0347(6) Uani 1 1 d . . . . .
O4 O 0.2933(2) 0.73446(17) 0.09953(15) 0.0344(6) Uani 1 1 d . . . . .
O6 O -0.0918(2) 0.5769(2) 0.06613(15) 0.0394(6) Uani 1 1 d . . . . .
O2 O 0.1682(2) 0.42531(17) 0.21257(15) 0.0374(6) Uani 1 1 d . . . . .
O1 O -0.0367(2) 0.41701(18) 0.13832(16) 0.0392(6) Uani 1 1 d . . . . .
O3 O 0.3297(2) 0.56322(19) 0.15841(15) 0.0363(6) Uani 1 1 d . . . . .
N1 N 0.1206(2) 0.60068(19) 0.15444(16) 0.0274(6) Uani 1 1 d . . . . .
H1A H 0.102805 0.624489 0.109247 0.033 Uiso 1 1 calc R U . . .
H1B H 0.087019 0.536801 0.152446 0.033 Uiso 1 1 calc R U . . .
H1C H 0.193097 0.609345 0.165718 0.033 Uiso 1 1 calc R U . . .
O12 O 0.6519(16) 0.8519(13) 0.3727(10) 0.061(6) Uani 0.561(7) 1 d . . P A 1
N2 N 0.4327(3) 0.8158(2) 0.39518(18) 0.0346(7) Uani 1 1 d . . . . .
H2A H 0.394140 0.833552 0.353618 0.042 Uiso 1 1 calc R U . . .
H2B H 0.504265 0.840765 0.395894 0.042 Uiso 1 1 calc R U . . .
H2C H 0.414945 0.838464 0.436834 0.042 Uiso 1 1 calc R U . . .
O8 O 0.4252(14) 0.8608(14) 0.5552(9) 0.047(4) Uani 0.561(7) 1 d . . P A 1
O13 O 0.6056(7) 0.8091(6) 0.5143(5) 0.0479(19) Uani 0.561(7) 1 d . . P A 1
C26 C 0.1308(3) 0.6315(3) 0.2910(2) 0.0338(8) Uani 1 1 d . . . . .
H26A H 0.095358 0.657197 0.327426 0.041 Uiso 1 1 calc R U . . .
H26B H 0.117396 0.561219 0.295444 0.041 Uiso 1 1 calc R U . . .
C9 C 0.6733(3) 0.6565(3) 1.0975(2) 0.0322(8) Uani 1 1 d . . . . .
C5 C 0.8285(3) 1.0243(2) 1.1313(2) 0.0331(8) Uani 1 1 d . . . . .
C27 C 0.2898(3) 0.6627(3) 0.3811(2) 0.0375(9) Uani 1 1 d . . . . .
H27A H 0.276971 0.593249 0.389250 0.045 Uiso 1 1 calc R U . . .
H27B H 0.256390 0.691920 0.416965 0.045 Uiso 1 1 calc R U . . .
C25 C 0.0859(3) 0.6520(3) 0.2132(2) 0.0367(9) Uani 1 1 d . . . . .
H25A H 0.006346 0.632918 0.205631 0.044 Uiso 1 1 calc R U . . .
H25B H 0.109166 0.722066 0.207432 0.044 Uiso 1 1 calc R U . . .
C28 C 0.4081(3) 0.7093(3) 0.3939(2) 0.0378(9) Uani 1 1 d . . . . .
H28A H 0.442641 0.690195 0.442110 0.045 Uiso 1 1 calc R U . . .
H28B H 0.438949 0.685845 0.353612 0.045 Uiso 1 1 calc R U . . .
C4 C 0.9054(3) 0.9987(3) 1.1000(2) 0.0332(8) Uani 1 1 d . . . . .
C2 C 0.5662(3) 0.7976(2) 0.8479(2) 0.0310(7) Uani 1 1 d . . . . .
C13 C 0.2685(3) 0.7919(3) 0.0396(2) 0.0413(9) Uani 1 1 d . . . . .
H13A H 0.267665 0.758882 -0.008752 0.050 Uiso 1 1 calc R U . . .
H13B H 0.323961 0.854220 0.045017 0.050 Uiso 1 1 calc R U . . .
C21 C 0.2692(3) 0.4097(3) 0.2067(2) 0.0406(9) Uani 1 1 d . . . . .
H21A H 0.265283 0.379826 0.156521 0.049 Uiso 1 1 calc R U . . .
H21B H 0.288554 0.365666 0.244771 0.049 Uiso 1 1 calc R U . . .
C14 C 0.1605(3) 0.8086(3) 0.0406(2) 0.0419(9) Uani 1 1 d . . . . .
H14A H 0.160749 0.840005 0.089505 0.050 Uiso 1 1 calc R U . . .
H14B H 0.143806 0.851523 0.000806 0.050 Uiso 1 1 calc R U . . .
C7 C 0.8168(3) 0.7181(3) 1.2193(2) 0.0390(9) Uani 1 1 d . . . . .
C12 C 0.7228(3) 0.5445(3) 0.4623(2) 0.0364(8) Uani 1 1 d . . . . .
C16 C -0.1027(3) 0.6338(3) 0.0030(2) 0.0430(10) Uani 1 1 d . . . . .
H16A H -0.177024 0.640838 -0.008792 0.052 Uiso 1 1 calc R U . . .
H16B H -0.088506 0.601735 -0.041195 0.052 Uiso 1 1 calc R U . . .
C3 C 0.4920(3) 0.8283(2) 0.8790(2) 0.0290(7) Uani 1 1 d . . . . .
C22 C 0.3525(3) 0.5037(3) 0.2184(2) 0.0392(9) Uani 1 1 d . . . . .
H22A H 0.352293 0.535977 0.266843 0.047 Uiso 1 1 calc R U . . .
H22B H 0.424583 0.493127 0.219910 0.047 Uiso 1 1 calc R U . . .
C8 C 0.6650(3) 0.5793(3) 1.1401(2) 0.0326(8) Uani 1 1 d . . . . .
C11 C 0.7424(3) 0.5781(3) 0.5351(2) 0.0347(8) Uani 1 1 d . . . . .
C24 C 0.3882(3) 0.7045(3) 0.0956(2) 0.0409(9) Uani 1 1 d . . . . .
H24A H 0.449342 0.761345 0.094650 0.049 Uiso 1 1 calc R U . . .
H24B H 0.376967 0.663292 0.049364 0.049 Uiso 1 1 calc R U . . .
C23 C 0.4122(3) 0.6498(3) 0.1628(2) 0.0424(9) Uani 1 1 d . . . . .
H23A H 0.482481 0.635187 0.164645 0.051 Uiso 1 1 calc R U . . .
H23B H 0.416140 0.688842 0.208985 0.051 Uiso 1 1 calc R U . . .
C18 C -0.1442(3) 0.4275(3) 0.1198(3) 0.0481(11) Uani 1 1 d . . . . .
H18A H -0.160000 0.462644 0.161801 0.058 Uiso 1 1 calc R U . . .
H18B H -0.196299 0.363265 0.111585 0.058 Uiso 1 1 calc R U . . .
C6 C 1.0041(3) 1.0763(3) 1.2331(2) 0.0418(9) Uani 1 1 d . . . . .
C17 C -0.1555(3) 0.4815(3) 0.0505(3) 0.0461(10) Uani 1 1 d . . . . .
H17A H -0.132007 0.450338 0.010013 0.055 Uiso 1 1 calc R U . . .
H17B H -0.231834 0.481020 0.033605 0.055 Uiso 1 1 calc R U . . .
C1 C 0.3788(3) 0.7167(3) 0.7623(3) 0.0436(10) Uani 1 1 d . . . . .
O10 O 0.3055(7) 0.9292(5) 0.3076(4) 0.0440(18) Uani 0.561(7) 1 d . . P A 1
C15 C -0.0252(3) 0.7301(3) 0.0200(2) 0.0438(10) Uani 1 1 d . . . . .
H15A H -0.037408 0.772273 -0.021383 0.053 Uiso 1 1 calc R U . . .
H15B H -0.035157 0.760281 0.066547 0.053 Uiso 1 1 calc R U . . .
C10 C 0.9316(4) 0.6120(3) 0.4978(2) 0.0461(10) Uani 1 1 d . . . . .
C20 C 0.0837(4) 0.3378(3) 0.2053(3) 0.0492(11) Uani 1 1 d . . . . .
H20A H 0.096702 0.298789 0.248669 0.059 Uiso 1 1 calc R U . . .
H20B H 0.082173 0.299735 0.159150 0.059 Uiso 1 1 calc R U . . .
C19 C -0.0206(4) 0.3619(3) 0.2019(3) 0.0495(11) Uani 1 1 d . . . . .
H19A H -0.079863 0.302311 0.197359 0.059 Uiso 1 1 calc R U . . .
H19B H -0.019452 0.399475 0.248219 0.059 Uiso 1 1 calc R U . . .
O11 O 0.4856(6) 0.8880(5) 0.2609(4) 0.0467(16) Uani 0.561(7) 1 d . . P A 1
C38 C 0.7063(17) 0.8224(10) 0.4992(12) 0.066(5) Uani 0.561(7) 1 d . . P A 1
H38A H 0.743664 0.780898 0.530396 0.079 Uiso 0.561(7) 1 calc R U P A 1
H38B H 0.747356 0.890073 0.513004 0.079 Uiso 0.561(7) 1 calc R U P A 1
C39 C 0.5953(19) 0.8384(13) 0.5857(13) 0.066(7) Uani 0.561(7) 1 d . . P A 1
H39A H 0.620159 0.909483 0.591803 0.079 Uiso 0.561(7) 1 calc R U P A 1
H39B H 0.643324 0.812633 0.623495 0.079 Uiso 0.561(7) 1 calc R U P A 1
C37 C 0.7056(9) 0.8003(8) 0.4203(9) 0.066(4) Uani 0.561(7) 1 d . . P A 1
H37A H 0.780758 0.813619 0.412297 0.080 Uiso 0.561(7) 1 calc R U P A 1
H37B H 0.671455 0.730835 0.408033 0.080 Uiso 0.561(7) 1 calc R U P A 1
C40 C 0.4877(9) 0.8085(7) 0.6009(5) 0.063(3) Uani 0.561(7) 1 d . . P A 1
H40A H 0.457264 0.738575 0.588850 0.076 Uiso 0.561(7) 1 calc R U P A 1
H40B H 0.488064 0.822344 0.654455 0.076 Uiso 0.561(7) 1 calc R U P A 1
C35 C 0.5958(15) 0.9153(13) 0.2550(11) 0.068(5) Uani 0.561(7) 1 d . . P A 1
H35A H 0.629348 0.982102 0.276034 0.081 Uiso 0.561(7) 1 calc R U P A 1
H35B H 0.602825 0.912199 0.201719 0.081 Uiso 0.561(7) 1 calc R U P A 1
O9 O 0.2518(6) 0.8733(5) 0.4466(4) 0.0447(17) Uani 0.561(7) 1 d . . P A 1
C32 C 0.1974(12) 0.9016(10) 0.3199(8) 0.044(3) Uani 0.561(7) 1 d . . P A 1
H32A H 0.167063 0.831549 0.308555 0.053 Uiso 0.561(7) 1 calc R U P A 1
H32B H 0.152829 0.935311 0.286177 0.053 Uiso 0.561(7) 1 calc R U P A 1
C36 C 0.6513(9) 0.8475(9) 0.2977(8) 0.064(3) Uani 0.561(7) 1 d . . P A 1
H36A H 0.615117 0.780945 0.276973 0.077 Uiso 0.561(7) 1 calc R U P A 1
H36B H 0.726621 0.862383 0.289666 0.077 Uiso 0.561(7) 1 calc R U P A 1
C34 C 0.4270(10) 0.9499(9) 0.2213(6) 0.046(3) Uani 0.561(7) 1 d . . P A 1
H34A H 0.430948 0.946431 0.167455 0.056 Uiso 0.561(7) 1 calc R U P A 1
H34B H 0.459276 1.017339 0.241292 0.056 Uiso 0.561(7) 1 calc R U P A 1
C29 C 0.3184(9) 0.8407(7) 0.5696(5) 0.063(3) Uani 0.561(7) 1 d . . P A 1
H29A H 0.320288 0.856100 0.623166 0.076 Uiso 0.561(7) 1 calc R U P A 1
H29B H 0.282058 0.771530 0.558067 0.076 Uiso 0.561(7) 1 calc R U P A 1
C30 C 0.2585(12) 0.8990(9) 0.5226(7) 0.049(3) Uani 0.561(7) 1 d . . P A 1
H30A H 0.185275 0.887951 0.534125 0.059 Uiso 0.561(7) 1 calc R U P A 1
H30B H 0.295732 0.968098 0.533400 0.059 Uiso 0.561(7) 1 calc R U P A 1
C29A C 0.3292(10) 0.9110(7) 0.5501(6) 0.039(3) Uani 0.439(7) 1 d . . P A 2
H29C H 0.365054 0.980713 0.554364 0.047 Uiso 0.439(7) 1 calc R U P A 2
H29D H 0.302926 0.893102 0.597125 0.047 Uiso 0.439(7) 1 calc R U P A 2
O12A O 0.6605(18) 0.8494(16) 0.3823(11) 0.039(4) Uani 0.439(7) 1 d . . P A 2
C37A C 0.7423(8) 0.8382(8) 0.4458(7) 0.034(2) Uani 0.439(7) 1 d . . P A 2
H37C H 0.791422 0.901784 0.464311 0.041 Uiso 0.439(7) 1 calc R U P A 2
H37D H 0.785385 0.797167 0.429546 0.041 Uiso 0.439(7) 1 calc R U P A 2
C36A C 0.7101(9) 0.8978(7) 0.3248(6) 0.042(2) Uani 0.439(7) 1 d . . P A 2
H36C H 0.767911 0.869539 0.314415 0.050 Uiso 0.439(7) 1 calc R U P A 2
H36D H 0.741714 0.966891 0.339901 0.050 Uiso 0.439(7) 1 calc R U P A 2
C38A C 0.6870(17) 0.7926(11) 0.5073(13) 0.038(4) Uani 0.439(7) 1 d . . P A 2
H38C H 0.644635 0.725799 0.491543 0.046 Uiso 0.439(7) 1 calc R U P A 2
H38D H 0.740296 0.791863 0.553136 0.046 Uiso 0.439(7) 1 calc R U P A 2
C35A C 0.6237(17) 0.8851(13) 0.2575(11) 0.046(4) Uani 0.439(7) 1 d . . P A 2
H35C H 0.654430 0.914197 0.214545 0.055 Uiso 0.439(7) 1 calc R U P A 2
H35D H 0.590346 0.815803 0.244210 0.055 Uiso 0.439(7) 1 calc R U P A 2
O13A O 0.6165(8) 0.8522(5) 0.5208(6) 0.034(2) Uani 0.439(7) 1 d . . P A 2
O11A O 0.5451(9) 0.9303(7) 0.2733(4) 0.043(2) Uani 0.439(7) 1 d . . P A 2
C39A C 0.574(2) 0.8176(14) 0.5889(14) 0.037(4) Uani 0.439(7) 1 d . . P A 2
H39C H 0.632258 0.827278 0.633379 0.044 Uiso 0.439(7) 1 calc R U P A 2
H39D H 0.534151 0.748692 0.581930 0.044 Uiso 0.439(7) 1 calc R U P A 2
C34A C 0.4683(14) 0.9295(11) 0.2087(9) 0.050(4) Uani 0.439(7) 1 d . . P A 2
H34C H 0.436981 0.862729 0.187074 0.061 Uiso 0.439(7) 1 calc R U P A 2
H34D H 0.503399 0.968022 0.170979 0.061 Uiso 0.439(7) 1 calc R U P A 2
C40A C 0.4979(8) 0.8818(6) 0.5962(5) 0.035(2) Uani 0.439(7) 1 d . . P A 2
H40C H 0.474880 0.874167 0.645266 0.042 Uiso 0.439(7) 1 calc R U P A 2
H40D H 0.536711 0.950014 0.593734 0.042 Uiso 0.439(7) 1 calc R U P A 2
O8A O 0.4044(14) 0.8561(16) 0.5368(10) 0.027(3) Uani 0.439(7) 1 d . . P A 2
O10A O 0.3237(7) 0.9128(6) 0.2766(7) 0.040(2) Uani 0.439(7) 1 d . . P A 2
C30A C 0.2361(11) 0.8871(10) 0.4839(11) 0.044(4) Uani 0.439(7) 1 d . . P A 2
H30C H 0.205013 0.816666 0.476883 0.053 Uiso 0.439(7) 1 calc R U P A 2
H30D H 0.179048 0.917074 0.493257 0.053 Uiso 0.439(7) 1 calc R U P A 2
C32A C 0.2330(11) 0.9421(9) 0.2897(7) 0.049(3) Uani 0.439(7) 1 d . . P A 2
H32C H 0.175575 0.925077 0.244569 0.059 Uiso 0.439(7) 1 calc R U P A 2
H32D H 0.252956 1.012819 0.299285 0.059 Uiso 0.439(7) 1 calc R U P A 2
O9A O 0.2736(5) 0.9218(5) 0.4203(4) 0.0382(18) Uani 0.439(7) 1 d . . P A 2
C33 C 0.3136(9) 0.9190(7) 0.2306(6) 0.047(2) Uani 0.561(7) 1 d . . P A 1
H33A H 0.271814 0.958254 0.200581 0.056 Uiso 0.561(7) 1 calc R U P A 1
H33B H 0.282484 0.850921 0.212059 0.056 Uiso 0.561(7) 1 calc R U P A 1
C31 C 0.1949(8) 0.9258(7) 0.3975(6) 0.048(2) Uani 0.561(7) 1 d . . P A 1
H31A H 0.227607 0.995509 0.409207 0.058 Uiso 0.561(7) 1 calc R U P A 1
H31B H 0.119296 0.911065 0.404742 0.058 Uiso 0.561(7) 1 calc R U P A 1
C31A C 0.1912(14) 0.8948(14) 0.3556(10) 0.048(4) Uani 0.439(7) 1 d . . P A 2
H31C H 0.127094 0.915371 0.363412 0.057 Uiso 0.439(7) 1 calc R U P A 2
H31D H 0.169995 0.824055 0.346194 0.057 Uiso 0.439(7) 1 calc R U P A 2
C33A C 0.3809(13) 0.9703(11) 0.2272(8) 0.048(3) Uani 0.439(7) 1 d . . P A 2
H33C H 0.412771 1.036238 0.250547 0.058 Uiso 0.439(7) 1 calc R U P A 2
H33D H 0.330569 0.974299 0.180518 0.058 Uiso 0.439(7) 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 S4 2.1532(9) . ?
Ni1 S6 2.1626(10) . ?
Ni1 S5 2.1710(10) . ?
Ni1 S7 2.1585(9) . ?
Ni2 S15 2.1607(9) 2_667 ?
Ni2 S15 2.1607(9) . ?
Ni2 S14 2.1670(9) 2_667 ?
Ni2 S14 2.1670(9) . ?
Ni3 S20 2.1610(10) . ?
Ni3 S20 2.1610(10) 2_666 ?
Ni3 S19 2.1594(10) 2_666 ?
Ni3 S19 2.1594(10) . ?
S4 C3 1.715(4) . ?
S6 C5 1.716(4) . ?
S5 C2 1.715(4) . ?
S7 C4 1.725(4) . ?
S15 C9 1.726(4) . ?
S14 C8 1.716(4) . ?
S13 C9 1.743(4) . ?
S13 C7 1.735(4) . ?
S2 C3 1.736(4) . ?
S2 C1 1.741(4) . ?
S9 C4 1.742(4) . ?
S9 C6 1.736(5) . ?
S20 C12 1.719(4) . ?
S19 C11 1.721(4) . ?
S17 C11 1.740(4) . ?
S17 C10 1.740(4) . ?
S12 C7 1.739(4) . ?
S12 C8 1.758(4) . ?
S8 C5 1.746(4) . ?
S8 C6 1.735(4) . ?
S11 C7 1.645(4) . ?
S3 C2 1.749(4) . ?
S3 C1 1.745(4) . ?
S18 C12 1.748(4) . ?
S18 C10 1.730(4) . ?
S10 C6 1.645(4) . ?
S1 C1 1.628(4) . ?
S16 C10 1.636(5) . ?
O7 C26 1.417(4) . ?
O7 C27 1.428(5) . ?
O5 C14 1.427(5) . ?
O5 C15 1.425(4) . ?
O4 C13 1.421(5) . ?
O4 C24 1.428(4) . ?
O6 C16 1.428(5) . ?
O6 C17 1.409(5) . ?
O2 C21 1.418(5) . ?
O2 C20 1.435(5) . ?
O1 C18 1.435(5) . ?
O1 C19 1.428(5) . ?
O3 C22 1.435(5) . ?
O3 C23 1.416(5) . ?
N1 C25 1.488(4) . ?
O12 C37 1.37(2) . ?
O12 C36 1.36(2) . ?
N2 C28 1.486(4) . ?
O8 C40 1.42(2) . ?
O8 C29 1.424(18) . ?
O13 C38 1.36(2) . ?
O13 C39 1.40(2) . ?
C26 C25 1.497(6) . ?
C9 C8 1.357(5) . ?
C5 C4 1.364(5) . ?
C27 C28 1.495(6) . ?
C2 C3 1.365(5) . ?
C13 C14 1.497(6) . ?
C21 C22 1.490(6) . ?
C12 C11 1.361(5) . ?
C16 C15 1.485(6) . ?
C24 C23 1.494(6) . ?
C18 C17 1.495(7) . ?
O10 C32 1.426(17) . ?
O10 C33 1.430(11) . ?
C20 C19 1.484(6) . ?
O11 C35 1.418(18) . ?
O11 C34 1.441(14) . ?
C38 C37 1.46(2) . ?
C39 C40 1.44(2) . ?
C35 C36 1.508(19) . ?
O9 C30 1.407(12) . ?
O9 C31 1.414(11) . ?
C32 C31 1.455(15) . ?
C34 C33 1.478(15) . ?
C29 C30 1.473(16) . ?
C29A O8A 1.459(19) . ?
C29A C30A 1.519(19) . ?
O12A C37A 1.47(2) . ?
O12A C36A 1.42(2) . ?
C37A C38A 1.506(19) . ?
C36A C35A 1.49(2) . ?
C38A O13A 1.459(18) . ?
C35A O11A 1.42(2) . ?
O13A C39A 1.49(2) . ?
O11A C34A 1.402(18) . ?
C39A C40A 1.54(2) . ?
C34A C33A 1.498(18) . ?
C40A O8A 1.445(19) . ?
O10A C32A 1.413(14) . ?
O10A C33A 1.412(19) . ?
C30A O9A 1.385(18) . ?
C32A C31A 1.50(2) . ?
O9A C31A 1.421(17) . ?

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 S6 85.60(4) . . ?
S4 Ni1 S5 93.35(4) . . ?
S4 Ni1 S7 178.67(4) . . ?
S6 Ni1 S5 177.31(4) . . ?
S7 Ni1 S6 93.20(4) . . ?
S7 Ni1 S5 87.83(4) . . ?
S15 Ni2 S15 180.0 . 2_667 ?
S15 Ni2 S14 93.34(4) . . ?
S15 Ni2 S14 86.66(4) 2_667 . ?
S15 Ni2 S14 93.34(4) 2_667 2_667 ?
S15 Ni2 S14 86.66(4) . 2_667 ?
S14 Ni2 S14 180.0 2_667 . ?
S20 Ni3 S20 180.00(4) . 2_666 ?
S19 Ni3 S20 86.41(4) . 2_666 ?
S19 Ni3 S20 86.41(4) 2_666 . ?
S19 Ni3 S20 93.59(4) . . ?
S19 Ni3 S20 93.59(4) 2_666 2_666 ?
S19 Ni3 S19 180.0 2_666 . ?
C3 S4 Ni1 102.35(12) . . ?
C5 S6 Ni1 102.07(13) . . ?
C2 S5 Ni1 101.65(12) . . ?
C4 S7 Ni1 102.31(13) . . ?
C9 S15 Ni2 102.13(13) . . ?
C8 S14 Ni2 101.83(13) . . ?
C7 S13 C9 97.48(19) . . ?
C3 S2 C1 97.72(18) . . ?
C6 S9 C4 97.65(19) . . ?
C12 S20 Ni3 101.75(14) . . ?
C11 S19 Ni3 101.98(14) . . ?
C11 S17 C10 97.2(2) . . ?
C7 S12 C8 97.25(19) . . ?
C6 S8 C5 97.43(19) . . ?
C1 S3 C2 97.81(18) . . ?
C10 S18 C12 97.4(2) . . ?
C26 O7 C27 111.3(3) . . ?
C15 O5 C14 111.9(3) . . ?
C13 O4 C24 111.8(3) . . ?
C17 O6 C16 112.0(3) . . ?
C21 O2 C20 112.9(3) . . ?
C19 O1 C18 113.2(3) . . ?
C23 O3 C22 111.6(3) . . ?
C36 O12 C37 121.4(13) . . ?
C40 O8 C29 111.6(14) . . ?
C38 O13 C39 118.2(14) . . ?
O7 C26 C25 108.5(3) . . ?
S15 C9 S13 122.7(2) . . ?
C8 C9 S15 120.8(3) . . ?
C8 C9 S13 116.5(3) . . ?
S6 C5 S8 122.4(2) . . ?
C4 C5 S6 121.5(3) . . ?
C4 C5 S8 116.1(3) . . ?
O7 C27 C28 109.1(3) . . ?
N1 C25 C26 113.0(3) . . ?
N2 C28 C27 112.4(3) . . ?
S7 C4 S9 123.5(2) . . ?
C5 C4 S7 120.6(3) . . ?
C5 C4 S9 115.9(3) . . ?
S5 C2 S3 123.1(2) . . ?
C3 C2 S5 121.5(3) . . ?
C3 C2 S3 115.4(3) . . ?
O4 C13 C14 108.9(3) . . ?
O2 C21 C22 109.0(3) . . ?
O5 C14 C13 109.0(3) . . ?
S13 C7 S12 113.0(2) . . ?
S11 C7 S13 123.3(2) . . ?
S11 C7 S12 123.7(3) . . ?
S20 C12 S18 122.5(2) . . ?
C11 C12 S20 121.6(3) . . ?
C11 C12 S18 115.8(3) . . ?
O6 C16 C15 109.6(3) . . ?
S4 C3 S2 122.3(2) . . ?
C2 C3 S4 121.0(3) . . ?
C2 C3 S2 116.7(3) . . ?
O3 C22 C21 109.3(3) . . ?
S14 C8 S12 122.5(2) . . ?
C9 C8 S14 121.9(3) . . ?
C9 C8 S12 115.7(3) . . ?
S19 C11 S17 122.5(2) . . ?
C12 C11 S19 121.0(3) . . ?
C12 C11 S17 116.4(3) . . ?
O4 C24 C23 108.4(3) . . ?
O3 C23 C24 109.0(3) . . ?
O1 C18 C17 109.6(3) . . ?
S8 C6 S9 112.9(2) . . ?
S10 C6 S9 124.5(3) . . ?
S10 C6 S8 122.6(3) . . ?
O6 C17 C18 109.1(3) . . ?
S2 C1 S3 112.3(2) . . ?
S1 C1 S2 122.7(2) . . ?
S1 C1 S3 125.0(2) . . ?
C32 O10 C33 113.3(9) . . ?
O5 C15 C16 108.4(3) . . ?
S18 C10 S17 113.2(2) . . ?
S16 C10 S17 123.1(3) . . ?
S16 C10 S18 123.7(3) . . ?
O2 C20 C19 108.9(3) . . ?
O1 C19 C20 108.1(3) . . ?
C35 O11 C34 111.7(11) . . ?
O13 C38 C37 112.6(16) . . ?
O13 C39 C40 114.6(17) . . ?
O12 C37 C38 113.2(12) . . ?
O8 C40 C39 107.2(13) . . ?
O11 C35 C36 108.6(13) . . ?
C30 O9 C31 113.1(9) . . ?
O10 C32 C31 109.9(12) . . ?
O12 C36 C35 113.9(12) . . ?
O11 C34 C33 109.1(8) . . ?
O8 C29 C30 109.2(11) . . ?
O9 C30 C29 109.4(9) . . ?
O8A C29A C30A 107.2(11) . . ?
C36A O12A C37A 110.6(16) . . ?
O12A C37A C38A 109.0(14) . . ?
O12A C36A C35A 106.2(14) . . ?
O13A C38A C37A 105.4(12) . . ?
O11A C35A C36A 108.9(14) . . ?
C38A O13A C39A 106.2(12) . . ?
C34A O11A C35A 110.7(12) . . ?
O13A C39A C40A 101.9(14) . . ?
O11A C34A C33A 110.3(14) . . ?
O8A C40A C39A 110.6(14) . . ?
C40A O8A C29A 108.9(13) . . ?
C33A O10A C32A 113.5(10) . . ?
O9A C30A C29A 108.8(10) . . ?
O10A C32A C31A 111.1(11) . . ?
C30A O9A C31A 111.0(12) . . ?
O10 C33 C34 110.8(9) . . ?
O9 C31 C32 110.7(9) . . ?
O9A C31A C32A 108.7(13) . . ?
O10A C33A C34A 111.1(13) . . ?

_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 2.830
_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_18c6_nc2oc2n_lt_03_123_00_autored
_database_code_depnum_ccdc_archive 'CCDC 2384650'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2024-09-17 deposited with the CCDC.	2024-11-08 downloaded from the CCDC.
;
_audit_creation_date             2023-12-22
_audit_creation_method           
;
Olex2 1.5-ac5-023
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C6 Ni S10), C4 H14 N2 O, 2(C12 H24 O6)'
_chemical_formula_sum            'C40 H62 N2 Ni2 O13 S20'
_chemical_formula_weight         1537.53
_chemical_melting_point          ?
_chemical_oxdiff_formula         C40H62N2Ni2O13S20
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                   13.0913(3)
_cell_length_b                   14.4264(3)
_cell_length_c                   18.1799(4)
_cell_angle_alpha                90.747(2)
_cell_angle_beta                 100.171(2)
_cell_angle_gamma                104.861(2)
_cell_volume                     3260.32(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    17215
_cell_measurement_temperature    123.00(14)
_cell_measurement_theta_max      30.9350
_cell_measurement_theta_min      2.0260
_shelx_estimated_absorpt_T_max   0.873
_shelx_estimated_absorpt_T_min   0.478
_exptl_absorpt_coefficient_mu    1.272
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29512
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.67a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark black'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-17 0 11 0.1850
1 -20 3 0.2424
17 0 -11 0.3121
0 20 -3 0.2620
-1 0 -25 0.0384
0 1 25 0.0332

_exptl_crystal_size_max          0.679
_exptl_crystal_size_mid          0.508
_exptl_crystal_size_min          0.108
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-17.2533 0.2325 11.2751 -0.1592 0.5392 0.8270
0.6149 -19.7989 2.6003 -0.2642 0.8911 -0.3689
17.1178 0.3514 -11.2748 0.1659 -0.5617 -0.8105
-0.1023 19.6570 -2.9148 0.2671 -0.9009 0.3420
-1.4622 0.1708 -24.7218 0.9710 0.1801 -0.1571
0.0434 0.7994 25.0845 -0.9551 -0.1772 0.2377

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.789
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            43134
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.789
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.941
_diffrn_reflns_theta_min         2.163
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(14)
_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 0.789
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -17.00  28.00   0.50    1.46    --   -5.80 -99.00   0.00   90
  2  ω    -77.00   4.00   0.50    1.46    --   -5.80 -37.00 -90.00  162
  3  ω    -75.00 -43.00   0.50    1.46    --   -5.80 -57.00  30.00   64
  4  ω    -38.00   3.00   0.50    1.46    --   -5.80 -57.00  30.00   82
  5  ω    -15.00  68.00   0.50    1.46    --   -5.80  37.00-150.00  166
  6  ω    -67.00   7.00   0.50    1.46    --   -5.80 -37.00  30.00  148
  7  ω    -11.00  35.00   0.50    1.46    --    6.03 -99.00-150.00   92
;
_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      -0.0156952000
_diffrn_orient_matrix_UB_12      0.0078259000
_diffrn_orient_matrix_UB_13      -0.0382959000
_diffrn_orient_matrix_UB_21      -0.0354806000
_diffrn_orient_matrix_UB_22      -0.0468341000
_diffrn_orient_matrix_UB_23      -0.0055086000
_diffrn_orient_matrix_UB_31      -0.0418317000
_diffrn_orient_matrix_UB_32      0.0185112000
_diffrn_orient_matrix_UB_33      0.0089566000
_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                10986
_reflns_number_total             16308
_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 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.049
_refine_diff_density_min         -1.133
_refine_diff_density_rms         0.097
_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     862
_refine_ls_number_reflns         16308
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0523
_refine_ls_restrained_S_all      1.019
_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)+(0.0584P)²+5.0773P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1223
_refine_ls_wR_factor_ref         0.1410
_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. Others
 Sof(C29A)=Sof(H29C)=Sof(H29D)=Sof(O12A)=Sof(C37A)=Sof(H37C)=Sof(H37D)=
 Sof(C36A)=Sof(H36C)=Sof(H36D)=Sof(C38A)=Sof(H38C)=Sof(H38D)=Sof(C35A)=
 Sof(H35C)=Sof(H35D)=Sof(O13A)=Sof(O11A)=Sof(C39A)=Sof(H39C)=Sof(H39D)=
 Sof(C34A)=Sof(H34C)=Sof(H34D)=Sof(C40A)=Sof(H40C)=Sof(H40D)=Sof(O8A)=Sof(O10A)=
 Sof(C30A)=Sof(H30C)=Sof(H30D)=Sof(C32A)=Sof(H32C)=Sof(H32D)=Sof(O9A)=Sof(C31A)=
 Sof(H31C)=Sof(H31D)=Sof(C33A)=Sof(H33C)=Sof(H33D)=1-FVAR(1)
 Sof(O12)=Sof(O8)=Sof(O13)=Sof(O10)=Sof(O11)=Sof(C38)=Sof(H38A)=Sof(H38B)=
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C40)=Sof(H40A)=
 Sof(H40B)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(O9)=Sof(C32)=Sof(H32A)=Sof(H32B)=
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(C29)=Sof(H29A)=
 Sof(H29B)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C31)=
 Sof(H31A)=Sof(H31B)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C27(H27A,H27B), C25(H25A,H25B), C28(H28A,H28B), C13(H13A,
 H13B), C21(H21A,H21B), C14(H14A,H14B), C16(H16A,H16B), C22(H22A,H22B),
 C24(H24A,H24B), C23(H23A,H23B), C18(H18A,H18B), C17(H17A,H17B), C15(H15A,H15B),
  C20(H20A,H20B), C19(H19A,H19B), C38(H38A,H38B), C39(H39A,H39B), C37(H37A,
 H37B), C40(H40A,H40B), C35(H35A,H35B), C32(H32A,H32B), C36(H36A,H36B),
 C34(H34A,H34B), C29(H29A,H29B), C30(H30A,H30B), C29A(H29C,H29D), C37A(H37C,
 H37D), C36A(H36C,H36D), C38A(H38C,H38D), C35A(H35C,H35D), C39A(H39C,H39D),
 C34A(H34C,H34D), C40A(H40C,H40D), C30A(H30C,H30D), C32A(H32C,H32D), C33(H33A,
 H33B), C31(H31A,H31B), C31A(H31C,H31D), C33A(H33C,H33D)
3.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(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 0.70134(3) 0.92138(3) 0.98424(3) 0.02778(11) Uani 1 1 d . . . . .
Ni2 Ni 0.500000 0.500000 1.000000 0.03019(15) Uani 1 2 d S . P . .
Ni3 Ni 0.500000 0.500000 0.500000 0.03484(16) Uani 1 2 d S . P . .
S4 S 0.53012(7) 0.90270(6) 0.95899(5) 0.03039(19) Uani 1 1 d . . . . .
S6 S 0.69757(7) 1.00114(7) 1.08481(5) 0.0341(2) Uani 1 1 d . . . . .
S5 S 0.70097(7) 0.83527(6) 0.88529(6) 0.0336(2) Uani 1 1 d . . . . .
S7 S 0.87301(7) 0.94066(7) 1.01216(6) 0.0336(2) Uani 1 1 d . . . . .
S15 S 0.59515(7) 0.64755(7) 1.00910(6) 0.0351(2) Uani 1 1 d . . . . .
S14 S 0.57654(7) 0.47011(7) 1.10955(6) 0.0353(2) Uani 1 1 d . . . . .
S13 S 0.76703(8) 0.76227(7) 1.13581(6) 0.0406(2) Uani 1 1 d . . . . .
S2 S 0.35924(7) 0.78930(7) 0.83321(6) 0.0360(2) Uani 1 1 d . . . . .
S9 S 1.03396(8) 1.02708(7) 1.15440(6) 0.0431(2) Uani 1 1 d . . . . .
S20 S 0.59398(8) 0.49475(8) 0.41433(6) 0.0427(2) Uani 1 1 d . . . . .
S19 S 0.63875(9) 0.56973(7) 0.58341(6) 0.0411(2) Uani 1 1 d . . . . .
S17 S 0.87635(9) 0.62697(8) 0.57610(6) 0.0443(2) Uani 1 1 d . . . . .
S12 S 0.75002(8) 0.59903(8) 1.22832(6) 0.0414(2) Uani 1 1 d . . . . .
S8 S 0.87035(9) 1.07951(7) 1.22153(6) 0.0449(2) Uani 1 1 d . . . . .
S11 S 0.91548(9) 0.78247(9) 1.28261(7) 0.0532(3) Uani 1 1 d . . . . .
S3 S 0.51412(8) 0.71934(8) 0.76827(7) 0.0441(3) Uani 1 1 d . . . . .
S18 S 0.83559(9) 0.55885(10) 0.42035(6) 0.0528(3) Uani 1 1 d . . . . .
S10 S 1.09131(11) 1.11733(8) 1.31052(8) 0.0617(4) Uani 1 1 d . . . . .
S1 S 0.28054(10) 0.65384(11) 0.69946(9) 0.0724(4) Uani 1 1 d . . . . .
S16 S 1.06060(11) 0.64350(13) 0.49804(8) 0.0766(4) Uani 1 1 d . . . . .
O7 O 0.2428(2) 0.67570(17) 0.30629(14) 0.0329(5) Uani 1 1 d . . . . .
O5 O 0.0807(2) 0.71834(18) 0.02878(15) 0.0376(6) Uani 1 1 d . . . . .
O4 O 0.2928(2) 0.73452(18) 0.09942(15) 0.0369(6) Uani 1 1 d . . . . .
O6 O -0.0918(2) 0.5766(2) 0.06628(16) 0.0431(7) Uani 1 1 d . . . . .
O2 O 0.1685(2) 0.42548(17) 0.21249(16) 0.0401(6) Uani 1 1 d . . . . .
O1 O -0.0364(2) 0.41694(18) 0.13855(16) 0.0428(7) Uani 1 1 d . . . . .
O3 O 0.3295(2) 0.56328(19) 0.15845(15) 0.0377(6) Uani 1 1 d . . . . .
N1 N 0.1205(2) 0.60061(19) 0.15452(17) 0.0292(6) Uani 1 1 d . . . . .
H1A H 0.103219 0.624822 0.109416 0.035 Uiso 1 1 calc R U . . .
H1B H 0.086754 0.536810 0.152204 0.035 Uiso 1 1 calc R U . . .
H1C H 0.192973 0.609000 0.166018 0.035 Uiso 1 1 calc R U . . .
O12 O 0.6516(16) 0.8529(14) 0.3723(10) 0.068(6) Uani 0.554(7) 1 d . . P A 1
N2 N 0.4323(3) 0.8157(2) 0.39510(18) 0.0357(7) Uani 1 1 d . . . . .
H2A H 0.394252 0.833450 0.353271 0.043 Uiso 1 1 calc R U . . .
H2B H 0.503881 0.840731 0.396379 0.043 Uiso 1 1 calc R U . . .
H2C H 0.413700 0.838240 0.436445 0.043 Uiso 1 1 calc R U . . .
O8 O 0.4254(16) 0.8600(15) 0.5548(11) 0.053(5) Uani 0.554(7) 1 d . . P A 1
O13 O 0.6043(7) 0.8089(6) 0.5131(5) 0.049(2) Uani 0.554(7) 1 d . . P A 1
C26 C 0.1309(3) 0.6314(3) 0.2912(2) 0.0364(8) Uani 1 1 d . . . . .
H26A H 0.095538 0.657111 0.327628 0.044 Uiso 1 1 calc R U . . .
H26B H 0.117706 0.561191 0.295840 0.044 Uiso 1 1 calc R U . . .
C9 C 0.6728(3) 0.6565(3) 1.0973(2) 0.0338(8) Uani 1 1 d . . . . .
C5 C 0.8283(3) 1.0243(3) 1.1314(2) 0.0349(8) Uani 1 1 d . . . . .
C27 C 0.2896(3) 0.6626(3) 0.3811(2) 0.0396(9) Uani 1 1 d . . . . .
H27A H 0.276660 0.593163 0.389206 0.048 Uiso 1 1 calc R U . . .
H27B H 0.256274 0.691857 0.416860 0.048 Uiso 1 1 calc R U . . .
C25 C 0.0856(3) 0.6516(3) 0.2132(2) 0.0400(9) Uani 1 1 d . . . . .
H25A H 0.006116 0.632169 0.205802 0.048 Uiso 1 1 calc R U . . .
H25B H 0.108380 0.721653 0.207415 0.048 Uiso 1 1 calc R U . . .
C28 C 0.4077(3) 0.7088(3) 0.3938(2) 0.0396(9) Uani 1 1 d . . . . .
H28A H 0.442170 0.689700 0.442073 0.048 Uiso 1 1 calc R U . . .
H28B H 0.438556 0.685428 0.353601 0.048 Uiso 1 1 calc R U . . .
C4 C 0.9051(3) 0.9986(3) 1.0999(2) 0.0354(8) Uani 1 1 d . . . . .
C2 C 0.5663(3) 0.7978(2) 0.8481(2) 0.0318(8) Uani 1 1 d . . . . .
C13 C 0.2679(4) 0.7916(3) 0.0396(3) 0.0456(10) Uani 1 1 d . . . . .
H13A H 0.267253 0.758504 -0.008579 0.055 Uiso 1 1 calc R U . . .
H13B H 0.323282 0.853845 0.045036 0.055 Uiso 1 1 calc R U . . .
C21 C 0.2695(4) 0.4101(3) 0.2067(2) 0.0455(10) Uani 1 1 d . . . . .
H21A H 0.265657 0.380188 0.156595 0.055 Uiso 1 1 calc R U . . .
H21B H 0.288901 0.366094 0.244841 0.055 Uiso 1 1 calc R U . . .
C14 C 0.1600(4) 0.8083(3) 0.0404(3) 0.0452(10) Uani 1 1 d . . . . .
H14A H 0.160154 0.839921 0.089072 0.054 Uiso 1 1 calc R U . . .
H14B H 0.143426 0.850950 0.000341 0.054 Uiso 1 1 calc R U . . .
C7 C 0.8167(3) 0.7182(3) 1.2194(2) 0.0412(9) Uani 1 1 d . . . . .
C12 C 0.7228(3) 0.5446(3) 0.4623(2) 0.0379(9) Uani 1 1 d . . . . .
C16 C -0.1028(3) 0.6335(3) 0.0031(2) 0.0465(10) Uani 1 1 d . . . . .
H16A H -0.177131 0.640302 -0.008801 0.056 Uiso 1 1 calc R U . . .
H16B H -0.088391 0.601424 -0.041020 0.056 Uiso 1 1 calc R U . . .
C3 C 0.4922(3) 0.8285(2) 0.8793(2) 0.0306(7) Uani 1 1 d . . . . .
C22 C 0.3524(3) 0.5040(3) 0.2184(2) 0.0422(9) Uani 1 1 d . . . . .
H22A H 0.352184 0.536214 0.266737 0.051 Uiso 1 1 calc R U . . .
H22B H 0.424592 0.493518 0.219890 0.051 Uiso 1 1 calc R U . . .
C8 C 0.6648(3) 0.5792(3) 1.1401(2) 0.0348(8) Uani 1 1 d . . . . .
C11 C 0.7424(3) 0.5782(3) 0.5352(2) 0.0369(8) Uani 1 1 d . . . . .
C24 C 0.3878(3) 0.7046(3) 0.0958(3) 0.0447(10) Uani 1 1 d . . . . .
H24A H 0.448846 0.761387 0.094905 0.054 Uiso 1 1 calc R U . . .
H24B H 0.376741 0.663420 0.049623 0.054 Uiso 1 1 calc R U . . .
C23 C 0.4119(3) 0.6499(3) 0.1630(3) 0.0461(10) Uani 1 1 d . . . . .
H23A H 0.482204 0.635410 0.164856 0.055 Uiso 1 1 calc R U . . .
H23B H 0.415594 0.688740 0.209131 0.055 Uiso 1 1 calc R U . . .
C18 C -0.1440(3) 0.4273(3) 0.1199(3) 0.0520(12) Uani 1 1 d . . . . .
H18A H -0.160021 0.462333 0.161825 0.062 Uiso 1 1 calc R U . . .
H18B H -0.196008 0.363157 0.111524 0.062 Uiso 1 1 calc R U . . .
C6 C 1.0039(3) 1.0763(3) 1.2332(3) 0.0443(10) Uani 1 1 d . . . . .
C17 C -0.1550(3) 0.4814(3) 0.0508(3) 0.0497(11) Uani 1 1 d . . . . .
H17A H -0.131236 0.450404 0.010404 0.060 Uiso 1 1 calc R U . . .
H17B H -0.231303 0.480823 0.033704 0.060 Uiso 1 1 calc R U . . .
C1 C 0.3791(3) 0.7168(3) 0.7625(3) 0.0454(10) Uani 1 1 d . . . . .
O10 O 0.3045(8) 0.9295(6) 0.3079(5) 0.047(2) Uani 0.554(7) 1 d . . P A 1
C15 C -0.0253(3) 0.7300(3) 0.0201(3) 0.0482(11) Uani 1 1 d . . . . .
H15A H -0.037648 0.772192 -0.021264 0.058 Uiso 1 1 calc R U . . .
H15B H -0.035281 0.760082 0.066659 0.058 Uiso 1 1 calc R U . . .
C10 C 0.9312(4) 0.6122(3) 0.4976(2) 0.0493(10) Uani 1 1 d . . . . .
C20 C 0.0841(4) 0.3379(3) 0.2050(3) 0.0513(11) Uani 1 1 d . . . . .
H20A H 0.097309 0.298654 0.248197 0.062 Uiso 1 1 calc R U . . .
H20B H 0.082476 0.300275 0.158734 0.062 Uiso 1 1 calc R U . . .
C19 C -0.0201(4) 0.3616(3) 0.2021(3) 0.0538(12) Uani 1 1 d . . . . .
H19A H -0.079233 0.301954 0.197424 0.065 Uiso 1 1 calc R U . . .
H19B H -0.019000 0.398917 0.248429 0.065 Uiso 1 1 calc R U . . .
O11 O 0.4841(6) 0.8880(5) 0.2607(4) 0.0489(17) Uani 0.554(7) 1 d . . P A 1
C38 C 0.706(2) 0.8231(12) 0.4986(14) 0.072(7) Uani 0.554(7) 1 d . . P A 1
H38A H 0.743599 0.782504 0.530426 0.086 Uiso 0.554(7) 1 calc R U P A 1
H38B H 0.745736 0.891057 0.511737 0.086 Uiso 0.554(7) 1 calc R U P A 1
C39 C 0.594(2) 0.8376(16) 0.5851(14) 0.071(8) Uani 0.554(7) 1 d . . P A 1
H39A H 0.620065 0.908548 0.591648 0.085 Uiso 0.554(7) 1 calc R U P A 1
H39B H 0.642363 0.811052 0.622422 0.085 Uiso 0.554(7) 1 calc R U P A 1
C37 C 0.7046(10) 0.7996(9) 0.4196(9) 0.070(4) Uani 0.554(7) 1 d . . P A 1
H37A H 0.779574 0.811696 0.411455 0.084 Uiso 0.554(7) 1 calc R U P A 1
H37B H 0.669079 0.730467 0.407512 0.084 Uiso 0.554(7) 1 calc R U P A 1
C40 C 0.4881(9) 0.8088(8) 0.6009(5) 0.066(3) Uani 0.554(7) 1 d . . P A 1
H40A H 0.457576 0.738707 0.589957 0.080 Uiso 0.554(7) 1 calc R U P A 1
H40B H 0.489196 0.823886 0.654379 0.080 Uiso 0.554(7) 1 calc R U P A 1
C35 C 0.5943(16) 0.9158(14) 0.2544(13) 0.074(6) Uani 0.554(7) 1 d . . P A 1
H35A H 0.627904 0.982350 0.275813 0.089 Uiso 0.554(7) 1 calc R U P A 1
H35B H 0.601061 0.913238 0.201073 0.089 Uiso 0.554(7) 1 calc R U P A 1
O9 O 0.2513(6) 0.8721(6) 0.4469(5) 0.0471(18) Uani 0.554(7) 1 d . . P A 1
C32 C 0.1966(12) 0.9015(11) 0.3203(8) 0.045(3) Uani 0.554(7) 1 d . . P A 1
H32A H 0.166577 0.831539 0.308709 0.054 Uiso 0.554(7) 1 calc R U P A 1
H32B H 0.151957 0.935223 0.286678 0.054 Uiso 0.554(7) 1 calc R U P A 1
C36 C 0.6497(9) 0.8468(9) 0.2968(8) 0.068(3) Uani 0.554(7) 1 d . . P A 1
H36A H 0.612000 0.780319 0.276793 0.081 Uiso 0.554(7) 1 calc R U P A 1
H36B H 0.724433 0.860383 0.288003 0.081 Uiso 0.554(7) 1 calc R U P A 1
C34 C 0.4251(12) 0.9495(9) 0.2213(6) 0.052(3) Uani 0.554(7) 1 d . . P A 1
H34A H 0.428635 0.945871 0.167451 0.062 Uiso 0.554(7) 1 calc R U P A 1
H34B H 0.457410 1.016910 0.241119 0.062 Uiso 0.554(7) 1 calc R U P A 1
C29 C 0.3178(9) 0.8401(7) 0.5691(5) 0.065(3) Uani 0.554(7) 1 d . . P A 1
H29A H 0.319874 0.855046 0.622697 0.079 Uiso 0.554(7) 1 calc R U P A 1
H29B H 0.281482 0.771052 0.557364 0.079 Uiso 0.554(7) 1 calc R U P A 1
C30 C 0.2570(14) 0.8986(10) 0.5227(7) 0.052(4) Uani 0.554(7) 1 d . . P A 1
H30A H 0.183717 0.886878 0.534029 0.062 Uiso 0.554(7) 1 calc R U P A 1
H30B H 0.293724 0.967718 0.533309 0.062 Uiso 0.554(7) 1 calc R U P A 1
C29A C 0.3294(11) 0.9106(8) 0.5505(7) 0.048(3) Uani 0.446(7) 1 d . . P A 2
H29C H 0.364486 0.980424 0.555064 0.058 Uiso 0.446(7) 1 calc R U P A 2
H29D H 0.302576 0.892241 0.597301 0.058 Uiso 0.446(7) 1 calc R U P A 2
O12A O 0.6595(18) 0.8487(16) 0.3814(9) 0.044(5) Uani 0.446(7) 1 d . . P A 2
C37A C 0.7417(9) 0.8378(9) 0.4450(8) 0.038(2) Uani 0.446(7) 1 d . . P A 2
H37C H 0.791055 0.901453 0.462942 0.046 Uiso 0.446(7) 1 calc R U P A 2
H37D H 0.784414 0.796447 0.428906 0.046 Uiso 0.446(7) 1 calc R U P A 2
C36A C 0.7091(10) 0.8969(8) 0.3246(6) 0.048(3) Uani 0.446(7) 1 d . . P A 2
H36C H 0.766571 0.868361 0.314093 0.058 Uiso 0.446(7) 1 calc R U P A 2
H36D H 0.741153 0.965814 0.340023 0.058 Uiso 0.446(7) 1 calc R U P A 2
C38A C 0.6878(19) 0.7938(13) 0.5066(15) 0.044(4) Uani 0.446(7) 1 d . . P A 2
H38C H 0.645616 0.726842 0.491371 0.053 Uiso 0.446(7) 1 calc R U P A 2
H38D H 0.741874 0.793320 0.552061 0.053 Uiso 0.446(7) 1 calc R U P A 2
C35A C 0.6227(18) 0.8852(14) 0.2572(13) 0.051(4) Uani 0.446(7) 1 d . . P A 2
H35C H 0.653435 0.915250 0.214519 0.061 Uiso 0.446(7) 1 calc R U P A 2
H35D H 0.589480 0.816090 0.243132 0.061 Uiso 0.446(7) 1 calc R U P A 2
O13A O 0.6178(8) 0.8521(6) 0.5210(6) 0.037(2) Uani 0.446(7) 1 d . . P A 2
O11A O 0.5445(11) 0.9295(7) 0.2736(5) 0.051(2) Uani 0.446(7) 1 d . . P A 2
C39A C 0.575(2) 0.8191(17) 0.5891(14) 0.041(5) Uani 0.446(7) 1 d . . P A 2
H39C H 0.633781 0.829674 0.633495 0.049 Uiso 0.446(7) 1 calc R U P A 2
H39D H 0.536211 0.750129 0.582839 0.049 Uiso 0.446(7) 1 calc R U P A 2
C34A C 0.4670(15) 0.9295(11) 0.2093(9) 0.056(4) Uani 0.446(7) 1 d . . P A 2
H34C H 0.434989 0.862878 0.187582 0.067 Uiso 0.446(7) 1 calc R U P A 2
H34D H 0.501784 0.967932 0.171480 0.067 Uiso 0.446(7) 1 calc R U P A 2
C40A C 0.4988(9) 0.8820(7) 0.5962(6) 0.042(2) Uani 0.446(7) 1 d . . P A 2
H40C H 0.476283 0.874059 0.645481 0.051 Uiso 0.446(7) 1 calc R U P A 2
H40D H 0.537171 0.950282 0.593908 0.051 Uiso 0.446(7) 1 calc R U P A 2
O8A O 0.4056(15) 0.8571(15) 0.5381(12) 0.030(3) Uani 0.446(7) 1 d . . P A 2
O10A O 0.3236(8) 0.9128(7) 0.2776(7) 0.046(2) Uani 0.446(7) 1 d . . P A 2
C30A C 0.2364(12) 0.8866(11) 0.4838(12) 0.054(5) Uani 0.446(7) 1 d . . P A 2
H30C H 0.205682 0.816145 0.476779 0.065 Uiso 0.446(7) 1 calc R U P A 2
H30D H 0.179137 0.916259 0.492892 0.065 Uiso 0.446(7) 1 calc R U P A 2
C32A C 0.2323(13) 0.9411(10) 0.2901(8) 0.058(4) Uani 0.446(7) 1 d . . P A 2
H32C H 0.174739 0.922516 0.245115 0.070 Uiso 0.446(7) 1 calc R U P A 2
H32D H 0.250969 1.011865 0.298590 0.070 Uiso 0.446(7) 1 calc R U P A 2
O9A O 0.2732(5) 0.9207(6) 0.4213(5) 0.0424(19) Uani 0.446(7) 1 d . . P A 2
C33 C 0.3113(9) 0.9187(7) 0.2310(6) 0.049(2) Uani 0.554(7) 1 d . . P A 1
H33A H 0.269441 0.957940 0.201044 0.059 Uiso 0.554(7) 1 calc R U P A 1
H33B H 0.280015 0.850618 0.212727 0.059 Uiso 0.554(7) 1 calc R U P A 1
C31 C 0.1933(8) 0.9248(7) 0.3976(7) 0.052(3) Uani 0.554(7) 1 d . . P A 1
H31A H 0.225195 0.994532 0.409640 0.062 Uiso 0.554(7) 1 calc R U P A 1
H31B H 0.117649 0.909197 0.404697 0.062 Uiso 0.554(7) 1 calc R U P A 1
C31A C 0.1917(14) 0.8947(14) 0.3569(10) 0.050(4) Uani 0.446(7) 1 d . . P A 2
H31C H 0.127955 0.915727 0.364818 0.060 Uiso 0.446(7) 1 calc R U P A 2
H31D H 0.169815 0.823983 0.347605 0.060 Uiso 0.446(7) 1 calc R U P A 2
C33A C 0.3809(15) 0.9706(12) 0.2284(9) 0.056(4) Uani 0.446(7) 1 d . . P A 2
H33C H 0.413497 1.036104 0.252175 0.067 Uiso 0.446(7) 1 calc R U P A 2
H33D H 0.330619 0.975434 0.181977 0.067 Uiso 0.446(7) 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 S4 2.1520(9) . ?
Ni1 S6 2.1622(10) . ?
Ni1 S5 2.1714(10) . ?
Ni1 S7 2.1584(10) . ?
Ni2 S15 2.1606(9) 2_667 ?
Ni2 S15 2.1606(9) . ?
Ni2 S14 2.1670(10) . ?
Ni2 S14 2.1670(10) 2_667 ?
Ni3 S20 2.1602(10) 2_666 ?
Ni3 S20 2.1602(10) . ?
Ni3 S19 2.1588(11) 2_666 ?
Ni3 S19 2.1589(11) . ?
S4 C3 1.710(4) . ?
S6 C5 1.716(4) . ?
S5 C2 1.714(4) . ?
S7 C4 1.723(4) . ?
S15 C9 1.724(4) . ?
S14 C8 1.714(4) . ?
S13 C9 1.745(4) . ?
S13 C7 1.739(4) . ?
S2 C3 1.737(4) . ?
S2 C1 1.743(4) . ?
S9 C4 1.744(4) . ?
S9 C6 1.739(5) . ?
S20 C12 1.721(4) . ?
S19 C11 1.721(4) . ?
S17 C11 1.736(4) . ?
S17 C10 1.740(5) . ?
S12 C7 1.742(4) . ?
S12 C8 1.759(4) . ?
S8 C5 1.744(4) . ?
S8 C6 1.737(4) . ?
S11 C7 1.638(4) . ?
S3 C2 1.751(4) . ?
S3 C1 1.743(4) . ?
S18 C12 1.747(4) . ?
S18 C10 1.729(5) . ?
S10 C6 1.643(4) . ?
S1 C1 1.629(4) . ?
S16 C10 1.637(5) . ?
O7 C26 1.416(4) . ?
O7 C27 1.425(5) . ?
O5 C14 1.426(5) . ?
O5 C15 1.422(4) . ?
O4 C13 1.414(5) . ?
O4 C24 1.429(4) . ?
O6 C16 1.428(5) . ?
O6 C17 1.405(5) . ?
O2 C21 1.417(5) . ?
O2 C20 1.436(5) . ?
O1 C18 1.437(5) . ?
O1 C19 1.428(5) . ?
O3 C22 1.431(5) . ?
O3 C23 1.416(5) . ?
N1 C25 1.488(4) . ?
O12 C37 1.37(2) . ?
O12 C36 1.37(2) . ?
N2 C28 1.491(4) . ?
O8 C40 1.42(2) . ?
O8 C29 1.434(19) . ?
O13 C38 1.36(2) . ?
O13 C39 1.41(2) . ?
C26 C25 1.499(6) . ?
C9 C8 1.360(5) . ?
C5 C4 1.367(5) . ?
C27 C28 1.492(6) . ?
C2 C3 1.367(5) . ?
C13 C14 1.495(6) . ?
C21 C22 1.489(6) . ?
C12 C11 1.363(6) . ?
C16 C15 1.489(6) . ?
C24 C23 1.493(6) . ?
C18 C17 1.492(7) . ?
O10 C32 1.425(17) . ?
O10 C33 1.425(13) . ?
C20 C19 1.482(7) . ?
O11 C35 1.421(19) . ?
O11 C34 1.438(15) . ?
C38 C37 1.47(3) . ?
C39 C40 1.43(3) . ?
C35 C36 1.52(2) . ?
O9 C30 1.409(12) . ?
O9 C31 1.425(12) . ?
C32 C31 1.451(15) . ?
C34 C33 1.484(17) . ?
C29 C30 1.477(17) . ?
C29A O8A 1.454(19) . ?
C29A C30A 1.52(2) . ?
O12A C37A 1.47(2) . ?
O12A C36A 1.412(19) . ?
C37A C38A 1.49(2) . ?
C36A C35A 1.49(2) . ?
C38A O13A 1.446(19) . ?
C35A O11A 1.41(2) . ?
O13A C39A 1.48(3) . ?
O11A C34A 1.406(19) . ?
C39A C40A 1.53(2) . ?
C34A C33A 1.49(2) . ?
C40A O8A 1.43(2) . ?
O10A C32A 1.410(17) . ?
O10A C33A 1.41(2) . ?
C30A O9A 1.36(2) . ?
C32A C31A 1.51(2) . ?
O9A C31A 1.412(17) . ?

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 S6 85.66(4) . . ?
S4 Ni1 S5 93.30(4) . . ?
S4 Ni1 S7 178.72(4) . . ?
S6 Ni1 S5 177.32(4) . . ?
S7 Ni1 S6 93.17(4) . . ?
S7 Ni1 S5 87.85(4) . . ?
S15 Ni2 S15 180.00(5) . 2_667 ?
S15 Ni2 S14 86.68(4) . 2_667 ?
S15 Ni2 S14 93.32(4) 2_667 2_667 ?
S15 Ni2 S14 86.68(4) 2_667 . ?
S15 Ni2 S14 93.32(4) . . ?
S14 Ni2 S14 180.0 . 2_667 ?
S20 Ni3 S20 180.00(6) 2_666 . ?
S19 Ni3 S20 93.60(4) . . ?
S19 Ni3 S20 93.60(4) 2_666 2_666 ?
S19 Ni3 S20 86.40(4) . 2_666 ?
S19 Ni3 S20 86.40(4) 2_666 . ?
S19 Ni3 S19 180.0 2_666 . ?
C3 S4 Ni1 102.42(12) . . ?
C5 S6 Ni1 102.20(13) . . ?
C2 S5 Ni1 101.62(13) . . ?
C4 S7 Ni1 102.30(13) . . ?
C9 S15 Ni2 102.12(13) . . ?
C8 S14 Ni2 101.89(14) . . ?
C7 S13 C9 97.73(19) . . ?
C3 S2 C1 97.76(18) . . ?
C6 S9 C4 97.7(2) . . ?
C12 S20 Ni3 101.74(14) . . ?
C11 S19 Ni3 102.12(14) . . ?
C11 S17 C10 97.2(2) . . ?
C7 S12 C8 97.5(2) . . ?
C6 S8 C5 97.5(2) . . ?
C1 S3 C2 97.82(18) . . ?
C10 S18 C12 97.3(2) . . ?
C26 O7 C27 111.2(3) . . ?
C15 O5 C14 111.9(3) . . ?
C13 O4 C24 112.0(3) . . ?
C17 O6 C16 112.1(3) . . ?
C21 O2 C20 112.9(3) . . ?
C19 O1 C18 113.3(3) . . ?
C23 O3 C22 111.5(3) . . ?
C36 O12 C37 120.7(13) . . ?
C40 O8 C29 111.9(16) . . ?
C38 O13 C39 117.4(16) . . ?
O7 C26 C25 108.6(3) . . ?
S15 C9 S13 122.7(2) . . ?
C8 C9 S15 120.9(3) . . ?
C8 C9 S13 116.3(3) . . ?
S6 C5 S8 122.5(2) . . ?
C4 C5 S6 121.2(3) . . ?
C4 C5 S8 116.3(3) . . ?
O7 C27 C28 109.2(3) . . ?
N1 C25 C26 113.1(3) . . ?
N2 C28 C27 112.2(3) . . ?
S7 C4 S9 123.5(2) . . ?
C5 C4 S7 120.8(3) . . ?
C5 C4 S9 115.7(3) . . ?
S5 C2 S3 123.1(2) . . ?
C3 C2 S5 121.5(3) . . ?
C3 C2 S3 115.4(3) . . ?
O4 C13 C14 109.2(3) . . ?
O2 C21 C22 109.0(3) . . ?
O5 C14 C13 109.1(3) . . ?
S13 C7 S12 112.7(2) . . ?
S11 C7 S13 123.4(3) . . ?
S11 C7 S12 124.0(3) . . ?
S20 C12 S18 122.5(2) . . ?
C11 C12 S20 121.6(3) . . ?
C11 C12 S18 115.9(3) . . ?
O6 C16 C15 109.6(3) . . ?
S4 C3 S2 122.4(2) . . ?
C2 C3 S4 121.0(3) . . ?
C2 C3 S2 116.5(3) . . ?
O3 C22 C21 109.3(3) . . ?
S14 C8 S12 122.6(2) . . ?
C9 C8 S14 121.7(3) . . ?
C9 C8 S12 115.7(3) . . ?
S19 C11 S17 122.7(2) . . ?
C12 C11 S19 120.9(3) . . ?
C12 C11 S17 116.4(3) . . ?
O4 C24 C23 108.7(3) . . ?
O3 C23 C24 108.9(3) . . ?
O1 C18 C17 109.6(3) . . ?
S8 C6 S9 112.8(2) . . ?
S10 C6 S9 124.5(3) . . ?
S10 C6 S8 122.7(3) . . ?
O6 C17 C18 109.3(4) . . ?
S2 C1 S3 112.4(2) . . ?
S1 C1 S2 122.6(2) . . ?
S1 C1 S3 125.0(2) . . ?
C33 O10 C32 112.8(10) . . ?
O5 C15 C16 108.2(3) . . ?
S18 C10 S17 113.3(3) . . ?
S16 C10 S17 123.1(3) . . ?
S16 C10 S18 123.7(3) . . ?
O2 C20 C19 109.1(3) . . ?
O1 C19 C20 107.9(3) . . ?
C35 O11 C34 111.6(12) . . ?
O13 C38 C37 111.9(19) . . ?
O13 C39 C40 115.1(18) . . ?
O12 C37 C38 112.1(13) . . ?
O8 C40 C39 107.2(15) . . ?
O11 C35 C36 107.9(14) . . ?
C30 O9 C31 112.0(9) . . ?
O10 C32 C31 110.4(12) . . ?
O12 C36 C35 113.2(13) . . ?
O11 C34 C33 109.4(9) . . ?
O8 C29 C30 110.1(12) . . ?
O9 C30 C29 108.0(10) . . ?
O8A C29A C30A 107.7(12) . . ?
C36A O12A C37A 110.2(16) . . ?
O12A C37A C38A 109.3(15) . . ?
O12A C36A C35A 106.2(14) . . ?
O13A C38A C37A 106.5(14) . . ?
O11A C35A C36A 108.7(16) . . ?
C38A O13A C39A 107.9(13) . . ?
C34A O11A C35A 110.9(13) . . ?
O13A C39A C40A 103.0(15) . . ?
O11A C34A C33A 110.5(14) . . ?
O8A C40A C39A 111.5(14) . . ?
C40A O8A C29A 110.4(14) . . ?
C32A O10A C33A 113.7(11) . . ?
O9A C30A C29A 109.2(11) . . ?
O10A C32A C31A 110.9(13) . . ?
C30A O9A C31A 111.4(13) . . ?
O10 C33 C34 110.4(9) . . ?
O9 C31 C32 110.5(9) . . ?
O9A C31A C32A 109.9(13) . . ?
O10A C33A C34A 111.1(14) . . ?

_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 2.914
_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_18c6_nc2oc2n_lt_04_133_00_autored
_database_code_depnum_ccdc_archive 'CCDC 2384651'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2024-09-17 deposited with the CCDC.	2024-11-08 downloaded from the CCDC.
;
_audit_creation_date             2023-12-22
_audit_creation_method           
;
Olex2 1.5-ac5-023
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C6 Ni S10), C4 H14 N2 O, 2(C12 H24 O6)'
_chemical_formula_sum            'C40 H62 N2 Ni2 O13 S20'
_chemical_formula_weight         1537.53
_chemical_melting_point          ?
_chemical_oxdiff_formula         C40H62N2Ni2O13S20
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                   13.0962(3)
_cell_length_b                   14.4347(3)
_cell_length_c                   18.1822(5)
_cell_angle_alpha                90.702(2)
_cell_angle_beta                 100.195(2)
_cell_angle_gamma                104.820(2)
_cell_volume                     3264.37(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    16822
_cell_measurement_temperature    132.90(14)
_cell_measurement_theta_max      30.6190
_cell_measurement_theta_min      2.0110
_shelx_estimated_absorpt_T_max   0.915
_shelx_estimated_absorpt_T_min   0.492
_exptl_absorpt_coefficient_mu    1.271
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.67a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light black'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-18 1 9 0.2087
1 -20 -2 0.2398
18 0 -8 0.3242
-1 20 2 0.2492
-1 0 -25 0.0328
2 -1 24 0.0172

_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.507
_exptl_crystal_size_min          0.071
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-17.7787 0.6712 8.6169 -0.0429 0.5521 0.8327
0.8117 -19.6661 -2.4249 -0.0714 0.9046 -0.4202
17.6176 0.1490 -8.4546 0.0456 -0.5856 -0.8093
-0.6531 19.6328 2.3451 0.0717 -0.9083 0.4122
-1.0560 -0.1883 -24.8370 0.9667 0.1793 -0.1825
2.1576 -0.5675 24.4771 -0.9762 -0.1810 0.1192

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0572
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.790
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            43163
_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         30.914
_diffrn_reflns_theta_min         2.162
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      132.90(14)
_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    -17.00  28.00   0.50    1.46    --   -5.80 -99.00   0.00   90
  2  ω    -77.00   4.00   0.50    1.46    --   -5.80 -37.00 -90.00  162
  3  ω    -75.00 -43.00   0.50    1.46    --   -5.80 -57.00  30.00   64
  4  ω    -38.00   3.00   0.50    1.46    --   -5.80 -57.00  30.00   82
  5  ω    -15.00  68.00   0.50    1.46    --   -5.80  37.00-150.00  166
  6  ω    -67.00   7.00   0.50    1.46    --   -5.80 -37.00  30.00  148
  7  ω    -11.00  35.00   0.50    1.46    --    6.03 -99.00-150.00   92
;
_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      -0.0158602000
_diffrn_orient_matrix_UB_12      0.0077009000
_diffrn_orient_matrix_UB_13      -0.0383067000
_diffrn_orient_matrix_UB_21      -0.0354174000
_diffrn_orient_matrix_UB_22      -0.0468007000
_diffrn_orient_matrix_UB_23      -0.0053577000
_diffrn_orient_matrix_UB_31      -0.0417815000
_diffrn_orient_matrix_UB_32      0.0185331000
_diffrn_orient_matrix_UB_33      0.0089839000
_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                10760
_reflns_number_total             16316
_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 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.978
_refine_diff_density_min         -1.036
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     862
_refine_ls_number_reflns         16316
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0523
_refine_ls_restrained_S_all      1.023
_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)+(0.0594P)²+4.2283P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1223
_refine_ls_wR_factor_ref         0.1413
_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. Rigid body (RIGU) restrains
 C31A, O9A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(C29A)=Sof(H29C)=Sof(H29D)=Sof(O12A)=Sof(C37A)=Sof(H37C)=Sof(H37D)=
 Sof(C36A)=Sof(H36C)=Sof(H36D)=Sof(C38A)=Sof(H38C)=Sof(H38D)=Sof(C35A)=
 Sof(H35C)=Sof(H35D)=Sof(O13A)=Sof(O11A)=Sof(C39A)=Sof(H39C)=Sof(H39D)=
 Sof(C34A)=Sof(H34C)=Sof(H34D)=Sof(C40A)=Sof(H40C)=Sof(H40D)=Sof(O8A)=Sof(O10A)=
 Sof(C30A)=Sof(H30C)=Sof(H30D)=Sof(C32A)=Sof(H32C)=Sof(H32D)=Sof(O9A)=Sof(C31A)=
 Sof(H31C)=Sof(H31D)=Sof(C33A)=Sof(H33C)=Sof(H33D)=1-FVAR(1)
 Sof(O12)=Sof(O8)=Sof(O13)=Sof(O10)=Sof(O11)=Sof(C38)=Sof(H38A)=Sof(H38B)=
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C40)=Sof(H40A)=
 Sof(H40B)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(O9)=Sof(C32)=Sof(H32A)=Sof(H32B)=
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(C29)=Sof(H29A)=
 Sof(H29B)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C31)=
 Sof(H31A)=Sof(H31B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C27(H27A,H27B), C25(H25A,H25B), C28(H28A,H28B), C13(H13A,
 H13B), C21(H21A,H21B), C14(H14A,H14B), C16(H16A,H16B), C22(H22A,H22B),
 C24(H24A,H24B), C23(H23A,H23B), C18(H18A,H18B), C17(H17A,H17B), C15(H15A,H15B),
  C20(H20A,H20B), C19(H19A,H19B), C38(H38A,H38B), C39(H39A,H39B), C37(H37A,
 H37B), C40(H40A,H40B), C35(H35A,H35B), C32(H32A,H32B), C36(H36A,H36B),
 C34(H34A,H34B), C29(H29A,H29B), C30(H30A,H30B), C29A(H29C,H29D), C37A(H37C,
 H37D), C36A(H36C,H36D), C38A(H38C,H38D), C35A(H35C,H35D), C39A(H39C,H39D),
 C34A(H34C,H34D), C40A(H40C,H40D), C30A(H30C,H30D), C32A(H32C,H32D), C33(H33A,
 H33B), C31(H31A,H31B), C31A(H31C,H31D), C33A(H33C,H33D)
4.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(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 0.70128(3) 0.92142(3) 0.98429(3) 0.02948(11) Uani 1 1 d . . . . .
Ni2 Ni 0.500000 0.500000 1.000000 0.03201(15) Uani 1 2 d S . P . .
Ni3 Ni 0.500000 0.500000 0.500000 0.03732(16) Uani 1 2 d S . P . .
S4 S 0.53010(7) 0.90271(6) 0.95906(5) 0.03245(19) Uani 1 1 d . . . . .
S6 S 0.69740(7) 1.00094(7) 1.08486(5) 0.0358(2) Uani 1 1 d . . . . .
S5 S 0.70093(7) 0.83544(6) 0.88546(6) 0.0354(2) Uani 1 1 d . . . . .
S7 S 0.87292(7) 0.94066(7) 1.01228(6) 0.0358(2) Uani 1 1 d . . . . .
S15 S 0.59479(7) 0.64750(7) 1.00910(6) 0.0375(2) Uani 1 1 d . . . . .
S14 S 0.57665(7) 0.47009(7) 1.10958(6) 0.0373(2) Uani 1 1 d . . . . .
S13 S 0.76639(8) 0.76213(7) 1.13571(6) 0.0433(2) Uani 1 1 d . . . . .
S2 S 0.35944(7) 0.78929(7) 0.83345(6) 0.0378(2) Uani 1 1 d . . . . .
S9 S 1.03376(8) 1.02721(7) 1.15441(6) 0.0458(2) Uani 1 1 d . . . . .
S20 S 0.59396(9) 0.49453(8) 0.41440(6) 0.0455(2) Uani 1 1 d . . . . .
S19 S 0.63864(9) 0.57002(7) 0.58329(6) 0.0438(2) Uani 1 1 d . . . . .
S17 S 0.87605(9) 0.62728(8) 0.57587(6) 0.0472(2) Uani 1 1 d . . . . .
S12 S 0.74986(8) 0.59891(8) 1.22823(6) 0.0438(2) Uani 1 1 d . . . . .
S8 S 0.87009(9) 1.07928(7) 1.22148(6) 0.0474(3) Uani 1 1 d . . . . .
S11 S 0.91480(9) 0.78228(9) 1.28250(8) 0.0567(3) Uani 1 1 d . . . . .
S3 S 0.51428(8) 0.71963(7) 0.76853(7) 0.0456(3) Uani 1 1 d . . . . .
S18 S 0.83528(9) 0.55867(10) 0.42038(6) 0.0560(3) Uani 1 1 d . . . . .
S10 S 1.09105(11) 1.11730(8) 1.31043(8) 0.0661(4) Uani 1 1 d . . . . .
S1 S 0.28076(10) 0.65397(11) 0.69980(9) 0.0741(4) Uani 1 1 d . . . . .
S16 S 1.06008(11) 0.64372(13) 0.49797(9) 0.0810(5) Uani 1 1 d . . . . .
O7 O 0.2425(2) 0.67549(17) 0.30633(14) 0.0352(6) Uani 1 1 d . . . . .
O5 O 0.0801(2) 0.71829(18) 0.02883(16) 0.0408(6) Uani 1 1 d . . . . .
O4 O 0.2923(2) 0.73450(18) 0.09941(15) 0.0399(6) Uani 1 1 d . . . . .
O6 O -0.0918(2) 0.5763(2) 0.06636(16) 0.0455(7) Uani 1 1 d . . . . .
O2 O 0.1690(2) 0.42556(17) 0.21254(16) 0.0435(6) Uani 1 1 d . . . . .
O1 O -0.0360(2) 0.41686(19) 0.13884(16) 0.0459(7) Uani 1 1 d . . . . .
O3 O 0.3297(2) 0.56376(19) 0.15834(15) 0.0406(6) Uani 1 1 d . . . . .
N1 N 0.1205(2) 0.60068(19) 0.15473(17) 0.0309(6) Uani 1 1 d . . . . .
H1A H 0.103436 0.625030 0.109642 0.037 Uiso 1 1 calc R U . . .
H1B H 0.086791 0.536930 0.152292 0.037 Uiso 1 1 calc R U . . .
H1C H 0.192934 0.609023 0.166397 0.037 Uiso 1 1 calc R U . . .
O12 O 0.6453(17) 0.8566(18) 0.3709(13) 0.069(5) Uani 0.563(7) 1 d . . P A 1
N2 N 0.4317(3) 0.8153(2) 0.39538(18) 0.0382(7) Uani 1 1 d . . . . .
H2A H 0.394686 0.833215 0.353151 0.046 Uiso 1 1 calc R U . . .
H2B H 0.503471 0.840312 0.397560 0.046 Uiso 1 1 calc R U . . .
H2C H 0.411983 0.837693 0.436267 0.046 Uiso 1 1 calc R U . . .
O8 O 0.4257(16) 0.8604(15) 0.5543(12) 0.057(5) Uani 0.563(7) 1 d . . P A 1
O13 O 0.6041(7) 0.8089(6) 0.5129(5) 0.055(2) Uani 0.563(7) 1 d . . P A 1
C26 C 0.1307(3) 0.6312(3) 0.2912(2) 0.0390(9) Uani 1 1 d . . . . .
H26A H 0.095332 0.656898 0.327637 0.047 Uiso 1 1 calc R U . . .
H26B H 0.117631 0.561082 0.295930 0.047 Uiso 1 1 calc R U . . .
C9 C 0.6724(3) 0.6566(3) 1.0973(2) 0.0358(8) Uani 1 1 d . . . . .
C5 C 0.8281(3) 1.0239(3) 1.1314(2) 0.0372(8) Uani 1 1 d . . . . .
C27 C 0.2894(3) 0.6623(3) 0.3812(2) 0.0427(9) Uani 1 1 d . . . . .
H27A H 0.276931 0.592866 0.389302 0.051 Uiso 1 1 calc R U . . .
H27B H 0.255698 0.691068 0.417071 0.051 Uiso 1 1 calc R U . . .
C25 C 0.0854(3) 0.6514(3) 0.2133(2) 0.0428(9) Uani 1 1 d . . . . .
H25A H 0.005901 0.631739 0.205809 0.051 Uiso 1 1 calc R U . . .
H25B H 0.107828 0.721379 0.207431 0.051 Uiso 1 1 calc R U . . .
C28 C 0.4072(3) 0.7091(3) 0.3940(2) 0.0432(9) Uani 1 1 d . . . . .
H28A H 0.441806 0.689948 0.442238 0.052 Uiso 1 1 calc R U . . .
H28B H 0.438188 0.685882 0.353808 0.052 Uiso 1 1 calc R U . . .
C4 C 0.9049(3) 0.9987(3) 1.1000(2) 0.0375(8) Uani 1 1 d . . . . .
C2 C 0.5663(3) 0.7979(2) 0.8481(2) 0.0330(8) Uani 1 1 d . . . . .
C13 C 0.2674(4) 0.7914(3) 0.0395(3) 0.0494(10) Uani 1 1 d . . . . .
H13A H 0.266637 0.758177 -0.008613 0.059 Uiso 1 1 calc R U . . .
H13B H 0.322739 0.853543 0.044802 0.059 Uiso 1 1 calc R U . . .
C21 C 0.2697(4) 0.4100(3) 0.2066(2) 0.0480(10) Uani 1 1 d . . . . .
H21A H 0.265772 0.380213 0.156537 0.058 Uiso 1 1 calc R U . . .
H21B H 0.289248 0.366132 0.244803 0.058 Uiso 1 1 calc R U . . .
C14 C 0.1593(4) 0.8082(3) 0.0403(3) 0.0491(10) Uani 1 1 d . . . . .
H14A H 0.159503 0.839833 0.089010 0.059 Uiso 1 1 calc R U . . .
H14B H 0.142628 0.850816 0.000265 0.059 Uiso 1 1 calc R U . . .
C7 C 0.8160(3) 0.7182(3) 1.2192(3) 0.0440(10) Uani 1 1 d . . . . .
C12 C 0.7225(3) 0.5446(3) 0.4624(2) 0.0403(9) Uani 1 1 d . . . . .
C16 C -0.1030(3) 0.6334(4) 0.0033(2) 0.0503(11) Uani 1 1 d . . . . .
H16A H -0.177373 0.640393 -0.008393 0.060 Uiso 1 1 calc R U . . .
H16B H -0.088977 0.601545 -0.040999 0.060 Uiso 1 1 calc R U . . .
C3 C 0.4923(3) 0.8287(2) 0.8795(2) 0.0311(7) Uani 1 1 d . . . . .
C22 C 0.3522(3) 0.5041(3) 0.2182(2) 0.0457(10) Uani 1 1 d . . . . .
H22A H 0.351798 0.536168 0.266585 0.055 Uiso 1 1 calc R U . . .
H22B H 0.424468 0.493756 0.219891 0.055 Uiso 1 1 calc R U . . .
C8 C 0.6647(3) 0.5793(3) 1.1401(2) 0.0370(8) Uani 1 1 d . . . . .
C11 C 0.7422(3) 0.5782(3) 0.5349(2) 0.0394(9) Uani 1 1 d . . . . .
C24 C 0.3872(3) 0.7048(3) 0.0958(3) 0.0478(10) Uani 1 1 d . . . . .
H24A H 0.448156 0.761661 0.094959 0.057 Uiso 1 1 calc R U . . .
H24B H 0.376325 0.663829 0.049589 0.057 Uiso 1 1 calc R U . . .
C23 C 0.4115(3) 0.6500(3) 0.1628(3) 0.0478(10) Uani 1 1 d . . . . .
H23A H 0.481830 0.635695 0.164613 0.057 Uiso 1 1 calc R U . . .
H23B H 0.415216 0.688787 0.209000 0.057 Uiso 1 1 calc R U . . .
C18 C -0.1435(3) 0.4274(3) 0.1200(3) 0.0563(12) Uani 1 1 d . . . . .
H18A H -0.159459 0.462507 0.161858 0.068 Uiso 1 1 calc R U . . .
H18B H -0.195449 0.363271 0.111844 0.068 Uiso 1 1 calc R U . . .
C6 C 1.0035(3) 1.0760(3) 1.2332(3) 0.0474(10) Uani 1 1 d . . . . .
C17 C -0.1549(3) 0.4810(3) 0.0510(3) 0.0536(11) Uani 1 1 d . . . . .
H17A H -0.131189 0.450007 0.010575 0.064 Uiso 1 1 calc R U . . .
H17B H -0.231257 0.480305 0.033938 0.064 Uiso 1 1 calc R U . . .
C1 C 0.3790(3) 0.7170(3) 0.7627(3) 0.0472(10) Uani 1 1 d . . . . .
O10 O 0.3022(8) 0.9296(6) 0.3075(5) 0.052(2) Uani 0.563(7) 1 d . . P A 1
C15 C -0.0258(4) 0.7296(3) 0.0202(3) 0.0511(11) Uani 1 1 d . . . . .
H15A H -0.038270 0.771714 -0.021195 0.061 Uiso 1 1 calc R U . . .
H15B H -0.035781 0.759570 0.066710 0.061 Uiso 1 1 calc R U . . .
C10 C 0.9306(4) 0.6123(3) 0.4972(2) 0.0511(10) Uani 1 1 d . . . . .
C20 C 0.0843(4) 0.3379(3) 0.2052(3) 0.0567(12) Uani 1 1 d . . . . .
H20A H 0.097547 0.298602 0.248384 0.068 Uiso 1 1 calc R U . . .
H20B H 0.082456 0.300188 0.158908 0.068 Uiso 1 1 calc R U . . .
C19 C -0.0194(4) 0.3618(3) 0.2024(3) 0.0598(13) Uani 1 1 d . . . . .
H19A H -0.078493 0.302252 0.197984 0.072 Uiso 1 1 calc R U . . .
H19B H -0.017914 0.399206 0.248706 0.072 Uiso 1 1 calc R U . . .
O11 O 0.4836(6) 0.8879(5) 0.2605(4) 0.0521(18) Uani 0.563(7) 1 d . . P A 1
C38 C 0.705(2) 0.8239(13) 0.4973(14) 0.089(8) Uani 0.563(7) 1 d . . P A 1
H38A H 0.743650 0.783491 0.528468 0.106 Uiso 0.563(7) 1 calc R U P A 1
H38B H 0.744346 0.891901 0.510467 0.106 Uiso 0.563(7) 1 calc R U P A 1
C39 C 0.596(2) 0.8378(16) 0.5847(13) 0.076(8) Uani 0.563(7) 1 d . . P A 1
H39A H 0.622358 0.908636 0.591268 0.091 Uiso 0.563(7) 1 calc R U P A 1
H39B H 0.643378 0.810531 0.621758 0.091 Uiso 0.563(7) 1 calc R U P A 1
C37 C 0.7026(10) 0.8012(10) 0.4178(11) 0.084(5) Uani 0.563(7) 1 d . . P A 1
H37A H 0.777149 0.814693 0.408602 0.101 Uiso 0.563(7) 1 calc R U P A 1
H37B H 0.667897 0.732093 0.405300 0.101 Uiso 0.563(7) 1 calc R U P A 1
C40 C 0.4875(9) 0.8093(8) 0.6006(5) 0.072(3) Uani 0.563(7) 1 d . . P A 1
H40A H 0.456658 0.739357 0.589898 0.086 Uiso 0.563(7) 1 calc R U P A 1
H40B H 0.488570 0.824896 0.653925 0.086 Uiso 0.563(7) 1 calc R U P A 1
C35 C 0.5928(17) 0.9157(15) 0.2546(13) 0.082(7) Uani 0.563(7) 1 d . . P A 1
H35A H 0.626219 0.981941 0.276628 0.098 Uiso 0.563(7) 1 calc R U P A 1
H35B H 0.599820 0.914190 0.201277 0.098 Uiso 0.563(7) 1 calc R U P A 1
O9 O 0.2514(6) 0.8719(6) 0.4471(4) 0.0505(18) Uani 0.563(7) 1 d . . P A 1
C32 C 0.1940(14) 0.9001(14) 0.3210(8) 0.055(4) Uani 0.563(7) 1 d . . P A 1
H32A H 0.165111 0.829957 0.310257 0.066 Uiso 0.563(7) 1 calc R U P A 1
H32B H 0.147792 0.932550 0.287303 0.066 Uiso 0.563(7) 1 calc R U P A 1
C36 C 0.6479(9) 0.8468(9) 0.2959(8) 0.071(3) Uani 0.563(7) 1 d . . P A 1
H36A H 0.610763 0.780139 0.276317 0.086 Uiso 0.563(7) 1 calc R U P A 1
H36B H 0.723303 0.860763 0.288523 0.086 Uiso 0.563(7) 1 calc R U P A 1
C34 C 0.4244(12) 0.9501(9) 0.2209(6) 0.055(4) Uani 0.563(7) 1 d . . P A 1
H34A H 0.427705 0.946590 0.167013 0.066 Uiso 0.563(7) 1 calc R U P A 1
H34B H 0.456604 1.017387 0.240797 0.066 Uiso 0.563(7) 1 calc R U P A 1
C29 C 0.3175(10) 0.8397(8) 0.5687(5) 0.072(3) Uani 0.563(7) 1 d . . P A 1
H29A H 0.319606 0.854547 0.622377 0.087 Uiso 0.563(7) 1 calc R U P A 1
H29B H 0.281744 0.770624 0.557107 0.087 Uiso 0.563(7) 1 calc R U P A 1
C30 C 0.2562(16) 0.8975(12) 0.5225(7) 0.058(4) Uani 0.563(7) 1 d . . P A 1
H30A H 0.182733 0.884833 0.533656 0.070 Uiso 0.563(7) 1 calc R U P A 1
H30B H 0.291984 0.966673 0.533478 0.070 Uiso 0.563(7) 1 calc R U P A 1
C29A C 0.3296(11) 0.9103(7) 0.5510(8) 0.051(3) Uani 0.437(7) 1 d . . P A 2
H29C H 0.364717 0.980093 0.555350 0.061 Uiso 0.437(7) 1 calc R U P A 2
H29D H 0.303182 0.892296 0.597992 0.061 Uiso 0.437(7) 1 calc R U P A 2
O12A O 0.6635(17) 0.8456(17) 0.3820(11) 0.033(3) Uani 0.437(7) 1 d . . P A 2
C37A C 0.7407(10) 0.8365(10) 0.4444(8) 0.042(3) Uani 0.437(7) 1 d . . P A 2
H37C H 0.790082 0.900477 0.460876 0.050 Uiso 0.437(7) 1 calc R U P A 2
H37D H 0.783806 0.794729 0.429376 0.050 Uiso 0.437(7) 1 calc R U P A 2
C36A C 0.7088(11) 0.8968(9) 0.3244(7) 0.054(3) Uani 0.437(7) 1 d . . P A 2
H36C H 0.768054 0.871568 0.312893 0.064 Uiso 0.437(7) 1 calc R U P A 2
H36D H 0.738132 0.965689 0.340601 0.064 Uiso 0.437(7) 1 calc R U P A 2
C38A C 0.6906(17) 0.7954(13) 0.5075(13) 0.043(4) Uani 0.437(7) 1 d . . P A 2
H38C H 0.650452 0.727435 0.494762 0.052 Uiso 0.437(7) 1 calc R U P A 2
H38D H 0.746391 0.798392 0.552680 0.052 Uiso 0.437(7) 1 calc R U P A 2
C35A C 0.623(2) 0.8849(15) 0.2567(13) 0.057(5) Uani 0.437(7) 1 d . . P A 2
H35C H 0.653223 0.914926 0.213976 0.069 Uiso 0.437(7) 1 calc R U P A 2
H35D H 0.589090 0.815916 0.242760 0.069 Uiso 0.437(7) 1 calc R U P A 2
O13A O 0.6179(9) 0.8520(6) 0.5213(6) 0.037(2) Uani 0.437(7) 1 d . . P A 2
O11A O 0.5446(12) 0.9303(8) 0.2743(5) 0.058(3) Uani 0.437(7) 1 d . . P A 2
C39A C 0.575(2) 0.8203(17) 0.5896(15) 0.043(5) Uani 0.437(7) 1 d . . P A 2
H39C H 0.633755 0.831326 0.633997 0.052 Uiso 0.437(7) 1 calc R U P A 2
H39D H 0.536375 0.751303 0.583909 0.052 Uiso 0.437(7) 1 calc R U P A 2
C34A C 0.4671(17) 0.9285(13) 0.2102(12) 0.066(5) Uani 0.437(7) 1 d . . P A 2
H34C H 0.435696 0.861508 0.189435 0.079 Uiso 0.437(7) 1 calc R U P A 2
H34D H 0.501470 0.966058 0.171749 0.079 Uiso 0.437(7) 1 calc R U P A 2
C40A C 0.4996(10) 0.8821(7) 0.5962(6) 0.045(3) Uani 0.437(7) 1 d . . P A 2
H40C H 0.477864 0.875008 0.645730 0.054 Uiso 0.437(7) 1 calc R U P A 2
H40D H 0.537707 0.950287 0.593194 0.054 Uiso 0.437(7) 1 calc R U P A 2
O8A O 0.4055(16) 0.8570(16) 0.5387(13) 0.032(3) Uani 0.437(7) 1 d . . P A 2
O10A O 0.3226(9) 0.9124(7) 0.2792(8) 0.049(3) Uani 0.437(7) 1 d . . P A 2
C30A C 0.2368(15) 0.8867(12) 0.4852(12) 0.058(6) Uani 0.437(7) 1 d . . P A 2
H30C H 0.205627 0.816337 0.478490 0.069 Uiso 0.437(7) 1 calc R U P A 2
H30D H 0.179911 0.916769 0.494566 0.069 Uiso 0.437(7) 1 calc R U P A 2
C32A C 0.2312(14) 0.9401(10) 0.2919(9) 0.064(5) Uani 0.437(7) 1 d . . P A 2
H32C H 0.173633 0.921412 0.247004 0.077 Uiso 0.437(7) 1 calc R U P A 2
H32D H 0.249562 1.010762 0.300388 0.077 Uiso 0.437(7) 1 calc R U P A 2
O9A O 0.2731(6) 0.9205(6) 0.4218(5) 0.049(2) Uani 0.437(7) 1 d . . P A 2
C33 C 0.3108(9) 0.9188(8) 0.2310(6) 0.053(2) Uani 0.563(7) 1 d . . P A 1
H33A H 0.268516 0.957288 0.200511 0.063 Uiso 0.563(7) 1 calc R U P A 1
H33B H 0.280291 0.850597 0.213022 0.063 Uiso 0.563(7) 1 calc R U P A 1
C31 C 0.1925(9) 0.9244(7) 0.3977(6) 0.056(3) Uani 0.563(7) 1 d . . P A 1
H31A H 0.224818 0.994162 0.409019 0.067 Uiso 0.563(7) 1 calc R U P A 1
H31B H 0.117304 0.909410 0.405623 0.067 Uiso 0.563(7) 1 calc R U P A 1
C31A C 0.1917(16) 0.8947(18) 0.3572(13) 0.067(7) Uani 0.437(7) 1 d . . P A 2
H31C H 0.127948 0.915718 0.365187 0.080 Uiso 0.437(7) 1 calc R U P A 2
H31D H 0.169805 0.824049 0.347959 0.080 Uiso 0.437(7) 1 calc R U P A 2
C33A C 0.3798(18) 0.9698(14) 0.2281(11) 0.063(5) Uani 0.437(7) 1 d . . P A 2
H33C H 0.411504 1.035962 0.250541 0.075 Uiso 0.437(7) 1 calc R U P A 2
H33D H 0.329084 0.972751 0.181348 0.075 Uiso 0.437(7) 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 S4 2.1523(9) . ?
Ni1 S6 2.1623(10) . ?
Ni1 S5 2.1699(11) . ?
Ni1 S7 2.1589(10) . ?
Ni2 S15 2.1606(9) . ?
Ni2 S15 2.1606(9) 2_667 ?
Ni2 S14 2.1676(10) . ?
Ni2 S14 2.1676(10) 2_667 ?
Ni3 S20 2.1605(10) . ?
Ni3 S20 2.1605(10) 2_666 ?
Ni3 S19 2.1591(11) . ?
Ni3 S19 2.1592(11) 2_666 ?
S4 C3 1.708(4) . ?
S6 C5 1.717(4) . ?
S5 C2 1.716(4) . ?
S7 C4 1.723(4) . ?
S15 C9 1.724(4) . ?
S14 C8 1.716(4) . ?
S13 C9 1.742(4) . ?
S13 C7 1.735(5) . ?
S2 C3 1.737(4) . ?
S2 C1 1.741(4) . ?
S9 C4 1.744(4) . ?
S9 C6 1.739(5) . ?
S20 C12 1.721(4) . ?
S19 C11 1.723(4) . ?
S17 C11 1.738(4) . ?
S17 C10 1.742(5) . ?
S12 C7 1.743(4) . ?
S12 C8 1.757(4) . ?
S8 C5 1.746(4) . ?
S8 C6 1.735(4) . ?
S11 C7 1.640(4) . ?
S3 C2 1.746(4) . ?
S3 C1 1.747(4) . ?
S18 C12 1.748(4) . ?
S18 C10 1.724(5) . ?
S10 C6 1.644(4) . ?
S1 C1 1.626(4) . ?
S16 C10 1.637(5) . ?
O7 C26 1.415(4) . ?
O7 C27 1.428(5) . ?
O5 C14 1.426(5) . ?
O5 C15 1.419(5) . ?
O4 C13 1.413(5) . ?
O4 C24 1.427(5) . ?
O6 C16 1.430(5) . ?
O6 C17 1.407(5) . ?
O2 C21 1.414(5) . ?
O2 C20 1.441(5) . ?
O1 C18 1.436(5) . ?
O1 C19 1.427(6) . ?
O3 C22 1.433(5) . ?
O3 C23 1.411(5) . ?
N1 C25 1.486(4) . ?
O12 C37 1.42(2) . ?
O12 C36 1.38(2) . ?
N2 C28 1.483(5) . ?
O8 C40 1.41(2) . ?
O8 C29 1.443(19) . ?
O13 C38 1.36(3) . ?
O13 C39 1.40(2) . ?
C26 C25 1.499(6) . ?
C9 C8 1.360(5) . ?
C5 C4 1.362(5) . ?
C27 C28 1.492(6) . ?
C2 C3 1.368(5) . ?
C13 C14 1.499(6) . ?
C21 C22 1.489(6) . ?
C12 C11 1.357(6) . ?
C16 C15 1.485(7) . ?
C24 C23 1.491(6) . ?
C18 C17 1.488(7) . ?
O10 C32 1.44(2) . ?
O10 C33 1.425(13) . ?
C20 C19 1.477(7) . ?
O11 C35 1.41(2) . ?
O11 C34 1.449(14) . ?
C38 C37 1.47(3) . ?
C39 C40 1.45(3) . ?
C35 C36 1.51(2) . ?
O9 C30 1.402(13) . ?
O9 C31 1.431(12) . ?
C32 C31 1.439(18) . ?
C34 C33 1.485(17) . ?
C29 C30 1.472(19) . ?
C29A O8A 1.45(2) . ?
C29A C30A 1.51(2) . ?
O12A C37A 1.41(2) . ?
O12A C36A 1.42(2) . ?
C37A C38A 1.48(2) . ?
C36A C35A 1.49(3) . ?
C38A O13A 1.454(17) . ?
C35A O11A 1.42(2) . ?
O13A C39A 1.48(3) . ?
O11A C34A 1.40(2) . ?
C39A C40A 1.51(2) . ?
C34A C33A 1.50(2) . ?
C40A O8A 1.43(3) . ?
O10A C32A 1.410(17) . ?
O10A C33A 1.43(3) . ?
C30A O9A 1.37(2) . ?
C32A C31A 1.47(3) . ?
O9A C31A 1.413(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 S6 85.64(4) . . ?
S4 Ni1 S5 93.30(4) . . ?
S4 Ni1 S7 178.69(4) . . ?
S6 Ni1 S5 177.25(4) . . ?
S7 Ni1 S6 93.16(4) . . ?
S7 Ni1 S5 87.88(4) . . ?
S15 Ni2 S15 180.0 2_667 . ?
S15 Ni2 S14 93.32(4) 2_667 2_667 ?
S15 Ni2 S14 86.68(4) . 2_667 ?
S15 Ni2 S14 93.32(4) . . ?
S15 Ni2 S14 86.68(4) 2_667 . ?
S14 Ni2 S14 180.00(5) . 2_667 ?
S20 Ni3 S20 180.00(4) . 2_666 ?
S19 Ni3 S20 93.60(4) 2_666 2_666 ?
S19 Ni3 S20 93.60(4) . . ?
S19 Ni3 S20 86.40(4) 2_666 . ?
S19 Ni3 S20 86.40(4) . 2_666 ?
S19 Ni3 S19 180.0 . 2_666 ?
C3 S4 Ni1 102.40(12) . . ?
C5 S6 Ni1 102.06(14) . . ?
C2 S5 Ni1 101.74(13) . . ?
C4 S7 Ni1 102.28(13) . . ?
C9 S15 Ni2 102.19(13) . . ?
C8 S14 Ni2 101.83(14) . . ?
C7 S13 C9 97.7(2) . . ?
C3 S2 C1 97.98(18) . . ?
C6 S9 C4 97.6(2) . . ?
C12 S20 Ni3 101.66(14) . . ?
C11 S19 Ni3 101.98(14) . . ?
C11 S17 C10 97.0(2) . . ?
C7 S12 C8 97.3(2) . . ?
C6 S8 C5 97.4(2) . . ?
C2 S3 C1 97.86(18) . . ?
C10 S18 C12 97.3(2) . . ?
C26 O7 C27 111.1(3) . . ?
C15 O5 C14 112.1(3) . . ?
C13 O4 C24 111.9(3) . . ?
C17 O6 C16 112.2(3) . . ?
C21 O2 C20 112.9(3) . . ?
C19 O1 C18 113.6(3) . . ?
C23 O3 C22 111.8(3) . . ?
C36 O12 C37 114.9(19) . . ?
C40 O8 C29 111.1(16) . . ?
C38 O13 C39 117.2(16) . . ?
O7 C26 C25 108.6(3) . . ?
S15 C9 S13 122.8(2) . . ?
C8 C9 S15 120.8(3) . . ?
C8 C9 S13 116.3(3) . . ?
S6 C5 S8 122.3(2) . . ?
C4 C5 S6 121.5(3) . . ?
C4 C5 S8 116.3(3) . . ?
O7 C27 C28 109.1(3) . . ?
N1 C25 C26 113.0(3) . . ?
N2 C28 C27 112.6(3) . . ?
S7 C4 S9 123.4(2) . . ?
C5 C4 S7 120.7(3) . . ?
C5 C4 S9 115.8(3) . . ?
S5 C2 S3 123.2(2) . . ?
C3 C2 S5 121.2(3) . . ?
C3 C2 S3 115.7(3) . . ?
O4 C13 C14 109.1(3) . . ?
O2 C21 C22 108.7(3) . . ?
O5 C14 C13 109.0(3) . . ?
S13 C7 S12 112.8(2) . . ?
S11 C7 S13 123.5(3) . . ?
S11 C7 S12 123.7(3) . . ?
S20 C12 S18 122.4(2) . . ?
C11 C12 S20 121.7(3) . . ?
C11 C12 S18 115.9(3) . . ?
O6 C16 C15 109.6(3) . . ?
S4 C3 S2 122.4(2) . . ?
C2 C3 S4 121.3(3) . . ?
C2 C3 S2 116.3(3) . . ?
O3 C22 C21 109.7(3) . . ?
S14 C8 S12 122.4(2) . . ?
C9 C8 S14 121.8(3) . . ?
C9 C8 S12 115.8(3) . . ?
S19 C11 S17 122.5(2) . . ?
C12 C11 S19 121.0(3) . . ?
C12 C11 S17 116.5(3) . . ?
O4 C24 C23 108.7(3) . . ?
O3 C23 C24 109.0(3) . . ?
O1 C18 C17 109.9(3) . . ?
S8 C6 S9 112.8(2) . . ?
S10 C6 S9 124.4(3) . . ?
S10 C6 S8 122.8(3) . . ?
O6 C17 C18 109.2(4) . . ?
S2 C1 S3 112.2(2) . . ?
S1 C1 S2 122.9(2) . . ?
S1 C1 S3 124.9(2) . . ?
C33 O10 C32 114.2(10) . . ?
O5 C15 C16 108.5(3) . . ?
S18 C10 S17 113.3(3) . . ?
S16 C10 S17 122.7(3) . . ?
S16 C10 S18 124.0(3) . . ?
O2 C20 C19 109.0(3) . . ?
O1 C19 C20 108.0(4) . . ?
C35 O11 C34 111.4(12) . . ?
O13 C38 C37 112.1(18) . . ?
O13 C39 C40 114.3(18) . . ?
O12 C37 C38 110.9(16) . . ?
O8 C40 C39 107.3(14) . . ?
O11 C35 C36 108.1(15) . . ?
C30 O9 C31 112.0(10) . . ?
O10 C32 C31 109.8(12) . . ?
O12 C36 C35 108.8(13) . . ?
O11 C34 C33 108.9(9) . . ?
O8 C29 C30 110.1(13) . . ?
O9 C30 C29 108.0(12) . . ?
O8A C29A C30A 108.1(13) . . ?
C37A O12A C36A 113.6(16) . . ?
O12A C37A C38A 112.1(15) . . ?
O12A C36A C35A 108.3(15) . . ?
O13A C38A C37A 107.2(14) . . ?
O11A C35A C36A 107.6(17) . . ?
C38A O13A C39A 108.9(13) . . ?
C34A O11A C35A 109.5(14) . . ?
O13A C39A C40A 103.5(16) . . ?
O11A C34A C33A 110.8(18) . . ?
O8A C40A C39A 112.2(15) . . ?
C40A O8A C29A 110.9(15) . . ?
C32A O10A C33A 114.2(12) . . ?
O9A C30A C29A 109.2(12) . . ?
O10A C32A C31A 111.3(14) . . ?
C30A O9A C31A 111.9(15) . . ?
O10 C33 C34 111.5(10) . . ?
O9 C31 C32 110.5(10) . . ?
O9A C31A C32A 110.0(15) . . ?
O10A C33A C34A 110.9(17) . . ?

_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 2.646
_oxdiff_exptl_absorpt_empirical_full_min 0.543
####################################################################### 
# 
# 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_18c6_nc2oc2n_lt_05_143_00_auto
_database_code_depnum_ccdc_archive 'CCDC 2384652'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2024-09-17 deposited with the CCDC.	2024-11-08 downloaded from the CCDC.
;
_audit_creation_date             2023-12-22
_audit_creation_method           
;
Olex2 1.5-ac5-023
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C6 Ni S10), C4 H14 N2 O, 2(C12 H24 O6)'
_chemical_formula_sum            'C40 H62 N2 Ni2 O13 S20'
_chemical_formula_weight         1537.53
_chemical_melting_point          ?
_chemical_oxdiff_formula         C40H62N2Ni2O13S20
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                   13.0939(3)
_cell_length_b                   14.4272(3)
_cell_length_c                   18.1428(4)
_cell_angle_alpha                90.624(2)
_cell_angle_beta                 100.247(2)
_cell_angle_gamma                104.770(2)
_cell_volume                     3255.51(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    16464
_cell_measurement_temperature    142.90(14)
_cell_measurement_theta_max      30.9910
_cell_measurement_theta_min      2.0270
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.274
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33175
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.67a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark black'
_exptl_crystal_colour_modifier   dark
_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             1592
_exptl_crystal_size_max          0.587
_exptl_crystal_size_mid          0.508
_exptl_crystal_size_min          0.112
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_unetI/netI     0.0552
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.790
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            43224
_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         30.935
_diffrn_reflns_theta_min         2.165
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      142.90(14)
_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    -17.00  28.00   0.50    1.46    --   -5.80 -99.00   0.00   90
  2  ω    -77.00   4.00   0.50    1.46    --   -5.80 -37.00 -90.00  162
  3  ω    -75.00 -43.00   0.50    1.46    --   -5.80 -57.00  30.00   64
  4  ω    -38.00   3.00   0.50    1.46    --   -5.80 -57.00  30.00   82
  5  ω    -15.00  68.00   0.50    1.46    --   -5.80  37.00-150.00  166
  6  ω    -67.00   7.00   0.50    1.46    --   -5.80 -37.00  30.00  148
  7  ω    -11.00  35.00   0.50    1.46    --    6.03 -99.00-150.00   92
;
_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      -0.0160995000
_diffrn_orient_matrix_UB_12      0.0075850000
_diffrn_orient_matrix_UB_13      -0.0384062000
_diffrn_orient_matrix_UB_21      -0.0353762000
_diffrn_orient_matrix_UB_22      -0.0468101000
_diffrn_orient_matrix_UB_23      -0.0051878000
_diffrn_orient_matrix_UB_31      -0.0417281000
_diffrn_orient_matrix_UB_32      0.0185872000
_diffrn_orient_matrix_UB_33      0.0090537000
_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                10577
_reflns_number_total             16302
_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 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.006
_refine_diff_density_min         -1.021
_refine_diff_density_rms         0.090
_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     862
_refine_ls_number_reflns         16302
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0524
_refine_ls_restrained_S_all      1.011
_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)+(0.0568P)²+4.5696P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1199
_refine_ls_wR_factor_ref         0.1391
_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. Rigid body (RIGU) restrains
 C31A, O9A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(C29A)=Sof(H29C)=Sof(H29D)=Sof(O12A)=Sof(C37A)=Sof(H37C)=Sof(H37D)=
 Sof(C36A)=Sof(H36C)=Sof(H36D)=Sof(C38A)=Sof(H38C)=Sof(H38D)=Sof(C35A)=
 Sof(H35C)=Sof(H35D)=Sof(O13A)=Sof(O11A)=Sof(C39A)=Sof(H39C)=Sof(H39D)=
 Sof(C34A)=Sof(H34C)=Sof(H34D)=Sof(C40A)=Sof(H40C)=Sof(H40D)=Sof(O8A)=Sof(O10A)=
 Sof(C30A)=Sof(H30C)=Sof(H30D)=Sof(C32A)=Sof(H32C)=Sof(H32D)=Sof(O9A)=Sof(C31A)=
 Sof(H31C)=Sof(H31D)=Sof(C33A)=Sof(H33C)=Sof(H33D)=1-FVAR(1)
 Sof(O12)=Sof(O8)=Sof(O13)=Sof(O10)=Sof(O11)=Sof(C38)=Sof(H38A)=Sof(H38B)=
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C40)=Sof(H40A)=
 Sof(H40B)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(O9)=Sof(C32)=Sof(H32A)=Sof(H32B)=
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(C29)=Sof(H29A)=
 Sof(H29B)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C31)=
 Sof(H31A)=Sof(H31B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C27(H27A,H27B), C25(H25A,H25B), C28(H28A,H28B), C13(H13A,
 H13B), C21(H21A,H21B), C14(H14A,H14B), C16(H16A,H16B), C22(H22A,H22B),
 C24(H24A,H24B), C23(H23A,H23B), C18(H18A,H18B), C17(H17A,H17B), C15(H15A,H15B),
  C20(H20A,H20B), C19(H19A,H19B), C38(H38A,H38B), C39(H39A,H39B), C37(H37A,
 H37B), C40(H40A,H40B), C35(H35A,H35B), C32(H32A,H32B), C36(H36A,H36B),
 C34(H34A,H34B), C29(H29A,H29B), C30(H30A,H30B), C29A(H29C,H29D), C37A(H37C,
 H37D), C36A(H36C,H36D), C38A(H38C,H38D), C35A(H35C,H35D), C39A(H39C,H39D),
 C34A(H34C,H34D), C40A(H40C,H40D), C30A(H30C,H30D), C32A(H32C,H32D), C33(H33A,
 H33B), C31(H31A,H31B), C31A(H31C,H31D), C33A(H33C,H33D)
4.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(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 0.70123(3) 0.92143(3) 0.98438(3) 0.03078(11) Uani 1 1 d . . . . .
Ni2 Ni 0.500000 0.500000 1.000000 0.03337(15) Uani 1 2 d S . P . .
Ni3 Ni 0.500000 0.500000 0.500000 0.03933(17) Uani 1 2 d S . P . .
S4 S 0.53009(7) 0.90271(6) 0.95915(5) 0.0338(2) Uani 1 1 d . . . . .
S6 S 0.69730(7) 1.00074(7) 1.08489(6) 0.0376(2) Uani 1 1 d . . . . .
S5 S 0.70093(7) 0.83556(6) 0.88556(6) 0.0368(2) Uani 1 1 d . . . . .
S7 S 0.87280(7) 0.94085(7) 1.01236(6) 0.0377(2) Uani 1 1 d . . . . .
S15 S 0.59438(8) 0.64739(7) 1.00904(6) 0.0394(2) Uani 1 1 d . . . . .
S14 S 0.57668(8) 0.47007(7) 1.10955(6) 0.0390(2) Uani 1 1 d . . . . .
S13 S 0.76575(8) 0.76199(7) 1.13557(7) 0.0454(2) Uani 1 1 d . . . . .
S2 S 0.35959(7) 0.78933(7) 0.83372(6) 0.0394(2) Uani 1 1 d . . . . .
S9 S 1.03347(8) 1.02727(8) 1.15440(7) 0.0488(3) Uani 1 1 d . . . . .
S20 S 0.59387(9) 0.49428(8) 0.41451(6) 0.0482(3) Uani 1 1 d . . . . .
S19 S 0.63850(9) 0.57025(8) 0.58312(6) 0.0461(2) Uani 1 1 d . . . . .
S17 S 0.87569(9) 0.62769(8) 0.57560(6) 0.0501(3) Uani 1 1 d . . . . .
S12 S 0.74964(8) 0.59889(8) 1.22807(6) 0.0462(2) Uani 1 1 d . . . . .
S8 S 0.86983(9) 1.07914(8) 1.22144(6) 0.0500(3) Uani 1 1 d . . . . .
S11 S 0.91405(9) 0.78214(9) 1.28231(8) 0.0599(3) Uani 1 1 d . . . . .
S3 S 0.51443(8) 0.71994(7) 0.76867(7) 0.0471(3) Uani 1 1 d . . . . .
S18 S 0.83514(10) 0.55847(10) 0.42045(7) 0.0594(3) Uani 1 1 d . . . . .
S10 S 1.09071(12) 1.11733(9) 1.31031(8) 0.0702(4) Uani 1 1 d . . . . .
S1 S 0.28103(10) 0.65399(11) 0.70017(9) 0.0761(4) Uani 1 1 d . . . . .
S16 S 1.05970(12) 0.64383(13) 0.49774(9) 0.0849(5) Uani 1 1 d . . . . .
O7 O 0.2423(2) 0.67538(17) 0.30655(14) 0.0367(6) Uani 1 1 d . . . . .
O5 O 0.0795(2) 0.71797(18) 0.02884(16) 0.0435(6) Uani 1 1 d . . . . .
O4 O 0.2917(2) 0.73441(18) 0.09951(15) 0.0425(6) Uani 1 1 d . . . . .
O6 O -0.0920(2) 0.5759(2) 0.06659(16) 0.0486(7) Uani 1 1 d . . . . .
O2 O 0.1695(2) 0.42566(17) 0.21243(16) 0.0459(7) Uani 1 1 d . . . . .
O1 O -0.0357(2) 0.41662(19) 0.13894(17) 0.0496(7) Uani 1 1 d . . . . .
O3 O 0.3294(2) 0.5639(2) 0.15839(16) 0.0435(6) Uani 1 1 d . . . . .
N1 N 0.1202(2) 0.60052(19) 0.15480(17) 0.0327(6) Uani 1 1 d . . . . .
H1A H 0.101423 0.623845 0.109417 0.039 Uiso 1 1 calc R U . . .
H1B H 0.087868 0.536536 0.153238 0.039 Uiso 1 1 calc R U . . .
H1C H 0.192861 0.610130 0.165792 0.039 Uiso 1 1 calc R U . . .
O12 O 0.6488(17) 0.8521(15) 0.3702(11) 0.078(6) Uani 0.569(8) 1 d . . P A 1
N2 N 0.4310(3) 0.8151(2) 0.39537(18) 0.0393(7) Uani 1 1 d . . . . .
H2A H 0.393600 0.833062 0.353197 0.047 Uiso 1 1 calc R U . . .
H2B H 0.502731 0.840194 0.397253 0.047 Uiso 1 1 calc R U . . .
H2C H 0.411690 0.837374 0.436519 0.047 Uiso 1 1 calc R U . . .
O8 O 0.4251(16) 0.8612(14) 0.5552(11) 0.058(5) Uani 0.569(8) 1 d . . P A 1
O13 O 0.6036(7) 0.8099(6) 0.5127(5) 0.059(2) Uani 0.569(8) 1 d . . P A 1
C26 C 0.1306(3) 0.6309(3) 0.2912(2) 0.0405(9) Uani 1 1 d . . . . .
H26A H 0.095028 0.656286 0.327706 0.049 Uiso 1 1 calc R U . . .
H26B H 0.117764 0.560741 0.295821 0.049 Uiso 1 1 calc R U . . .
C9 C 0.6721(3) 0.6563(3) 1.0970(2) 0.0370(8) Uani 1 1 d . . . . .
C5 C 0.8281(3) 1.0240(3) 1.1315(2) 0.0389(8) Uani 1 1 d . . . . .
C27 C 0.2891(3) 0.6619(3) 0.3811(2) 0.0452(10) Uani 1 1 d . . . . .
H27A H 0.276940 0.592407 0.388990 0.054 Uiso 1 1 calc R U . . .
H27B H 0.255399 0.690345 0.417120 0.054 Uiso 1 1 calc R U . . .
C25 C 0.0852(3) 0.6512(3) 0.2135(2) 0.0446(10) Uani 1 1 d . . . . .
H25A H 0.005752 0.631535 0.206052 0.054 Uiso 1 1 calc R U . . .
H25B H 0.107624 0.721162 0.207590 0.054 Uiso 1 1 calc R U . . .
C28 C 0.4068(3) 0.7088(3) 0.3940(2) 0.0454(10) Uani 1 1 d . . . . .
H28A H 0.441493 0.689631 0.442293 0.055 Uiso 1 1 calc R U . . .
H28B H 0.437914 0.685808 0.353677 0.055 Uiso 1 1 calc R U . . .
C4 C 0.9045(3) 0.9983(3) 1.0999(2) 0.0407(9) Uani 1 1 d . . . . .
C2 C 0.5663(3) 0.7981(2) 0.8483(2) 0.0347(8) Uani 1 1 d . . . . .
C13 C 0.2666(4) 0.7911(3) 0.0396(3) 0.0514(11) Uani 1 1 d . . . . .
H13A H 0.265843 0.757878 -0.008621 0.062 Uiso 1 1 calc R U . . .
H13B H 0.321869 0.853285 0.044780 0.062 Uiso 1 1 calc R U . . .
C21 C 0.2705(4) 0.4108(3) 0.2067(2) 0.0521(11) Uani 1 1 d . . . . .
H21A H 0.266774 0.381039 0.156481 0.063 Uiso 1 1 calc R U . . .
H21B H 0.290179 0.366752 0.244909 0.063 Uiso 1 1 calc R U . . .
C14 C 0.1587(4) 0.8080(3) 0.0403(3) 0.0524(11) Uani 1 1 d . . . . .
H14A H 0.158886 0.839618 0.089003 0.063 Uiso 1 1 calc R U . . .
H14B H 0.142000 0.850533 0.000030 0.063 Uiso 1 1 calc R U . . .
C7 C 0.8154(3) 0.7182(3) 1.2189(3) 0.0464(10) Uani 1 1 d . . . . .
C12 C 0.7223(3) 0.5445(3) 0.4624(2) 0.0431(9) Uani 1 1 d . . . . .
C16 C -0.1030(3) 0.6332(4) 0.0035(2) 0.0531(11) Uani 1 1 d . . . . .
H16A H -0.177341 0.640164 -0.008216 0.064 Uiso 1 1 calc R U . . .
H16B H -0.088916 0.601301 -0.040783 0.064 Uiso 1 1 calc R U . . .
C3 C 0.4922(3) 0.8287(2) 0.8794(2) 0.0330(8) Uani 1 1 d . . . . .
C22 C 0.3526(3) 0.5041(3) 0.2183(2) 0.0486(10) Uani 1 1 d . . . . .
H22A H 0.352565 0.535975 0.266865 0.058 Uiso 1 1 calc R U . . .
H22B H 0.424800 0.493690 0.219598 0.058 Uiso 1 1 calc R U . . .
C8 C 0.6648(3) 0.5794(3) 1.1402(2) 0.0391(9) Uani 1 1 d . . . . .
C11 C 0.7421(3) 0.5786(3) 0.5351(2) 0.0412(9) Uani 1 1 d . . . . .
C24 C 0.3869(3) 0.7051(3) 0.0961(3) 0.0496(10) Uani 1 1 d . . . . .
H24A H 0.447624 0.762180 0.095368 0.059 Uiso 1 1 calc R U . . .
H24B H 0.376320 0.664421 0.049649 0.059 Uiso 1 1 calc R U . . .
C23 C 0.4113(3) 0.6502(3) 0.1629(3) 0.0518(11) Uani 1 1 d . . . . .
H23A H 0.481601 0.635802 0.164560 0.062 Uiso 1 1 calc R U . . .
H23B H 0.415165 0.688802 0.209262 0.062 Uiso 1 1 calc R U . . .
C18 C -0.1434(3) 0.4269(3) 0.1202(3) 0.0604(13) Uani 1 1 d . . . . .
H18A H -0.159510 0.461590 0.162257 0.073 Uiso 1 1 calc R U . . .
H18B H -0.195109 0.362750 0.111715 0.073 Uiso 1 1 calc R U . . .
C6 C 1.0036(4) 1.0760(3) 1.2331(3) 0.0509(11) Uani 1 1 d . . . . .
C17 C -0.1550(3) 0.4812(3) 0.0511(3) 0.0570(12) Uani 1 1 d . . . . .
H17A H -0.131623 0.450376 0.010438 0.068 Uiso 1 1 calc R U . . .
H17B H -0.231317 0.480807 0.034342 0.068 Uiso 1 1 calc R U . . .
C1 C 0.3791(3) 0.7171(3) 0.7629(3) 0.0483(10) Uani 1 1 d . . . . .
O10 O 0.3006(9) 0.9290(7) 0.3076(6) 0.054(2) Uani 0.569(8) 1 d . . P A 1
C15 C -0.0263(4) 0.7290(3) 0.0200(3) 0.0552(12) Uani 1 1 d . . . . .
H15A H -0.039001 0.770955 -0.021589 0.066 Uiso 1 1 calc R U . . .
H15B H -0.036324 0.759218 0.066577 0.066 Uiso 1 1 calc R U . . .
C10 C 0.9307(4) 0.6125(3) 0.4973(3) 0.0544(11) Uani 1 1 d . . . . .
C20 C 0.0851(4) 0.3380(3) 0.2053(3) 0.0609(13) Uani 1 1 d . . . . .
H20A H 0.098743 0.298812 0.248617 0.073 Uiso 1 1 calc R U . . .
H20B H 0.083218 0.300367 0.158925 0.073 Uiso 1 1 calc R U . . .
C19 C -0.0187(4) 0.3616(3) 0.2026(3) 0.0635(14) Uani 1 1 d . . . . .
H19A H -0.077629 0.301953 0.198297 0.076 Uiso 1 1 calc R U . . .
H19B H -0.017288 0.398975 0.249044 0.076 Uiso 1 1 calc R U . . .
O11 O 0.4810(7) 0.8881(5) 0.2602(4) 0.0561(18) Uani 0.569(8) 1 d . . P A 1
C38 C 0.702(2) 0.8240(13) 0.4967(15) 0.092(8) Uani 0.569(8) 1 d . . P A 1
H38A H 0.741131 0.784227 0.528670 0.111 Uiso 0.569(8) 1 calc R U P A 1
H38B H 0.741501 0.892138 0.509370 0.111 Uiso 0.569(8) 1 calc R U P A 1
C39 C 0.595(2) 0.8397(14) 0.5844(14) 0.076(8) Uani 0.569(8) 1 d . . P A 1
H39A H 0.620163 0.910578 0.590188 0.091 Uiso 0.569(8) 1 calc R U P A 1
H39B H 0.643426 0.813642 0.621972 0.091 Uiso 0.569(8) 1 calc R U P A 1
C37 C 0.7023(11) 0.8004(10) 0.4170(12) 0.092(6) Uani 0.569(8) 1 d . . P A 1
H37A H 0.777491 0.813776 0.409108 0.110 Uiso 0.569(8) 1 calc R U P A 1
H37B H 0.668227 0.731096 0.404930 0.110 Uiso 0.569(8) 1 calc R U P A 1
C40 C 0.4882(10) 0.8103(8) 0.6002(6) 0.078(3) Uani 0.569(8) 1 d . . P A 1
H40A H 0.457963 0.740409 0.588874 0.093 Uiso 0.569(8) 1 calc R U P A 1
H40B H 0.489516 0.824644 0.653952 0.093 Uiso 0.569(8) 1 calc R U P A 1
C35 C 0.5901(15) 0.9175(14) 0.2535(12) 0.082(6) Uani 0.569(8) 1 d . . P A 1
H35A H 0.622929 0.983768 0.275689 0.099 Uiso 0.569(8) 1 calc R U P A 1
H35B H 0.596700 0.916308 0.200016 0.099 Uiso 0.569(8) 1 calc R U P A 1
O9 O 0.2507(7) 0.8711(6) 0.4469(5) 0.054(2) Uani 0.569(8) 1 d . . P A 1
C32 C 0.1924(14) 0.8997(14) 0.3208(8) 0.056(4) Uani 0.569(8) 1 d . . P A 1
H32A H 0.146364 0.932402 0.287102 0.067 Uiso 0.569(8) 1 calc R U P A 1
H32B H 0.163364 0.829576 0.310131 0.067 Uiso 0.569(8) 1 calc R U P A 1
C36 C 0.6470(10) 0.8474(10) 0.2956(9) 0.076(4) Uani 0.569(8) 1 d . . P A 1
H36A H 0.609798 0.781113 0.274974 0.091 Uiso 0.569(8) 1 calc R U P A 1
H36B H 0.721730 0.861675 0.286726 0.091 Uiso 0.569(8) 1 calc R U P A 1
C34 C 0.4218(12) 0.9502(10) 0.2213(7) 0.058(4) Uani 0.569(8) 1 d . . P A 1
H34A H 0.425272 0.947576 0.167257 0.070 Uiso 0.569(8) 1 calc R U P A 1
H34B H 0.453779 1.017296 0.241698 0.070 Uiso 0.569(8) 1 calc R U P A 1
C29 C 0.3177(9) 0.8398(8) 0.5688(5) 0.075(3) Uani 0.569(8) 1 d . . P A 1
H29A H 0.318870 0.854145 0.622494 0.090 Uiso 0.569(8) 1 calc R U P A 1
H29B H 0.282570 0.770639 0.556857 0.090 Uiso 0.569(8) 1 calc R U P A 1
C30 C 0.2559(18) 0.8974(14) 0.5222(8) 0.061(5) Uani 0.569(8) 1 d . . P A 1
H30A H 0.182590 0.885095 0.533507 0.073 Uiso 0.569(8) 1 calc R U P A 1
H30B H 0.291773 0.966694 0.532633 0.073 Uiso 0.569(8) 1 calc R U P A 1
C29A C 0.3310(11) 0.9106(8) 0.5515(8) 0.054(3) Uani 0.431(8) 1 d . . P A 2
H29C H 0.366465 0.980300 0.555425 0.065 Uiso 0.431(8) 1 calc R U P A 2
H29D H 0.305024 0.892816 0.598691 0.065 Uiso 0.431(8) 1 calc R U P A 2
O12A O 0.659(2) 0.8508(18) 0.3823(11) 0.049(5) Uani 0.431(8) 1 d . . P A 2
C37A C 0.7399(10) 0.8370(10) 0.4437(9) 0.045(3) Uani 0.431(8) 1 d . . P A 2
H37C H 0.792077 0.899553 0.460638 0.055 Uiso 0.431(8) 1 calc R U P A 2
H37D H 0.779342 0.793711 0.426068 0.055 Uiso 0.431(8) 1 calc R U P A 2
C36A C 0.7076(12) 0.8968(9) 0.3244(7) 0.059(3) Uani 0.431(8) 1 d . . P A 2
H36C H 0.764329 0.867121 0.314114 0.071 Uiso 0.431(8) 1 calc R U P A 2
H36D H 0.740670 0.965786 0.338930 0.071 Uiso 0.431(8) 1 calc R U P A 2
C38A C 0.6917(18) 0.7957(14) 0.5072(13) 0.046(4) Uani 0.431(8) 1 d . . P A 2
H38C H 0.651631 0.727720 0.494699 0.055 Uiso 0.431(8) 1 calc R U P A 2
H38D H 0.748152 0.798999 0.552150 0.055 Uiso 0.431(8) 1 calc R U P A 2
C35A C 0.6228(18) 0.8854(14) 0.2582(11) 0.058(5) Uani 0.431(8) 1 d . . P A 2
H35C H 0.653526 0.915709 0.215565 0.069 Uiso 0.431(8) 1 calc R U P A 2
H35D H 0.590455 0.816246 0.244074 0.069 Uiso 0.431(8) 1 calc R U P A 2
O13A O 0.6188(9) 0.8529(6) 0.5214(6) 0.040(2) Uani 0.431(8) 1 d . . P A 2
O11A O 0.5423(13) 0.9290(8) 0.2738(5) 0.061(3) Uani 0.431(8) 1 d . . P A 2
C39A C 0.576(2) 0.8190(16) 0.5902(15) 0.043(5) Uani 0.431(8) 1 d . . P A 2
H39C H 0.634685 0.829051 0.634701 0.052 Uiso 0.431(8) 1 calc R U P A 2
H39D H 0.536559 0.750247 0.583749 0.052 Uiso 0.431(8) 1 calc R U P A 2
C34A C 0.4666(18) 0.9294(14) 0.2103(12) 0.070(5) Uani 0.431(8) 1 d . . P A 2
H34C H 0.435557 0.862963 0.188168 0.084 Uiso 0.431(8) 1 calc R U P A 2
H34D H 0.501965 0.968261 0.172763 0.084 Uiso 0.431(8) 1 calc R U P A 2
C40A C 0.5014(10) 0.8830(7) 0.5963(6) 0.047(3) Uani 0.431(8) 1 d . . P A 2
H40C H 0.480076 0.877491 0.646098 0.056 Uiso 0.431(8) 1 calc R U P A 2
H40D H 0.539848 0.950713 0.591980 0.056 Uiso 0.431(8) 1 calc R U P A 2
O8A O 0.4062(16) 0.8559(17) 0.5381(13) 0.035(3) Uani 0.431(8) 1 d . . P A 2
O10A O 0.3231(10) 0.9127(7) 0.2792(9) 0.055(3) Uani 0.431(8) 1 d . . P A 2
C30A C 0.2374(18) 0.8861(14) 0.4848(15) 0.070(9) Uani 0.431(8) 1 d . . P A 2
H30C H 0.207051 0.815683 0.478207 0.084 Uiso 0.431(8) 1 calc R U P A 2
H30D H 0.180061 0.915605 0.494163 0.084 Uiso 0.431(8) 1 calc R U P A 2
C32A C 0.2323(16) 0.9398(12) 0.2923(10) 0.073(6) Uani 0.431(8) 1 d . . P A 2
H32C H 0.174501 0.920873 0.247425 0.087 Uiso 0.431(8) 1 calc R U P A 2
H32D H 0.250381 1.010553 0.300394 0.087 Uiso 0.431(8) 1 calc R U P A 2
O9A O 0.2727(6) 0.9197(6) 0.4220(5) 0.052(2) Uani 0.431(8) 1 d . . P A 2
C33 C 0.3089(10) 0.9188(8) 0.2309(6) 0.059(3) Uani 0.569(8) 1 d . . P A 1
H33A H 0.266580 0.957659 0.200618 0.071 Uiso 0.569(8) 1 calc R U P A 1
H33B H 0.278419 0.850766 0.212575 0.071 Uiso 0.569(8) 1 calc R U P A 1
C31 C 0.1915(9) 0.9241(7) 0.3977(7) 0.059(3) Uani 0.569(8) 1 d . . P A 1
H31A H 0.223976 0.993800 0.408918 0.070 Uiso 0.569(8) 1 calc R U P A 1
H31B H 0.116377 0.909246 0.405817 0.070 Uiso 0.569(8) 1 calc R U P A 1
C31A C 0.1927(18) 0.8952(18) 0.3581(13) 0.076(8) Uani 0.431(8) 1 d . . P A 2
H31C H 0.129378 0.916999 0.365922 0.091 Uiso 0.431(8) 1 calc R U P A 2
H31D H 0.169920 0.824493 0.348880 0.091 Uiso 0.431(8) 1 calc R U P A 2
C33A C 0.378(2) 0.9697(16) 0.2275(13) 0.073(6) Uani 0.431(8) 1 d . . P A 2
H33C H 0.409010 1.036346 0.249278 0.088 Uiso 0.431(8) 1 calc R U P A 2
H33D H 0.327125 0.971244 0.180624 0.088 Uiso 0.431(8) 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 S4 2.1513(9) . ?
Ni1 S6 2.1576(11) . ?
Ni1 S5 2.1668(11) . ?
Ni1 S7 2.1572(10) . ?
Ni2 S15 2.1578(10) 2_667 ?
Ni2 S15 2.1578(10) . ?
Ni2 S14 2.1621(10) . ?
Ni2 S14 2.1621(10) 2_667 ?
Ni3 S20 2.1565(10) 2_666 ?
Ni3 S20 2.1565(10) . ?
Ni3 S19 2.1556(11) . ?
Ni3 S19 2.1557(11) 2_666 ?
S4 C3 1.709(4) . ?
S6 C5 1.716(4) . ?
S5 C2 1.714(4) . ?
S7 C4 1.715(4) . ?
S15 C9 1.717(4) . ?
S14 C8 1.719(4) . ?
S13 C9 1.743(4) . ?
S13 C7 1.728(5) . ?
S2 C3 1.732(4) . ?
S2 C1 1.739(4) . ?
S9 C4 1.744(4) . ?
S9 C6 1.734(5) . ?
S20 C12 1.719(4) . ?
S19 C11 1.719(4) . ?
S17 C11 1.732(4) . ?
S17 C10 1.737(5) . ?
S12 C7 1.742(4) . ?
S12 C8 1.748(4) . ?
S8 C5 1.741(4) . ?
S8 C6 1.738(5) . ?
S11 C7 1.639(5) . ?
S3 C2 1.745(4) . ?
S3 C1 1.747(4) . ?
S18 C12 1.748(4) . ?
S18 C10 1.725(5) . ?
S10 C6 1.638(5) . ?
S1 C1 1.623(4) . ?
S16 C10 1.633(5) . ?
O7 C26 1.415(4) . ?
O7 C27 1.419(5) . ?
O5 C14 1.427(5) . ?
O5 C15 1.417(5) . ?
O4 C13 1.410(5) . ?
O4 C24 1.425(5) . ?
O6 C16 1.427(5) . ?
O6 C17 1.399(5) . ?
O2 C21 1.415(5) . ?
O2 C20 1.438(5) . ?
O1 C18 1.437(5) . ?
O1 C19 1.426(6) . ?
O3 C22 1.433(5) . ?
O3 C23 1.411(5) . ?
N1 C25 1.485(5) . ?
O12 C37 1.36(3) . ?
O12 C36 1.35(2) . ?
N2 C28 1.484(5) . ?
O8 C40 1.40(2) . ?
O8 C29 1.428(19) . ?
O13 C38 1.34(3) . ?
O13 C39 1.40(3) . ?
C26 C25 1.492(6) . ?
C9 C8 1.359(5) . ?
C5 C4 1.362(6) . ?
C27 C28 1.491(6) . ?
C2 C3 1.366(5) . ?
C13 C14 1.495(6) . ?
C21 C22 1.480(6) . ?
C12 C11 1.358(6) . ?
C16 C15 1.478(7) . ?
C24 C23 1.487(6) . ?
C18 C17 1.490(7) . ?
O10 C32 1.44(2) . ?
O10 C33 1.422(14) . ?
C20 C19 1.476(7) . ?
O11 C35 1.410(18) . ?
O11 C34 1.442(15) . ?
C38 C37 1.48(3) . ?
C39 C40 1.44(3) . ?
C35 C36 1.54(2) . ?
O9 C30 1.398(16) . ?
O9 C31 1.434(13) . ?
C32 C31 1.436(18) . ?
C34 C33 1.474(18) . ?
C29 C30 1.47(2) . ?
C29A O8A 1.46(2) . ?
C29A C30A 1.53(3) . ?
O12A C37A 1.45(3) . ?
O12A C36A 1.41(2) . ?
C37A C38A 1.47(3) . ?
C36A C35A 1.46(2) . ?
C38A O13A 1.463(18) . ?
C35A O11A 1.42(2) . ?
O13A C39A 1.49(3) . ?
O11A C34A 1.38(2) . ?
C39A C40A 1.52(2) . ?
C34A C33A 1.50(2) . ?
C40A O8A 1.45(3) . ?
O10A C32A 1.399(19) . ?
O10A C33A 1.43(3) . ?
C30A O9A 1.35(3) . ?
C32A C31A 1.47(3) . ?
O9A C31A 1.39(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
S4 Ni1 S6 85.60(4) . . ?
S4 Ni1 S5 93.33(4) . . ?
S4 Ni1 S7 178.68(5) . . ?
S6 Ni1 S5 177.23(4) . . ?
S7 Ni1 S6 93.17(4) . . ?
S7 Ni1 S5 87.88(4) . . ?
S15 Ni2 S15 180.00(5) . 2_667 ?
S15 Ni2 S14 86.67(4) . 2_667 ?
S15 Ni2 S14 93.33(4) 2_667 2_667 ?
S15 Ni2 S14 86.67(4) 2_667 . ?
S15 Ni2 S14 93.33(4) . . ?
S14 Ni2 S14 180.00(5) . 2_667 ?
S20 Ni3 S20 180.0 2_666 . ?
S19 Ni3 S20 86.50(4) 2_666 . ?
S19 Ni3 S20 86.50(4) . 2_666 ?
S19 Ni3 S20 93.50(4) 2_666 2_666 ?
S19 Ni3 S20 93.50(4) . . ?
S19 Ni3 S19 180.0 . 2_666 ?
C3 S4 Ni1 102.43(12) . . ?
C5 S6 Ni1 102.09(14) . . ?
C2 S5 Ni1 101.65(13) . . ?
C4 S7 Ni1 102.25(13) . . ?
C9 S15 Ni2 102.20(13) . . ?
C8 S14 Ni2 101.92(14) . . ?
C7 S13 C9 97.7(2) . . ?
C3 S2 C1 97.87(19) . . ?
C6 S9 C4 97.8(2) . . ?
C12 S20 Ni3 101.75(14) . . ?
C11 S19 Ni3 102.25(15) . . ?
C11 S17 C10 97.4(2) . . ?
C7 S12 C8 97.3(2) . . ?
C6 S8 C5 97.4(2) . . ?
C2 S3 C1 97.84(18) . . ?
C10 S18 C12 97.4(2) . . ?
C26 O7 C27 111.3(3) . . ?
C15 O5 C14 112.2(3) . . ?
C13 O4 C24 111.9(3) . . ?
C17 O6 C16 112.3(3) . . ?
C21 O2 C20 113.2(3) . . ?
C19 O1 C18 113.6(3) . . ?
C23 O3 C22 111.6(3) . . ?
C36 O12 C37 121.1(15) . . ?
C40 O8 C29 112.3(16) . . ?
C38 O13 C39 118.0(16) . . ?
O7 C26 C25 108.8(3) . . ?
S15 C9 S13 122.9(2) . . ?
C8 C9 S15 121.1(3) . . ?
C8 C9 S13 116.0(3) . . ?
S6 C5 S8 122.3(2) . . ?
C4 C5 S6 121.2(3) . . ?
C4 C5 S8 116.5(3) . . ?
O7 C27 C28 109.1(3) . . ?
N1 C25 C26 113.0(3) . . ?
N2 C28 C27 112.7(3) . . ?
S7 C4 S9 123.5(2) . . ?
C5 C4 S7 121.0(3) . . ?
C5 C4 S9 115.5(3) . . ?
S5 C2 S3 123.1(2) . . ?
C3 C2 S5 121.5(3) . . ?
C3 C2 S3 115.4(3) . . ?
O4 C13 C14 109.2(3) . . ?
O2 C21 C22 109.2(3) . . ?
O5 C14 C13 109.0(3) . . ?
S13 C7 S12 112.8(2) . . ?
S11 C7 S13 123.5(3) . . ?
S11 C7 S12 123.6(3) . . ?
S20 C12 S18 122.5(2) . . ?
C11 C12 S20 121.8(3) . . ?
C11 C12 S18 115.7(3) . . ?
O6 C16 C15 110.0(4) . . ?
S4 C3 S2 122.4(2) . . ?
C2 C3 S4 121.0(3) . . ?
C2 C3 S2 116.6(3) . . ?
O3 C22 C21 109.5(3) . . ?
S14 C8 S12 122.6(2) . . ?
C9 C8 S14 121.4(3) . . ?
C9 C8 S12 116.0(3) . . ?
S19 C11 S17 122.9(2) . . ?
C12 C11 S19 120.7(3) . . ?
C12 C11 S17 116.4(3) . . ?
O4 C24 C23 108.8(3) . . ?
O3 C23 C24 109.0(3) . . ?
O1 C18 C17 109.8(3) . . ?
S9 C6 S8 112.7(2) . . ?
S10 C6 S9 124.6(3) . . ?
S10 C6 S8 122.6(3) . . ?
O6 C17 C18 109.3(4) . . ?
S2 C1 S3 112.2(2) . . ?
S1 C1 S2 122.9(2) . . ?
S1 C1 S3 124.9(2) . . ?
C33 O10 C32 113.9(11) . . ?
O5 C15 C16 108.6(3) . . ?
S18 C10 S17 113.0(3) . . ?
S16 C10 S17 123.1(3) . . ?
S16 C10 S18 123.8(3) . . ?
O2 C20 C19 109.1(3) . . ?
O1 C19 C20 107.9(4) . . ?
C35 O11 C34 110.6(12) . . ?
O13 C38 C37 113.9(19) . . ?
O13 C39 C40 114.3(19) . . ?
O12 C37 C38 111.5(14) . . ?
O8 C40 C39 107.8(14) . . ?
O11 C35 C36 107.3(14) . . ?
C30 O9 C31 111.3(11) . . ?
C31 C32 O10 109.5(12) . . ?
O12 C36 C35 112.9(13) . . ?
O11 C34 C33 109.2(9) . . ?
O8 C29 C30 110.1(14) . . ?
O9 C30 C29 107.9(13) . . ?
O8A C29A C30A 106.8(13) . . ?
C36A O12A C37A 110.4(19) . . ?
O12A C37A C38A 111.5(15) . . ?
O12A C36A C35A 106.7(16) . . ?
O13A C38A C37A 106.5(14) . . ?
O11A C35A C36A 109.7(16) . . ?
C38A O13A C39A 108.0(13) . . ?
C34A O11A C35A 111.7(14) . . ?
O13A C39A C40A 101.6(15) . . ?
O11A C34A C33A 112(2) . . ?
O8A C40A C39A 111.0(15) . . ?
C40A O8A C29A 109.2(15) . . ?
C32A O10A C33A 114.0(13) . . ?
O9A C30A C29A 109.4(15) . . ?
O10A C32A C31A 112.1(15) . . ?
C30A O9A C31A 112.5(17) . . ?
O10 C33 C34 111.1(10) . . ?
O9 C31 C32 110.3(10) . . ?
O9A C31A C32A 110.5(17) . . ?
O10A C33A C34A 110.5(18) . . ?

_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 2.908
_oxdiff_exptl_absorpt_empirical_full_min 0.528
####################################################################### 
# 
# 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_18c6_nc2oc2n_lt_07_163_00_auto
_database_code_depnum_ccdc_archive 'CCDC 2384654'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2024-09-17 deposited with the CCDC.	2024-11-08 downloaded from the CCDC.
;
_audit_creation_date             2023-12-22
_audit_creation_method           
;
Olex2 1.5-ac5-023
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C6 Ni S10), C4 H14 N2 O, 2(C12 H24 O6)'
_chemical_formula_sum            'C40 H62 N2 Ni2 O13 S20'
_chemical_formula_weight         1537.53
_chemical_melting_point          ?
_chemical_oxdiff_formula         C40H62N2Ni2O13S20
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                   13.1048(4)
_cell_length_b                   14.4438(3)
_cell_length_c                   18.1407(5)
_cell_angle_alpha                90.492(2)
_cell_angle_beta                 100.298(2)
_cell_angle_gamma                104.682(2)
_cell_volume                     3262.86(15)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    15764
_cell_measurement_temperature    163.00(14)
_cell_measurement_theta_max      31.0130
_cell_measurement_theta_min      2.0300
_shelx_estimated_absorpt_T_max   0.910
_shelx_estimated_absorpt_T_min   0.487
_exptl_absorpt_coefficient_mu    1.271
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.408
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.67a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark black'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-18 0 4 0.2163
1 -18 -9 0.2329
18 0 -4 0.3226
0 18 9 0.2227
-1 0 -25 0.0444
2 0 25 0.0250

_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.551
_exptl_crystal_size_min          0.076
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-17.8472 -0.0526 3.8204 0.1477 0.6131 0.7761
1.3119 -18.2679 -9.3610 0.2044 0.8526 -0.4810
17.7710 0.3512 -3.6556 -0.1506 -0.6251 -0.7659
-0.3532 18.0724 9.0572 -0.2100 -0.8758 0.4347
-1.2603 -0.3428 -24.6869 0.9672 0.1794 -0.1801
1.5971 0.1122 24.5835 -0.9704 -0.1800 0.1608

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0574
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.792
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            43468
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.792
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.918
_diffrn_reflns_theta_min         2.163
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      163.00(14)
_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 0.792
_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    1.46    --   -5.80 -99.00   0.00   90
  2  ω    -77.00   4.00   0.50    1.46    --   -5.80 -37.00 -90.00  162
  3  ω    -75.00 -43.00   0.50    1.46    --   -5.80 -57.00  30.00   64
  4  ω    -38.00   3.00   0.50    1.46    --   -5.80 -57.00  30.00   82
  5  ω    -15.00  68.00   0.50    1.46    --   -5.80  37.00-150.00  166
  6  ω    -67.00   7.00   0.50    1.46    --   -5.80 -37.00  30.00  148
  7  ω    -11.00  35.00   0.50    1.46    --    6.03 -99.00-150.00   92
;
_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      -0.0165233000
_diffrn_orient_matrix_UB_12      0.0073196000
_diffrn_orient_matrix_UB_13      -0.0384353000
_diffrn_orient_matrix_UB_21      -0.0352436000
_diffrn_orient_matrix_UB_22      -0.0467327000
_diffrn_orient_matrix_UB_23      -0.0048173000
_diffrn_orient_matrix_UB_31      -0.0415814000
_diffrn_orient_matrix_UB_32      0.0186507000
_diffrn_orient_matrix_UB_33      0.0091577000
_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                10269
_reflns_number_total             16348
_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 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.882
_refine_diff_density_min         -0.878
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     862
_refine_ls_number_reflns         16348
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1007
_refine_ls_R_factor_gt           0.0540
_refine_ls_restrained_S_all      1.028
_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)+(0.0593P)²+3.3280P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1235
_refine_ls_wR_factor_ref         0.1433
_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. Rigid body (RIGU) restrains
 C31A, O9A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C38, O13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(C29A)=Sof(H29C)=Sof(H29D)=Sof(O12A)=Sof(C37A)=Sof(H37C)=Sof(H37D)=
 Sof(C36A)=Sof(H36C)=Sof(H36D)=Sof(C38A)=Sof(H38C)=Sof(H38D)=Sof(C35A)=
 Sof(H35C)=Sof(H35D)=Sof(O13A)=Sof(O11A)=Sof(C39A)=Sof(H39C)=Sof(H39D)=
 Sof(C34A)=Sof(H34C)=Sof(H34D)=Sof(C40A)=Sof(H40C)=Sof(H40D)=Sof(O8A)=Sof(O10A)=
 Sof(C30A)=Sof(H30C)=Sof(H30D)=Sof(C32A)=Sof(H32C)=Sof(H32D)=Sof(O9A)=Sof(C31A)=
 Sof(H31C)=Sof(H31D)=Sof(C33A)=Sof(H33C)=Sof(H33D)=1-FVAR(1)
 Sof(O12)=Sof(O8)=Sof(O13)=Sof(O10)=Sof(O11)=Sof(C38)=Sof(H38A)=Sof(H38B)=
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C40)=Sof(H40A)=
 Sof(H40B)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(O9)=Sof(C32)=Sof(H32A)=Sof(H32B)=
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(C29)=Sof(H29A)=
 Sof(H29B)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C31)=
 Sof(H31A)=Sof(H31B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C27(H27A,H27B), C25(H25A,H25B), C28(H28A,H28B), C13(H13A,
 H13B), C21(H21A,H21B), C14(H14A,H14B), C16(H16A,H16B), C22(H22A,H22B),
 C24(H24A,H24B), C23(H23A,H23B), C18(H18A,H18B), C17(H17A,H17B), C15(H15A,H15B),
  C20(H20A,H20B), C19(H19A,H19B), C38(H38A,H38B), C39(H39A,H39B), C37(H37A,
 H37B), C40(H40A,H40B), C35(H35A,H35B), C32(H32A,H32B), C36(H36A,H36B),
 C34(H34A,H34B), C29(H29A,H29B), C30(H30A,H30B), C29A(H29C,H29D), C37A(H37C,
 H37D), C36A(H36C,H36D), C38A(H38C,H38D), C35A(H35C,H35D), C39A(H39C,H39D),
 C34A(H34C,H34D), C40A(H40C,H40D), C30A(H30C,H30D), C32A(H32C,H32D), C33(H33A,
 H33B), C31(H31A,H31B), C31A(H31C,H31D), C33A(H33C,H33D)
4.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(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 0.70112(3) 0.92147(3) 0.98457(3) 0.03488(12) Uani 1 1 d . . . . .
Ni2 Ni 0.500000 0.500000 1.000000 0.03751(16) Uani 1 2 d S . P . .
Ni3 Ni 0.500000 0.500000 0.500000 0.04451(18) Uani 1 2 d S . P . .
S4 S 0.53014(7) 0.90268(6) 0.95937(6) 0.0381(2) Uani 1 1 d . . . . .
S6 S 0.69689(7) 1.00018(7) 1.08507(6) 0.0422(2) Uani 1 1 d . . . . .
S5 S 0.70092(7) 0.83598(7) 0.88588(6) 0.0413(2) Uani 1 1 d . . . . .
S7 S 0.87259(7) 0.94109(7) 1.01253(6) 0.0428(2) Uani 1 1 d . . . . .
S15 S 0.59345(8) 0.64730(7) 1.00898(6) 0.0445(2) Uani 1 1 d . . . . .
S14 S 0.57693(8) 0.47009(7) 1.10960(6) 0.0439(2) Uani 1 1 d . . . . .
S13 S 0.76424(8) 0.76169(7) 1.13531(7) 0.0514(3) Uani 1 1 d . . . . .
S2 S 0.35999(7) 0.78946(7) 0.83421(6) 0.0440(2) Uani 1 1 d . . . . .
S9 S 1.03298(8) 1.02746(8) 1.15442(7) 0.0553(3) Uani 1 1 d . . . . .
S20 S 0.59378(9) 0.49359(8) 0.41471(6) 0.0549(3) Uani 1 1 d . . . . .
S19 S 0.63821(9) 0.57103(8) 0.58273(6) 0.0522(3) Uani 1 1 d . . . . .
S17 S 0.87496(10) 0.62851(8) 0.57504(7) 0.0567(3) Uani 1 1 d . . . . .
S12 S 0.74933(9) 0.59864(8) 1.22787(6) 0.0518(3) Uani 1 1 d . . . . .
S8 S 0.86918(9) 1.07859(8) 1.22143(7) 0.0560(3) Uani 1 1 d . . . . .
S11 S 0.91247(9) 0.78183(9) 1.28199(8) 0.0677(3) Uani 1 1 d . . . . .
S3 S 0.51483(8) 0.72065(8) 0.76923(7) 0.0514(3) Uani 1 1 d . . . . .
S18 S 0.83442(10) 0.55779(10) 0.42044(7) 0.0671(3) Uani 1 1 d . . . . .
S10 S 1.08994(12) 1.11733(9) 1.30996(9) 0.0800(4) Uani 1 1 d . . . . .
S1 S 0.28177(10) 0.65434(11) 0.70110(9) 0.0809(5) Uani 1 1 d . . . . .
S16 S 1.05849(12) 0.64423(14) 0.49739(9) 0.0951(5) Uani 1 1 d . . . . .
O7 O 0.2417(2) 0.67476(17) 0.30684(14) 0.0411(6) Uani 1 1 d . . . . .
O5 O 0.0782(2) 0.71749(19) 0.02876(16) 0.0505(7) Uani 1 1 d . . . . .
O4 O 0.2905(2) 0.73449(18) 0.09930(16) 0.0490(7) Uani 1 1 d . . . . .
O6 O -0.0919(2) 0.5751(2) 0.06682(17) 0.0569(8) Uani 1 1 d . . . . .
O2 O 0.1706(2) 0.42592(18) 0.21244(17) 0.0529(7) Uani 1 1 d . . . . .
O1 O -0.0346(2) 0.4163(2) 0.13949(18) 0.0576(8) Uani 1 1 d . . . . .
O3 O 0.3298(2) 0.5646(2) 0.15830(16) 0.0496(7) Uani 1 1 d . . . . .
N1 N 0.1202(2) 0.60038(19) 0.15514(17) 0.0368(7) Uani 1 1 d . . . . .
H1A H 0.100648 0.623372 0.109685 0.044 Uiso 1 1 calc R U . . .
H1B H 0.088967 0.536334 0.153813 0.044 Uiso 1 1 calc R U . . .
H1C H 0.192892 0.610893 0.165958 0.044 Uiso 1 1 calc R U . . .
O12 O 0.6453(19) 0.8512(17) 0.3667(12) 0.083(7) Uani 0.584(8) 1 d . . P A 1
N2 N 0.4295(3) 0.8145(2) 0.39558(19) 0.0445(8) Uani 1 1 d . . . . .
H2A H 0.391733 0.831951 0.353292 0.053 Uiso 1 1 calc R U . . .
H2B H 0.501011 0.839766 0.397281 0.053 Uiso 1 1 calc R U . . .
H2C H 0.410143 0.836809 0.436637 0.053 Uiso 1 1 calc R U . . .
O8 O 0.4274(13) 0.8625(12) 0.5558(10) 0.064(5) Uani 0.584(8) 1 d . . P A 1
O13 O 0.6042(8) 0.8117(7) 0.5119(6) 0.066(2) Uani 0.584(8) 1 d . . P A 1
C26 C 0.1303(3) 0.6303(3) 0.2916(2) 0.0463(9) Uani 1 1 d . . . . .
H26A H 0.094716 0.655565 0.328072 0.056 Uiso 1 1 calc R U . . .
H26B H 0.117772 0.560247 0.296412 0.056 Uiso 1 1 calc R U . . .
C9 C 0.6713(3) 0.6562(3) 1.0968(2) 0.0420(9) Uani 1 1 d . . . . .
C5 C 0.8276(3) 1.0236(3) 1.1315(2) 0.0444(9) Uani 1 1 d . . . . .
C27 C 0.2887(4) 0.6614(3) 0.3814(2) 0.0511(10) Uani 1 1 d . . . . .
H27A H 0.276777 0.591995 0.389319 0.061 Uiso 1 1 calc R U . . .
H27B H 0.254626 0.689505 0.417296 0.061 Uiso 1 1 calc R U . . .
C25 C 0.0845(3) 0.6502(3) 0.2138(2) 0.0501(10) Uani 1 1 d . . . . .
H25A H 0.005152 0.629983 0.206435 0.060 Uiso 1 1 calc R U . . .
H25B H 0.105970 0.720192 0.207875 0.060 Uiso 1 1 calc R U . . .
C28 C 0.4061(4) 0.7083(3) 0.3948(3) 0.0524(11) Uani 1 1 d . . . . .
H28A H 0.440391 0.689512 0.443510 0.063 Uiso 1 1 calc R U . . .
H28B H 0.437936 0.685256 0.355011 0.063 Uiso 1 1 calc R U . . .
C4 C 0.9043(3) 0.9985(3) 1.1000(2) 0.0455(9) Uani 1 1 d . . . . .
C2 C 0.5665(3) 0.7986(2) 0.8488(2) 0.0382(8) Uani 1 1 d . . . . .
C13 C 0.2651(4) 0.7908(3) 0.0395(3) 0.0593(12) Uani 1 1 d . . . . .
H13A H 0.264755 0.757856 -0.008620 0.071 Uiso 1 1 calc R U . . .
H13B H 0.319843 0.853083 0.044725 0.071 Uiso 1 1 calc R U . . .
C21 C 0.2712(4) 0.4112(3) 0.2064(3) 0.0608(12) Uani 1 1 d . . . . .
H21A H 0.267379 0.381982 0.156077 0.073 Uiso 1 1 calc R U . . .
H21B H 0.291106 0.366998 0.244453 0.073 Uiso 1 1 calc R U . . .
C14 C 0.1571(4) 0.8072(3) 0.0397(3) 0.0602(12) Uani 1 1 d . . . . .
H14A H 0.156925 0.839194 0.088185 0.072 Uiso 1 1 calc R U . . .
H14B H 0.140171 0.849368 -0.000890 0.072 Uiso 1 1 calc R U . . .
C7 C 0.8146(3) 0.7178(3) 1.2187(3) 0.0519(10) Uani 1 1 d . . . . .
C12 C 0.7220(3) 0.5442(3) 0.4624(2) 0.0490(10) Uani 1 1 d . . . . .
C16 C -0.1033(4) 0.6332(4) 0.0038(3) 0.0626(13) Uani 1 1 d . . . . .
H16A H -0.177567 0.640285 -0.007588 0.075 Uiso 1 1 calc R U . . .
H16B H -0.089579 0.601681 -0.040740 0.075 Uiso 1 1 calc R U . . .
C3 C 0.4921(3) 0.8288(2) 0.8796(2) 0.0364(8) Uani 1 1 d . . . . .
C22 C 0.3531(4) 0.5049(3) 0.2182(3) 0.0561(11) Uani 1 1 d . . . . .
H22A H 0.352639 0.536501 0.266779 0.067 Uiso 1 1 calc R U . . .
H22B H 0.425396 0.494770 0.219742 0.067 Uiso 1 1 calc R U . . .
C8 C 0.6643(3) 0.5788(3) 1.1401(2) 0.0424(9) Uani 1 1 d . . . . .
C11 C 0.7419(3) 0.5789(3) 0.5348(2) 0.0472(9) Uani 1 1 d . . . . .
C24 C 0.3859(3) 0.7054(3) 0.0962(3) 0.0581(12) Uani 1 1 d . . . . .
H24A H 0.446486 0.762427 0.095605 0.070 Uiso 1 1 calc R U . . .
H24B H 0.375784 0.664836 0.049891 0.070 Uiso 1 1 calc R U . . .
C23 C 0.4102(3) 0.6508(3) 0.1629(3) 0.0591(11) Uani 1 1 d . . . . .
H23A H 0.480846 0.637012 0.164982 0.071 Uiso 1 1 calc R U . . .
H23B H 0.413166 0.689061 0.209135 0.071 Uiso 1 1 calc R U . . .
C18 C -0.1426(4) 0.4264(4) 0.1205(3) 0.0721(15) Uani 1 1 d . . . . .
H18A H -0.159295 0.460336 0.162638 0.086 Uiso 1 1 calc R U . . .
H18B H -0.193992 0.362228 0.111601 0.086 Uiso 1 1 calc R U . . .
C6 C 1.0028(4) 1.0759(3) 1.2328(3) 0.0580(12) Uani 1 1 d . . . . .
C17 C -0.1540(4) 0.4813(4) 0.0519(3) 0.0677(14) Uani 1 1 d . . . . .
H17A H -0.130662 0.450650 0.011095 0.081 Uiso 1 1 calc R U . . .
H17B H -0.230260 0.480859 0.035070 0.081 Uiso 1 1 calc R U . . .
C1 C 0.3796(3) 0.7172(3) 0.7634(3) 0.0518(10) Uani 1 1 d . . . . .
O10 O 0.2965(10) 0.9281(7) 0.3082(6) 0.062(3) Uani 0.584(8) 1 d . . P A 1
C15 C -0.0271(4) 0.7285(4) 0.0202(3) 0.0643(13) Uani 1 1 d . . . . .
H15A H -0.039961 0.770417 -0.021474 0.077 Uiso 1 1 calc R U . . .
H15B H -0.036962 0.758480 0.066730 0.077 Uiso 1 1 calc R U . . .
C10 C 0.9297(4) 0.6125(3) 0.4971(3) 0.0606(12) Uani 1 1 d . . . . .
C20 C 0.0864(5) 0.3386(3) 0.2054(3) 0.0708(15) Uani 1 1 d . . . . .
H20A H 0.100374 0.299207 0.248594 0.085 Uiso 1 1 calc R U . . .
H20B H 0.084399 0.301225 0.158920 0.085 Uiso 1 1 calc R U . . .
C19 C -0.0171(5) 0.3613(3) 0.2030(3) 0.0741(15) Uani 1 1 d . . . . .
H19A H -0.075551 0.301494 0.198703 0.089 Uiso 1 1 calc R U . . .
H19B H -0.015849 0.398261 0.249515 0.089 Uiso 1 1 calc R U . . .
O11 O 0.4780(7) 0.8879(5) 0.2597(5) 0.064(2) Uani 0.584(8) 1 d . . P A 1
C38 C 0.7064(17) 0.8247(12) 0.4947(14) 0.083(6) Uani 0.584(8) 1 d . . P A 1
H38A H 0.744997 0.783673 0.525777 0.099 Uiso 0.584(8) 1 calc R U P A 1
H38B H 0.747550 0.892317 0.507049 0.099 Uiso 0.584(8) 1 calc R U P A 1
C39 C 0.596(2) 0.8412(15) 0.5829(14) 0.086(8) Uani 0.584(8) 1 d . . P A 1
H39A H 0.620523 0.912023 0.588321 0.104 Uiso 0.584(8) 1 calc R U P A 1
H39B H 0.645260 0.815768 0.620408 0.104 Uiso 0.584(8) 1 calc R U P A 1
C37 C 0.7006(11) 0.8010(10) 0.4160(12) 0.104(7) Uani 0.584(8) 1 d . . P A 1
H37A H 0.774613 0.812769 0.406150 0.125 Uiso 0.584(8) 1 calc R U P A 1
H37B H 0.665942 0.731632 0.405608 0.125 Uiso 0.584(8) 1 calc R U P A 1
C40 C 0.4885(11) 0.8112(9) 0.6001(6) 0.090(4) Uani 0.584(8) 1 d . . P A 1
H40A H 0.457875 0.741485 0.588465 0.107 Uiso 0.584(8) 1 calc R U P A 1
H40B H 0.490393 0.825213 0.653903 0.107 Uiso 0.584(8) 1 calc R U P A 1
C35 C 0.5845(17) 0.9180(17) 0.2513(15) 0.094(7) Uani 0.584(8) 1 d . . P A 1
H35A H 0.616916 0.984525 0.272574 0.112 Uiso 0.584(8) 1 calc R U P A 1
H35B H 0.589466 0.916015 0.197470 0.112 Uiso 0.584(8) 1 calc R U P A 1
O9 O 0.2499(7) 0.8696(6) 0.4476(5) 0.060(2) Uani 0.584(8) 1 d . . P A 1
C32 C 0.1899(13) 0.8993(15) 0.3227(9) 0.064(4) Uani 0.584(8) 1 d . . P A 1
H32A H 0.143425 0.932241 0.289555 0.077 Uiso 0.584(8) 1 calc R U P A 1
H32B H 0.160770 0.829324 0.311666 0.077 Uiso 0.584(8) 1 calc R U P A 1
C36 C 0.6437(11) 0.8479(11) 0.2941(10) 0.085(4) Uani 0.584(8) 1 d . . P A 1
H36A H 0.607971 0.781748 0.273193 0.101 Uiso 0.584(8) 1 calc R U P A 1
H36B H 0.718484 0.863591 0.285458 0.101 Uiso 0.584(8) 1 calc R U P A 1
C34 C 0.4166(14) 0.9503(13) 0.2218(8) 0.069(5) Uani 0.584(8) 1 d . . P A 1
H34A H 0.419483 0.948975 0.167596 0.083 Uiso 0.584(8) 1 calc R U P A 1
H34B H 0.447808 1.017015 0.242769 0.083 Uiso 0.584(8) 1 calc R U P A 1
C29 C 0.3172(10) 0.8387(8) 0.5691(6) 0.087(4) Uani 0.584(8) 1 d . . P A 1
H29A H 0.283358 0.769677 0.556495 0.104 Uiso 0.584(8) 1 calc R U P A 1
H29B H 0.317638 0.851819 0.622862 0.104 Uiso 0.584(8) 1 calc R U P A 1
C30 C 0.2560(19) 0.8950(15) 0.5237(8) 0.067(5) Uani 0.584(8) 1 d . . P A 1
H30A H 0.182929 0.882297 0.535461 0.081 Uiso 0.584(8) 1 calc R U P A 1
H30B H 0.291391 0.964201 0.534373 0.081 Uiso 0.584(8) 1 calc R U P A 1
C29A C 0.3328(12) 0.9105(9) 0.5532(9) 0.064(4) Uani 0.416(8) 1 d . . P A 2
H29C H 0.368961 0.979915 0.557023 0.077 Uiso 0.416(8) 1 calc R U P A 2
H29D H 0.307615 0.892889 0.600723 0.077 Uiso 0.416(8) 1 calc R U P A 2
O12A O 0.658(2) 0.853(2) 0.3848(15) 0.052(4) Uani 0.416(8) 1 d . . P A 2
C37A C 0.7390(11) 0.8372(11) 0.4431(10) 0.051(3) Uani 0.416(8) 1 d . . P A 2
H37C H 0.792952 0.898512 0.460354 0.061 Uiso 0.416(8) 1 calc R U P A 2
H37D H 0.775934 0.792374 0.424508 0.061 Uiso 0.416(8) 1 calc R U P A 2
C36A C 0.7054(15) 0.8960(11) 0.3237(9) 0.077(5) Uani 0.416(8) 1 d . . P A 2
H36C H 0.760190 0.863899 0.313357 0.093 Uiso 0.416(8) 1 calc R U P A 2
H36D H 0.740902 0.964665 0.336854 0.093 Uiso 0.416(8) 1 calc R U P A 2
C38A C 0.686(2) 0.7952(13) 0.5072(16) 0.054(5) Uani 0.416(8) 1 d . . P A 2
H38C H 0.642495 0.728430 0.493487 0.065 Uiso 0.416(8) 1 calc R U P A 2
H38D H 0.740054 0.795372 0.552719 0.065 Uiso 0.416(8) 1 calc R U P A 2
C35A C 0.622(2) 0.8859(17) 0.2583(16) 0.073(6) Uani 0.416(8) 1 d . . P A 2
H35C H 0.652444 0.917285 0.215988 0.087 Uiso 0.416(8) 1 calc R U P A 2
H35D H 0.589729 0.817071 0.243329 0.087 Uiso 0.416(8) 1 calc R U P A 2
O13A O 0.6191(11) 0.8538(7) 0.5201(8) 0.050(3) Uani 0.416(8) 1 d . . P A 2
O11A O 0.5410(18) 0.9284(11) 0.2742(7) 0.081(5) Uani 0.416(8) 1 d . . P A 2
C39A C 0.578(2) 0.8199(17) 0.5899(17) 0.049(5) Uani 0.416(8) 1 d . . P A 2
H39C H 0.637073 0.829531 0.633920 0.059 Uiso 0.416(8) 1 calc R U P A 2
H39D H 0.537753 0.751517 0.583715 0.059 Uiso 0.416(8) 1 calc R U P A 2
C34A C 0.467(2) 0.9320(18) 0.2128(17) 0.095(8) Uani 0.416(8) 1 d . . P A 2
H34C H 0.440258 0.867091 0.187610 0.114 Uiso 0.416(8) 1 calc R U P A 2
H34D H 0.503572 0.974865 0.177664 0.114 Uiso 0.416(8) 1 calc R U P A 2
C40A C 0.5044(13) 0.8846(8) 0.5969(6) 0.056(3) Uani 0.416(8) 1 d . . P A 2
H40C H 0.484927 0.880411 0.647275 0.067 Uiso 0.416(8) 1 calc R U P A 2
H40D H 0.542211 0.951959 0.591003 0.067 Uiso 0.416(8) 1 calc R U P A 2
O8A O 0.4061(14) 0.8548(16) 0.5386(12) 0.037(3) Uani 0.416(8) 1 d . . P A 2
O10A O 0.3218(12) 0.9132(9) 0.2813(10) 0.067(4) Uani 0.416(8) 1 d . . P A 2
C30A C 0.2370(18) 0.8864(16) 0.4859(16) 0.078(10) Uani 0.416(8) 1 d . . P A 2
H30C H 0.205568 0.816258 0.479629 0.093 Uiso 0.416(8) 1 calc R U P A 2
H30D H 0.180656 0.917122 0.495284 0.093 Uiso 0.416(8) 1 calc R U P A 2
C32A C 0.2297(19) 0.9374(15) 0.2937(13) 0.098(9) Uani 0.416(8) 1 d . . P A 2
H32C H 0.172258 0.915787 0.249036 0.117 Uiso 0.416(8) 1 calc R U P A 2
H32D H 0.245094 1.008070 0.299885 0.117 Uiso 0.416(8) 1 calc R U P A 2
O9A O 0.2725(7) 0.9187(7) 0.4241(7) 0.063(3) Uani 0.416(8) 1 d . . P A 2
C33 C 0.3055(10) 0.9176(9) 0.2319(7) 0.064(3) Uani 0.584(8) 1 d . . P A 1
H33A H 0.261832 0.954958 0.200947 0.077 Uiso 0.584(8) 1 calc R U P A 1
H33B H 0.276707 0.849331 0.214237 0.077 Uiso 0.584(8) 1 calc R U P A 1
C31 C 0.1898(10) 0.9224(8) 0.3991(7) 0.069(3) Uani 0.584(8) 1 d . . P A 1
H31A H 0.114977 0.906919 0.407742 0.083 Uiso 0.584(8) 1 calc R U P A 1
H31B H 0.221715 0.991947 0.410596 0.083 Uiso 0.584(8) 1 calc R U P A 1
C31A C 0.190(2) 0.894(2) 0.3614(16) 0.095(12) Uani 0.416(8) 1 d . . P A 2
H31C H 0.128507 0.918063 0.369946 0.115 Uiso 0.416(8) 1 calc R U P A 2
H31D H 0.165661 0.823630 0.353181 0.115 Uiso 0.416(8) 1 calc R U P A 2
C33A C 0.372(3) 0.966(2) 0.2269(18) 0.103(12) Uani 0.416(8) 1 d . . P A 2
H33C H 0.396760 1.035041 0.244147 0.124 Uiso 0.416(8) 1 calc R U P A 2
H33D H 0.319723 0.960356 0.179390 0.124 Uiso 0.416(8) 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 S4 2.1508(9) . ?
Ni1 S6 2.1569(11) . ?
Ni1 S5 2.1654(11) . ?
Ni1 S7 2.1574(10) . ?
Ni2 S15 2.1576(10) 2_667 ?
Ni2 S15 2.1575(10) . ?
Ni2 S14 2.1621(10) . ?
Ni2 S14 2.1621(10) 2_667 ?
Ni3 S20 2.1559(11) 2_666 ?
Ni3 S20 2.1559(11) . ?
Ni3 S19 2.1553(12) . ?
Ni3 S19 2.1553(12) 2_666 ?
S4 C3 1.710(4) . ?
S6 C5 1.715(4) . ?
S5 C2 1.713(4) . ?
S7 C4 1.716(4) . ?
S15 C9 1.716(4) . ?
S14 C8 1.712(4) . ?
S13 C9 1.740(4) . ?
S13 C7 1.732(5) . ?
S2 C3 1.726(4) . ?
S2 C1 1.742(4) . ?
S9 C4 1.742(4) . ?
S9 C6 1.729(5) . ?
S20 C12 1.718(5) . ?
S19 C11 1.720(4) . ?
S17 C11 1.729(4) . ?
S17 C10 1.735(5) . ?
S12 C7 1.741(4) . ?
S12 C8 1.748(4) . ?
S8 C5 1.741(4) . ?
S8 C6 1.737(5) . ?
S11 C7 1.635(5) . ?
S3 C2 1.744(4) . ?
S3 C1 1.744(4) . ?
S18 C12 1.745(4) . ?
S18 C10 1.725(5) . ?
S10 C6 1.640(5) . ?
S1 C1 1.619(5) . ?
S16 C10 1.632(5) . ?
O7 C26 1.414(5) . ?
O7 C27 1.419(5) . ?
O5 C14 1.425(5) . ?
O5 C15 1.410(5) . ?
O4 C13 1.405(5) . ?
O4 C24 1.427(5) . ?
O6 C16 1.432(6) . ?
O6 C17 1.389(6) . ?
O2 C21 1.410(5) . ?
O2 C20 1.437(5) . ?
O1 C18 1.440(6) . ?
O1 C19 1.424(6) . ?
O3 C22 1.432(5) . ?
O3 C23 1.402(5) . ?
N1 C25 1.486(5) . ?
O12 C37 1.38(3) . ?
O12 C36 1.31(3) . ?
N2 C28 1.485(5) . ?
O8 C40 1.38(2) . ?
O8 C29 1.461(17) . ?
O13 C38 1.40(2) . ?
O13 C39 1.38(3) . ?
C26 C25 1.492(6) . ?
C9 C8 1.365(5) . ?
C5 C4 1.363(6) . ?
C27 C28 1.491(6) . ?
C2 C3 1.365(5) . ?
C13 C14 1.494(7) . ?
C21 C22 1.486(7) . ?
C12 C11 1.359(6) . ?
C16 C15 1.472(7) . ?
C24 C23 1.480(6) . ?
C18 C17 1.487(7) . ?
O10 C32 1.42(2) . ?
O10 C33 1.422(15) . ?
C20 C19 1.467(7) . ?
O11 C35 1.39(2) . ?
O11 C34 1.453(16) . ?
C38 C37 1.45(3) . ?
C39 C40 1.46(3) . ?
C35 C36 1.56(3) . ?
O9 C30 1.409(17) . ?
O9 C31 1.429(14) . ?
C32 C31 1.42(2) . ?
C34 C33 1.46(2) . ?
C29 C30 1.45(2) . ?
C29A O8A 1.456(19) . ?
C29A C30A 1.55(3) . ?
O12A C37A 1.42(4) . ?
O12A C36A 1.44(3) . ?
C37A C38A 1.52(2) . ?
C36A C35A 1.44(3) . ?
C38A O13A 1.40(2) . ?
C35A O11A 1.42(3) . ?
O13A C39A 1.50(3) . ?
O11A C34A 1.35(3) . ?
C39A C40A 1.52(3) . ?
C34A C33A 1.51(3) . ?
C40A O8A 1.48(2) . ?
O10A C32A 1.39(2) . ?
O10A C33A 1.41(4) . ?
C30A O9A 1.33(3) . ?
C32A C31A 1.50(4) . ?
O9A C31A 1.39(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
S4 Ni1 S6 85.57(4) . . ?
S4 Ni1 S5 93.30(4) . . ?
S4 Ni1 S7 178.67(5) . . ?
S6 Ni1 S5 177.11(4) . . ?
S6 Ni1 S7 93.17(4) . . ?
S7 Ni1 S5 87.93(4) . . ?
S15 Ni2 S15 180.00(5) . 2_667 ?
S15 Ni2 S14 86.67(4) 2_667 . ?
S15 Ni2 S14 93.33(4) 2_667 2_667 ?
S15 Ni2 S14 86.67(4) . 2_667 ?
S15 Ni2 S14 93.33(4) . . ?
S14 Ni2 S14 180.0 . 2_667 ?
S20 Ni3 S20 180.00(7) 2_666 . ?
S19 Ni3 S20 86.52(4) 2_666 . ?
S19 Ni3 S20 86.52(4) . 2_666 ?
S19 Ni3 S20 93.48(4) 2_666 2_666 ?
S19 Ni3 S20 93.48(4) . . ?
S19 Ni3 S19 180.0 . 2_666 ?
C3 S4 Ni1 102.58(12) . . ?
C5 S6 Ni1 102.06(15) . . ?
C2 S5 Ni1 101.61(13) . . ?
C4 S7 Ni1 102.30(13) . . ?
C9 S15 Ni2 102.23(13) . . ?
C8 S14 Ni2 101.98(14) . . ?
C7 S13 C9 97.8(2) . . ?
C3 S2 C1 97.88(19) . . ?
C6 S9 C4 97.7(2) . . ?
C12 S20 Ni3 101.78(15) . . ?
C11 S19 Ni3 102.32(15) . . ?
C11 S17 C10 97.3(2) . . ?
C7 S12 C8 97.5(2) . . ?
C6 S8 C5 97.2(2) . . ?
C1 S3 C2 97.98(18) . . ?
C10 S18 C12 97.4(2) . . ?
C26 O7 C27 111.3(3) . . ?
C15 O5 C14 112.2(3) . . ?
C13 O4 C24 112.2(3) . . ?
C17 O6 C16 112.8(4) . . ?
C21 O2 C20 113.3(3) . . ?
C19 O1 C18 113.9(4) . . ?
C23 O3 C22 111.8(3) . . ?
C36 O12 C37 123(2) . . ?
C40 O8 C29 111.2(15) . . ?
C39 O13 C38 118.4(16) . . ?
O7 C26 C25 108.9(3) . . ?
S15 C9 S13 122.9(2) . . ?
C8 C9 S15 120.9(3) . . ?
C8 C9 S13 116.2(3) . . ?
S6 C5 S8 122.2(2) . . ?
C4 C5 S6 121.4(3) . . ?
C4 C5 S8 116.4(3) . . ?
O7 C27 C28 109.6(3) . . ?
N1 C25 C26 113.1(3) . . ?
N2 C28 C27 112.4(3) . . ?
S7 C4 S9 123.5(2) . . ?
C5 C4 S7 120.8(3) . . ?
C5 C4 S9 115.7(3) . . ?
S5 C2 S3 123.0(2) . . ?
C3 C2 S5 121.8(3) . . ?
C3 C2 S3 115.2(3) . . ?
O4 C13 C14 109.5(4) . . ?
O2 C21 C22 109.0(3) . . ?
O5 C14 C13 109.3(3) . . ?
S13 C7 S12 112.7(3) . . ?
S11 C7 S13 123.5(3) . . ?
S11 C7 S12 123.9(3) . . ?
S20 C12 S18 122.5(3) . . ?
C11 C12 S20 121.8(3) . . ?
C11 C12 S18 115.7(3) . . ?
O6 C16 C15 110.3(4) . . ?
S4 C3 S2 122.5(2) . . ?
C2 C3 S4 120.6(3) . . ?
C2 C3 S2 116.9(3) . . ?
O3 C22 C21 109.4(4) . . ?
S14 C8 S12 122.8(2) . . ?
C9 C8 S14 121.5(3) . . ?
C9 C8 S12 115.7(3) . . ?
S19 C11 S17 123.0(3) . . ?
C12 C11 S19 120.5(3) . . ?
C12 C11 S17 116.5(3) . . ?
O4 C24 C23 108.8(3) . . ?
O3 C23 C24 109.1(4) . . ?
O1 C18 C17 109.8(4) . . ?
S9 C6 S8 113.0(3) . . ?
S10 C6 S9 124.5(3) . . ?
S10 C6 S8 122.5(3) . . ?
O6 C17 C18 110.0(4) . . ?
S2 C1 S3 112.0(2) . . ?
S1 C1 S2 122.8(2) . . ?
S1 C1 S3 125.2(2) . . ?
C33 O10 C32 115.2(12) . . ?
O5 C15 C16 108.6(3) . . ?
S18 C10 S17 113.1(3) . . ?
S16 C10 S17 123.0(3) . . ?
S16 C10 S18 123.9(3) . . ?
O2 C20 C19 109.6(3) . . ?
O1 C19 C20 107.7(4) . . ?
C35 O11 C34 110.4(14) . . ?
O13 C38 C37 111.3(18) . . ?
O13 C39 C40 114.7(18) . . ?
O12 C37 C38 115.0(15) . . ?
O8 C40 C39 106.5(14) . . ?
O11 C35 C36 106.6(16) . . ?
C30 O9 C31 111.5(10) . . ?
C31 C32 O10 110.0(12) . . ?
O12 C36 C35 113.5(16) . . ?
O11 C34 C33 109.3(11) . . ?
C30 C29 O8 110.1(14) . . ?
O9 C30 C29 108.4(13) . . ?
O8A C29A C30A 106.3(13) . . ?
C37A O12A C36A 110(2) . . ?
O12A C37A C38A 107.9(18) . . ?
O12A C36A C35A 108(2) . . ?
O13A C38A C37A 106.0(16) . . ?
O11A C35A C36A 110(2) . . ?
C38A O13A C39A 105.7(15) . . ?
C34A O11A C35A 112.7(18) . . ?
O13A C39A C40A 101.5(16) . . ?
O11A C34A C33A 116(3) . . ?
O8A C40A C39A 109.7(15) . . ?
C29A O8A C40A 107.7(14) . . ?
C32A O10A C33A 114.4(17) . . ?
O9A C30A C29A 108.7(16) . . ?
O10A C32A C31A 113.2(18) . . ?
C30A O9A C31A 111(2) . . ?
O10 C33 C34 111.7(12) . . ?
C32 C31 O9 110.4(11) . . ?
O9A C31A C32A 110(2) . . ?
O10A C33A C34A 111(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 7.735
_oxdiff_exptl_absorpt_empirical_full_min 0.499
####################################################################### 
# 
# 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_18c6_nc2oc2n_lt_08_173_00_auto
_database_code_depnum_ccdc_archive 'CCDC 2384655'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2024-09-17 deposited with the CCDC.	2024-11-08 downloaded from the CCDC.
;
_audit_creation_date             2023-12-22
_audit_creation_method           
;
Olex2 1.5-ac5-023
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C6 Ni S10), C4 H14 N2 O, 2(C12 H24 O6)'
_chemical_formula_sum            'C40 H62 N2 Ni2 O13 S20'
_chemical_formula_weight         1537.53
_chemical_melting_point          ?
_chemical_oxdiff_formula         C40H62N2Ni2O13S20
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                   13.1087(4)
_cell_length_b                   14.4553(3)
_cell_length_c                   18.1391(5)
_cell_angle_alpha                90.412(2)
_cell_angle_beta                 100.304(2)
_cell_angle_gamma                104.620(2)
_cell_volume                     3267.30(15)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    15377
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      31.0270
_cell_measurement_theta_min      2.0140
_shelx_estimated_absorpt_T_max   0.919
_shelx_estimated_absorpt_T_min   0.476
_exptl_absorpt_coefficient_mu    1.270
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.398
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.67a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light black'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-18 0 4 0.2190
1 -18 -9 0.2235
18 0 -4 0.3240
0 18 9 0.2252
0 1 -25 0.0429
-1 0 25 0.0157

_exptl_crystal_size_max          0.687
_exptl_crystal_size_mid          0.511
_exptl_crystal_size_min          0.068
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-17.8510 -0.0918 3.9142 0.1479 0.6141 0.7753
0.8098 -18.2262 -9.1373 0.2072 0.8642 -0.4586
17.7996 0.2962 -3.8023 -0.1499 -0.6223 -0.7683
-0.3923 18.1368 9.0007 -0.2096 -0.8740 0.4383
0.2442 0.6569 -25.2149 0.9701 0.0765 -0.2303
-0.6124 -0.3952 25.2899 -0.9650 -0.0761 0.2511

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_unetI/netI     0.0583
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.791
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            43610
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.791
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.948
_diffrn_reflns_theta_min         2.162
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(14)
_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 0.791
_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    1.46    --   -5.80 -99.00   0.00   90
  2  ω    -77.00   4.00   0.50    1.46    --   -5.80 -37.00 -90.00  162
  3  ω    -75.00 -43.00   0.50    1.46    --   -5.80 -57.00  30.00   64
  4  ω    -38.00   3.00   0.50    1.46    --   -5.80 -57.00  30.00   82
  5  ω    -15.00  68.00   0.50    1.46    --   -5.80  37.00-150.00  166
  6  ω    -67.00   7.00   0.50    1.46    --   -5.80 -37.00  30.00  148
  7  ω    -11.00  35.00   0.50    1.46    --    6.03 -99.00-150.00   92
;
_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      -0.0167540000
_diffrn_orient_matrix_UB_12      0.0071632000
_diffrn_orient_matrix_UB_13      -0.0384497000
_diffrn_orient_matrix_UB_21      -0.0351673000
_diffrn_orient_matrix_UB_22      -0.0466745000
_diffrn_orient_matrix_UB_23      -0.0045902000
_diffrn_orient_matrix_UB_31      -0.0415041000
_diffrn_orient_matrix_UB_32      0.0186956000
_diffrn_orient_matrix_UB_33      0.0092167000
_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                10077
_reflns_number_total             16391
_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 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.958
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     862
_refine_ls_number_reflns         16391
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.1025
_refine_ls_R_factor_gt           0.0544
_refine_ls_restrained_S_all      1.029
_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)+(0.0619P)²+2.8232P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1259
_refine_ls_wR_factor_ref         0.1460
_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. Rigid body (RIGU) restrains
 C31A, O9A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C38, O13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C33A, O10A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(C29A)=Sof(H29C)=Sof(H29D)=Sof(O12A)=Sof(C37A)=Sof(H37C)=Sof(H37D)=
 Sof(C36A)=Sof(H36C)=Sof(H36D)=Sof(C38A)=Sof(H38C)=Sof(H38D)=Sof(C35A)=
 Sof(H35C)=Sof(H35D)=Sof(O13A)=Sof(O11A)=Sof(C39A)=Sof(H39C)=Sof(H39D)=
 Sof(C34A)=Sof(H34C)=Sof(H34D)=Sof(C40A)=Sof(H40C)=Sof(H40D)=Sof(O8A)=Sof(O10A)=
 Sof(C30A)=Sof(H30C)=Sof(H30D)=Sof(C32A)=Sof(H32C)=Sof(H32D)=Sof(O9A)=Sof(C31A)=
 Sof(H31C)=Sof(H31D)=Sof(C33A)=Sof(H33C)=Sof(H33D)=1-FVAR(1)
 Sof(O12)=Sof(O8)=Sof(O13)=Sof(O10)=Sof(O11)=Sof(C38)=Sof(H38A)=Sof(H38B)=
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C40)=Sof(H40A)=
 Sof(H40B)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(O9)=Sof(C32)=Sof(H32A)=Sof(H32B)=
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(C29)=Sof(H29A)=
 Sof(H29B)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C31)=
 Sof(H31A)=Sof(H31B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C27(H27A,H27B), C25(H25A,H25B), C28(H28A,H28B), C13(H13A,
 H13B), C21(H21A,H21B), C14(H14A,H14B), C16(H16A,H16B), C22(H22A,H22B),
 C24(H24A,H24B), C23(H23A,H23B), C18(H18A,H18B), C17(H17A,H17B), C15(H15A,H15B),
  C20(H20A,H20B), C19(H19A,H19B), C38(H38A,H38B), C39(H39A,H39B), C37(H37A,
 H37B), C40(H40A,H40B), C35(H35A,H35B), C32(H32A,H32B), C36(H36A,H36B),
 C34(H34A,H34B), C29(H29A,H29B), C30(H30A,H30B), C29A(H29C,H29D), C37A(H37C,
 H37D), C36A(H36C,H36D), C38A(H38C,H38D), C35A(H35C,H35D), C39A(H39C,H39D),
 C34A(H34C,H34D), C40A(H40C,H40D), C30A(H30C,H30D), C32A(H32C,H32D), C33(H33A,
 H33B), C31(H31A,H31B), C31A(H31C,H31D), C33A(H33C,H33D)
4.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(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 0.70104(3) 0.92155(3) 0.98467(3) 0.03706(12) Uani 1 1 d . . . . .
Ni2 Ni 0.500000 0.500000 1.000000 0.03982(16) Uani 1 2 d S . P . .
Ni3 Ni 0.500000 0.500000 0.500000 0.04717(18) Uani 1 2 d S . P . .
S4 S 0.53023(7) 0.90266(6) 0.95954(6) 0.0406(2) Uani 1 1 d . . . . .
S6 S 0.69668(7) 0.99990(7) 1.08522(6) 0.0448(2) Uani 1 1 d . . . . .
S5 S 0.70096(7) 0.83619(7) 0.88601(6) 0.0437(2) Uani 1 1 d . . . . .
S7 S 0.87246(7) 0.94122(7) 1.01266(6) 0.0456(2) Uani 1 1 d . . . . .
S15 S 0.59288(8) 0.64731(7) 1.00893(6) 0.0472(2) Uani 1 1 d . . . . .
S14 S 0.57700(8) 0.47009(7) 1.10948(6) 0.0467(2) Uani 1 1 d . . . . .
S13 S 0.76333(9) 0.76146(7) 1.13524(7) 0.0545(3) Uani 1 1 d . . . . .
S2 S 0.36017(7) 0.78947(7) 0.83446(6) 0.0464(2) Uani 1 1 d . . . . .
S9 S 1.03269(8) 1.02759(8) 1.15446(7) 0.0590(3) Uani 1 1 d . . . . .
S20 S 0.59370(9) 0.49323(9) 0.41482(6) 0.0582(3) Uani 1 1 d . . . . .
S19 S 0.63802(10) 0.57142(8) 0.58255(6) 0.0552(3) Uani 1 1 d . . . . .
S17 S 0.87443(10) 0.62896(8) 0.57478(7) 0.0599(3) Uani 1 1 d . . . . .
S12 S 0.74909(9) 0.59846(8) 1.22776(7) 0.0550(3) Uani 1 1 d . . . . .
S8 S 0.86882(10) 1.07835(8) 1.22142(7) 0.0594(3) Uani 1 1 d . . . . .
S11 S 0.91151(10) 0.78148(9) 1.28180(8) 0.0712(4) Uani 1 1 d . . . . .
S3 S 0.51507(8) 0.72112(8) 0.76950(7) 0.0540(3) Uani 1 1 d . . . . .
S18 S 0.83425(10) 0.55756(11) 0.42044(7) 0.0711(3) Uani 1 1 d . . . . .
S10 S 1.08946(12) 1.11726(9) 1.30987(9) 0.0849(5) Uani 1 1 d . . . . .
S1 S 0.28213(10) 0.65451(11) 0.70153(9) 0.0834(5) Uani 1 1 d . . . . .
S16 S 1.05797(13) 0.64439(14) 0.49723(10) 0.1009(6) Uani 1 1 d . . . . .
O7 O 0.2412(2) 0.67450(17) 0.30700(15) 0.0436(6) Uani 1 1 d . . . . .
O5 O 0.0774(2) 0.71720(19) 0.02878(17) 0.0542(7) Uani 1 1 d . . . . .
O4 O 0.2895(2) 0.73472(19) 0.09916(16) 0.0533(7) Uani 1 1 d . . . . .
O6 O -0.0922(2) 0.5746(2) 0.06714(18) 0.0609(8) Uani 1 1 d . . . . .
O2 O 0.1712(3) 0.42609(18) 0.21251(17) 0.0573(8) Uani 1 1 d . . . . .
O1 O -0.0339(2) 0.4160(2) 0.13983(18) 0.0620(8) Uani 1 1 d . . . . .
O3 O 0.3298(2) 0.5651(2) 0.15835(16) 0.0528(7) Uani 1 1 d . . . . .
N1 N 0.1199(2) 0.60026(19) 0.15534(17) 0.0385(7) Uani 1 1 d . . . . .
H1A H 0.098639 0.622066 0.109694 0.046 Uiso 1 1 calc R U . . .
H1B H 0.090123 0.536128 0.154991 0.046 Uiso 1 1 calc R U . . .
H1C H 0.192682 0.612019 0.165384 0.046 Uiso 1 1 calc R U . . .
O12 O 0.6490(14) 0.8565(12) 0.3690(10) 0.088(6) Uani 0.587(9) 1 d . . P A 1
N2 N 0.4285(3) 0.8142(2) 0.39583(19) 0.0463(8) Uani 1 1 d . . . . .
H2A H 0.393644 0.831973 0.352456 0.056 Uiso 1 1 calc R U . . .
H2B H 0.500456 0.839613 0.400146 0.056 Uiso 1 1 calc R U . . .
H2C H 0.405762 0.835950 0.435540 0.056 Uiso 1 1 calc R U . . .
O8 O 0.4275(14) 0.8616(14) 0.5566(9) 0.063(5) Uani 0.587(9) 1 d . . P A 1
O13 O 0.6028(8) 0.8123(7) 0.5117(6) 0.070(2) Uani 0.587(9) 1 d . . P A 1
C26 C 0.1300(3) 0.6299(3) 0.2915(2) 0.0484(9) Uani 1 1 d . . . . .
H26A H 0.094159 0.654801 0.327911 0.058 Uiso 1 1 calc R U . . .
H26B H 0.117818 0.559945 0.296156 0.058 Uiso 1 1 calc R U . . .
C9 C 0.6707(3) 0.6559(3) 1.0968(2) 0.0442(9) Uani 1 1 d . . . . .
C5 C 0.8273(3) 1.0233(3) 1.1315(2) 0.0467(9) Uani 1 1 d . . . . .
C27 C 0.2885(4) 0.6610(3) 0.3814(2) 0.0537(10) Uani 1 1 d . . . . .
H27A H 0.277119 0.591717 0.389214 0.064 Uiso 1 1 calc R U . . .
H27B H 0.254246 0.688674 0.417418 0.064 Uiso 1 1 calc R U . . .
C25 C 0.0844(3) 0.6501(3) 0.2139(2) 0.0523(10) Uani 1 1 d . . . . .
H25A H 0.005113 0.630015 0.206548 0.063 Uiso 1 1 calc R U . . .
H25B H 0.106001 0.719917 0.207932 0.063 Uiso 1 1 calc R U . . .
C28 C 0.4054(4) 0.7083(3) 0.3948(3) 0.0548(11) Uani 1 1 d . . . . .
H28A H 0.439752 0.689272 0.443407 0.066 Uiso 1 1 calc R U . . .
H28B H 0.437305 0.685597 0.354914 0.066 Uiso 1 1 calc R U . . .
C4 C 0.9040(3) 0.9984(3) 1.0998(2) 0.0477(10) Uani 1 1 d . . . . .
C2 C 0.5668(3) 0.7988(2) 0.8490(2) 0.0407(8) Uani 1 1 d . . . . .
C13 C 0.2642(4) 0.7905(3) 0.0392(3) 0.0656(13) Uani 1 1 d . . . . .
H13A H 0.263769 0.757218 -0.008836 0.079 Uiso 1 1 calc R U . . .
H13B H 0.318908 0.852655 0.044037 0.079 Uiso 1 1 calc R U . . .
C21 C 0.2716(4) 0.4118(3) 0.2062(3) 0.0647(13) Uani 1 1 d . . . . .
H21A H 0.267728 0.382925 0.155807 0.078 Uiso 1 1 calc R U . . .
H21B H 0.291710 0.367402 0.244097 0.078 Uiso 1 1 calc R U . . .
C14 C 0.1564(4) 0.8068(3) 0.0396(3) 0.0657(13) Uani 1 1 d . . . . .
H14A H 0.156496 0.838723 0.088066 0.079 Uiso 1 1 calc R U . . .
H14B H 0.139407 0.848981 -0.001011 0.079 Uiso 1 1 calc R U . . .
C7 C 0.8137(3) 0.7178(3) 1.2187(3) 0.0538(10) Uani 1 1 d . . . . .
C12 C 0.7213(4) 0.5441(3) 0.4625(2) 0.0528(10) Uani 1 1 d . . . . .
C16 C -0.1041(4) 0.6327(4) 0.0038(3) 0.0669(14) Uani 1 1 d . . . . .
H16A H -0.178423 0.639780 -0.007457 0.080 Uiso 1 1 calc R U . . .
H16B H -0.090558 0.601218 -0.040806 0.080 Uiso 1 1 calc R U . . .
C3 C 0.4924(3) 0.8290(2) 0.8800(2) 0.0384(8) Uani 1 1 d . . . . .
C22 C 0.3533(4) 0.5051(3) 0.2181(3) 0.0606(12) Uani 1 1 d . . . . .
H22A H 0.352947 0.536413 0.266779 0.073 Uiso 1 1 calc R U . . .
H22B H 0.425525 0.494924 0.219467 0.073 Uiso 1 1 calc R U . . .
C8 C 0.6641(3) 0.5788(3) 1.1400(2) 0.0447(9) Uani 1 1 d . . . . .
C11 C 0.7414(3) 0.5791(3) 0.5345(2) 0.0493(10) Uani 1 1 d . . . . .
C24 C 0.3850(3) 0.7058(3) 0.0965(3) 0.0633(12) Uani 1 1 d . . . . .
H24A H 0.445333 0.762836 0.095926 0.076 Uiso 1 1 calc R U . . .
H24B H 0.375154 0.665423 0.050178 0.076 Uiso 1 1 calc R U . . .
C23 C 0.4097(3) 0.6512(4) 0.1629(3) 0.0636(12) Uani 1 1 d . . . . .
H23A H 0.480450 0.637621 0.164781 0.076 Uiso 1 1 calc R U . . .
H23B H 0.412730 0.689174 0.209239 0.076 Uiso 1 1 calc R U . . .
C18 C -0.1419(4) 0.4263(4) 0.1207(3) 0.0779(16) Uani 1 1 d . . . . .
H18A H -0.158536 0.460298 0.162759 0.093 Uiso 1 1 calc R U . . .
H18B H -0.193246 0.362220 0.111947 0.093 Uiso 1 1 calc R U . . .
C6 C 1.0023(4) 1.0759(3) 1.2327(3) 0.0624(12) Uani 1 1 d . . . . .
C17 C -0.1533(4) 0.4810(4) 0.0519(3) 0.0725(14) Uani 1 1 d . . . . .
H17A H -0.129088 0.450827 0.011345 0.087 Uiso 1 1 calc R U . . .
H17B H -0.229575 0.480119 0.034705 0.087 Uiso 1 1 calc R U . . .
C1 C 0.3798(3) 0.7177(3) 0.7636(3) 0.0540(11) Uani 1 1 d . . . . .
O10 O 0.2965(11) 0.9284(8) 0.3090(7) 0.065(3) Uani 0.587(9) 1 d . . P A 1
C15 C -0.0277(4) 0.7280(4) 0.0203(3) 0.0695(14) Uani 1 1 d . . . . .
H15A H -0.040601 0.770138 -0.021259 0.083 Uiso 1 1 calc R U . . .
H15B H -0.037538 0.757822 0.066923 0.083 Uiso 1 1 calc R U . . .
C10 C 0.9290(4) 0.6126(3) 0.4968(3) 0.0642(12) Uani 1 1 d . . . . .
C20 C 0.0874(5) 0.3385(3) 0.2056(3) 0.0757(16) Uani 1 1 d . . . . .
H20A H 0.101638 0.299253 0.248850 0.091 Uiso 1 1 calc R U . . .
H20B H 0.085567 0.301272 0.159145 0.091 Uiso 1 1 calc R U . . .
C19 C -0.0161(5) 0.3612(3) 0.2032(3) 0.0774(16) Uani 1 1 d . . . . .
H19A H -0.074317 0.301423 0.199055 0.093 Uiso 1 1 calc R U . . .
H19B H -0.014775 0.398090 0.249711 0.093 Uiso 1 1 calc R U . . .
O11 O 0.4760(7) 0.8881(6) 0.2589(6) 0.066(2) Uani 0.587(9) 1 d . . P A 1
C38 C 0.697(2) 0.821(2) 0.4919(14) 0.118(10) Uani 0.587(9) 1 d . . P A 1
H38A H 0.733051 0.777708 0.522044 0.141 Uiso 0.587(9) 1 calc R U P A 1
H38B H 0.740626 0.887339 0.506893 0.141 Uiso 0.587(9) 1 calc R U P A 1
C39 C 0.596(2) 0.8423(16) 0.5839(14) 0.094(9) Uani 0.587(9) 1 d . . P A 1
H39A H 0.620526 0.913021 0.589461 0.113 Uiso 0.587(9) 1 calc R U P A 1
H39B H 0.645187 0.816422 0.621243 0.113 Uiso 0.587(9) 1 calc R U P A 1
C37 C 0.7008(11) 0.8029(10) 0.4149(11) 0.094(5) Uani 0.587(9) 1 d . . P A 1
H37A H 0.776636 0.817343 0.408666 0.113 Uiso 0.587(9) 1 calc R U P A 1
H37B H 0.667551 0.734267 0.400636 0.113 Uiso 0.587(9) 1 calc R U P A 1
C40 C 0.4884(11) 0.8115(9) 0.5997(6) 0.092(4) Uani 0.587(9) 1 d . . P A 1
H40A H 0.458638 0.741988 0.587444 0.111 Uiso 0.587(9) 1 calc R U P A 1
H40B H 0.489230 0.824438 0.653478 0.111 Uiso 0.587(9) 1 calc R U P A 1
C35 C 0.5837(18) 0.9219(17) 0.2517(15) 0.098(7) Uani 0.587(9) 1 d . . P A 1
H35A H 0.614891 0.987113 0.275586 0.118 Uiso 0.587(9) 1 calc R U P A 1
H35B H 0.590484 0.923238 0.198220 0.118 Uiso 0.587(9) 1 calc R U P A 1
O9 O 0.2494(8) 0.8691(6) 0.4476(5) 0.065(2) Uani 0.587(9) 1 d . . P A 1
C32 C 0.1876(12) 0.8986(15) 0.3235(10) 0.068(4) Uani 0.587(9) 1 d . . P A 1
H32A H 0.140923 0.931609 0.290562 0.081 Uiso 0.587(9) 1 calc R U P A 1
H32B H 0.158592 0.828751 0.312715 0.081 Uiso 0.587(9) 1 calc R U P A 1
C36 C 0.6414(11) 0.8471(11) 0.2939(12) 0.097(5) Uani 0.587(9) 1 d . . P A 1
H36A H 0.600226 0.781188 0.275642 0.116 Uiso 0.587(9) 1 calc R U P A 1
H36B H 0.714206 0.857452 0.282044 0.116 Uiso 0.587(9) 1 calc R U P A 1
C34 C 0.4163(17) 0.9529(15) 0.2208(11) 0.080(7) Uani 0.587(9) 1 d . . P A 1
H34A H 0.418783 0.952027 0.166585 0.096 Uiso 0.587(9) 1 calc R U P A 1
H34B H 0.447866 1.019279 0.242324 0.096 Uiso 0.587(9) 1 calc R U P A 1
C29 C 0.3168(11) 0.8382(9) 0.5685(6) 0.090(4) Uani 0.587(9) 1 d . . P A 1
H29A H 0.283177 0.769269 0.555511 0.108 Uiso 0.587(9) 1 calc R U P A 1
H29B H 0.316382 0.850425 0.622254 0.108 Uiso 0.587(9) 1 calc R U P A 1
C30 C 0.2553(17) 0.8936(14) 0.5241(8) 0.072(5) Uani 0.587(9) 1 d . . P A 1
H30A H 0.182217 0.879950 0.535880 0.086 Uiso 0.587(9) 1 calc R U P A 1
H30B H 0.289845 0.962734 0.535048 0.086 Uiso 0.587(9) 1 calc R U P A 1
C29A C 0.3341(14) 0.9107(9) 0.5548(10) 0.074(5) Uani 0.413(9) 1 d . . P A 2
H29C H 0.369667 0.980125 0.558730 0.089 Uiso 0.413(9) 1 calc R U P A 2
H29D H 0.309869 0.892148 0.602498 0.089 Uiso 0.413(9) 1 calc R U P A 2
O12A O 0.651(2) 0.847(2) 0.3814(11) 0.076(7) Uani 0.413(9) 1 d . . P A 2
C37A C 0.7386(10) 0.8375(11) 0.4454(11) 0.057(4) Uani 0.413(9) 1 d . . P A 2
H37C H 0.777906 0.793200 0.429048 0.068 Uiso 0.413(9) 1 calc R U P A 2
H37D H 0.790303 0.900655 0.459277 0.068 Uiso 0.413(9) 1 calc R U P A 2
C36A C 0.7023(17) 0.8935(13) 0.3215(10) 0.087(5) Uani 0.413(9) 1 d . . P A 2
H36C H 0.738414 0.961649 0.335945 0.104 Uiso 0.413(9) 1 calc R U P A 2
H36D H 0.755950 0.861027 0.309684 0.104 Uiso 0.413(9) 1 calc R U P A 2
C38A C 0.695(2) 0.8021(18) 0.5086(12) 0.057(5) Uani 0.413(9) 1 d . . P A 2
H38C H 0.657601 0.733130 0.499465 0.068 Uiso 0.413(9) 1 calc R U P A 2
H38D H 0.752224 0.809832 0.553364 0.068 Uiso 0.413(9) 1 calc R U P A 2
C35A C 0.617(2) 0.8849(15) 0.2590(12) 0.080(8) Uani 0.413(9) 1 d . . P A 2
H35C H 0.646448 0.915889 0.216071 0.096 Uiso 0.413(9) 1 calc R U P A 2
H35D H 0.584671 0.816239 0.244194 0.096 Uiso 0.413(9) 1 calc R U P A 2
O13A O 0.6214(11) 0.8542(7) 0.5204(8) 0.054(3) Uani 0.413(9) 1 d . . P A 2
O11A O 0.537(2) 0.9266(13) 0.2744(8) 0.098(7) Uani 0.413(9) 1 d . . P A 2
C39A C 0.579(2) 0.8210(18) 0.5889(16) 0.051(5) Uani 0.413(9) 1 d . . P A 2
H39C H 0.637206 0.829416 0.633146 0.061 Uiso 0.413(9) 1 calc R U P A 2
H39D H 0.537877 0.752879 0.582181 0.061 Uiso 0.413(9) 1 calc R U P A 2
C34A C 0.464(2) 0.9309(18) 0.2105(16) 0.101(9) Uani 0.413(9) 1 d . . P A 2
H34C H 0.438121 0.867312 0.183361 0.121 Uiso 0.413(9) 1 calc R U P A 2
H34D H 0.498911 0.977257 0.176925 0.121 Uiso 0.413(9) 1 calc R U P A 2
C40A C 0.5058(13) 0.8854(8) 0.5970(7) 0.059(4) Uani 0.413(9) 1 d . . P A 2
H40C H 0.486725 0.880478 0.647507 0.070 Uiso 0.413(9) 1 calc R U P A 2
H40D H 0.543592 0.952787 0.591500 0.070 Uiso 0.413(9) 1 calc R U P A 2
O8A O 0.4056(16) 0.8559(18) 0.5379(12) 0.041(4) Uani 0.413(9) 1 d . . P A 2
O10A O 0.3198(15) 0.9129(10) 0.2815(11) 0.078(5) Uani 0.413(9) 1 d . . P A 2
C30A C 0.2362(15) 0.8850(14) 0.4860(15) 0.074(9) Uani 0.413(9) 1 d . . P A 2
H30C H 0.205952 0.814807 0.479540 0.089 Uiso 0.413(9) 1 calc R U P A 2
H30D H 0.179002 0.914782 0.495098 0.089 Uiso 0.413(9) 1 calc R U P A 2
C32A C 0.229(2) 0.9350(16) 0.2944(14) 0.104(10) Uani 0.413(9) 1 d . . P A 2
H32C H 0.170639 0.911343 0.250371 0.125 Uiso 0.413(9) 1 calc R U P A 2
H32D H 0.242209 1.005525 0.298989 0.125 Uiso 0.413(9) 1 calc R U P A 2
O9A O 0.2724(7) 0.9183(7) 0.4250(7) 0.070(3) Uani 0.413(9) 1 d . . P A 2
C33 C 0.3023(11) 0.9180(9) 0.2324(8) 0.071(3) Uani 0.587(9) 1 d . . P A 1
H33A H 0.257305 0.954980 0.202280 0.085 Uiso 0.587(9) 1 calc R U P A 1
H33B H 0.273953 0.849766 0.214907 0.085 Uiso 0.587(9) 1 calc R U P A 1
C31 C 0.1888(10) 0.9217(8) 0.3991(7) 0.071(3) Uani 0.587(9) 1 d . . P A 1
H31A H 0.114328 0.906607 0.408277 0.085 Uiso 0.587(9) 1 calc R U P A 1
H31B H 0.220894 0.991220 0.410162 0.085 Uiso 0.587(9) 1 calc R U P A 1
C31A C 0.191(2) 0.8946(19) 0.3622(18) 0.118(15) Uani 0.413(9) 1 d . . P A 2
H31C H 0.130119 0.919269 0.370480 0.141 Uiso 0.413(9) 1 calc R U P A 2
H31D H 0.165906 0.824087 0.354567 0.141 Uiso 0.413(9) 1 calc R U P A 2
C33A C 0.371(3) 0.961(3) 0.2310(18) 0.100(8) Uani 0.413(9) 1 d . . P A 2
H33C H 0.397166 1.029171 0.249682 0.120 Uiso 0.413(9) 1 calc R U P A 2
H33D H 0.317729 0.958538 0.184353 0.120 Uiso 0.413(9) 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 S4 2.1494(9) . ?
Ni1 S6 2.1571(11) . ?
Ni1 S5 2.1660(11) . ?
Ni1 S7 2.1576(10) . ?
Ni2 S15 2.1584(10) 2_667 ?
Ni2 S15 2.1584(10) . ?
Ni2 S14 2.1599(10) . ?
Ni2 S14 2.1599(10) 2_667 ?
Ni3 S20 2.1548(11) . ?
Ni3 S20 2.1548(11) 2_666 ?
Ni3 S19 2.1557(12) . ?
Ni3 S19 2.1557(12) 2_666 ?
S4 C3 1.707(4) . ?
S6 C5 1.714(4) . ?
S5 C2 1.711(4) . ?
S7 C4 1.712(5) . ?
S15 C9 1.717(4) . ?
S14 C8 1.713(4) . ?
S13 C9 1.742(4) . ?
S13 C7 1.730(5) . ?
S2 C3 1.731(4) . ?
S2 C1 1.740(4) . ?
S9 C4 1.745(4) . ?
S9 C6 1.729(5) . ?
S20 C12 1.715(5) . ?
S19 C11 1.720(4) . ?
S17 C11 1.731(4) . ?
S17 C10 1.735(5) . ?
S12 C7 1.742(4) . ?
S12 C8 1.748(4) . ?
S8 C5 1.741(4) . ?
S8 C6 1.735(5) . ?
S11 C7 1.633(5) . ?
S3 C2 1.744(4) . ?
S3 C1 1.745(4) . ?
S18 C12 1.753(4) . ?
S18 C10 1.722(5) . ?
S10 C6 1.641(5) . ?
S1 C1 1.619(5) . ?
S16 C10 1.635(5) . ?
O7 C26 1.413(5) . ?
O7 C27 1.417(5) . ?
O5 C14 1.427(5) . ?
O5 C15 1.407(5) . ?
O4 C13 1.401(5) . ?
O4 C24 1.425(5) . ?
O6 C16 1.437(6) . ?
O6 C17 1.384(6) . ?
O2 C21 1.406(5) . ?
O2 C20 1.439(5) . ?
O1 C18 1.441(6) . ?
O1 C19 1.420(6) . ?
O3 C22 1.433(5) . ?
O3 C23 1.401(5) . ?
N1 C25 1.482(5) . ?
O12 C37 1.35(2) . ?
O12 C36 1.35(2) . ?
N2 C28 1.483(5) . ?
O8 C40 1.36(2) . ?
O8 C29 1.461(18) . ?
O13 C38 1.32(3) . ?
O13 C39 1.40(3) . ?
C26 C25 1.488(6) . ?
C9 C8 1.361(5) . ?
C5 C4 1.363(6) . ?
C27 C28 1.486(6) . ?
C2 C3 1.367(5) . ?
C13 C14 1.491(7) . ?
C21 C22 1.482(7) . ?
C12 C11 1.352(6) . ?
C16 C15 1.478(7) . ?
C24 C23 1.477(7) . ?
C18 C17 1.488(8) . ?
O10 C32 1.456(18) . ?
O10 C33 1.414(16) . ?
C20 C19 1.467(7) . ?
O11 C35 1.40(2) . ?
O11 C34 1.47(2) . ?
C38 C37 1.43(3) . ?
C39 C40 1.45(3) . ?
C35 C36 1.60(3) . ?
O9 C30 1.412(16) . ?
O9 C31 1.431(14) . ?
C32 C31 1.40(2) . ?
C34 C33 1.50(2) . ?
C29 C30 1.43(2) . ?
C29A O8A 1.44(2) . ?
C29A C30A 1.59(3) . ?
O12A C37A 1.51(3) . ?
O12A C36A 1.46(2) . ?
C37A C38A 1.42(4) . ?
C36A C35A 1.42(3) . ?
C38A O13A 1.40(3) . ?
C35A O11A 1.40(3) . ?
O13A C39A 1.49(3) . ?
O11A C34A 1.38(3) . ?
C39A C40A 1.51(2) . ?
C34A C33A 1.50(4) . ?
C40A O8A 1.50(2) . ?
O10A C32A 1.37(3) . ?
O10A C33A 1.33(3) . ?
C30A O9A 1.33(3) . ?
C32A C31A 1.47(4) . ?
O9A C31A 1.39(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
S4 Ni1 S6 85.59(4) . . ?
S4 Ni1 S5 93.28(4) . . ?
S4 Ni1 S7 178.64(5) . . ?
S6 Ni1 S5 177.03(4) . . ?
S6 Ni1 S7 93.13(4) . . ?
S7 Ni1 S5 87.97(4) . . ?
S15 Ni2 S15 180.00(3) 2_667 . ?
S15 Ni2 S14 93.34(4) . . ?
S15 Ni2 S14 86.66(4) . 2_667 ?
S15 Ni2 S14 93.34(4) 2_667 2_667 ?
S15 Ni2 S14 86.66(4) 2_667 . ?
S14 Ni2 S14 180.00(5) . 2_667 ?
S20 Ni3 S20 180.0 2_666 . ?
S20 Ni3 S19 86.49(4) . 2_666 ?
S20 Ni3 S19 93.51(4) . . ?
S20 Ni3 S19 86.49(4) 2_666 . ?
S20 Ni3 S19 93.51(4) 2_666 2_666 ?
S19 Ni3 S19 180.0 . 2_666 ?
C3 S4 Ni1 102.55(12) . . ?
C5 S6 Ni1 102.06(15) . . ?
C2 S5 Ni1 101.65(13) . . ?
C4 S7 Ni1 102.32(13) . . ?
C9 S15 Ni2 102.11(13) . . ?
C8 S14 Ni2 102.00(14) . . ?
C7 S13 C9 97.8(2) . . ?
C3 S2 C1 98.03(19) . . ?
C6 S9 C4 97.8(2) . . ?
C12 S20 Ni3 101.55(15) . . ?
C11 S19 Ni3 102.18(15) . . ?
C11 S17 C10 97.1(2) . . ?
C7 S12 C8 97.5(2) . . ?
C6 S8 C5 97.3(2) . . ?
C2 S3 C1 98.12(19) . . ?
C10 S18 C12 97.3(2) . . ?
C26 O7 C27 111.7(3) . . ?
C15 O5 C14 112.5(3) . . ?
C13 O4 C24 112.2(3) . . ?
C17 O6 C16 112.4(4) . . ?
C21 O2 C20 113.3(3) . . ?
C19 O1 C18 114.2(4) . . ?
C23 O3 C22 112.0(3) . . ?
C36 O12 C37 120.3(12) . . ?
C40 O8 C29 112.7(16) . . ?
C38 O13 C39 120.8(17) . . ?
O7 C26 C25 109.1(3) . . ?
S15 C9 S13 122.7(2) . . ?
C8 C9 S15 121.0(3) . . ?
C8 C9 S13 116.2(3) . . ?
S6 C5 S8 122.2(2) . . ?
C4 C5 S6 121.3(3) . . ?
C4 C5 S8 116.5(3) . . ?
O7 C27 C28 109.7(3) . . ?
N1 C25 C26 113.0(3) . . ?
N2 C28 C27 112.7(3) . . ?
S7 C4 S9 123.7(2) . . ?
C5 C4 S7 120.9(3) . . ?
C5 C4 S9 115.4(3) . . ?
S5 C2 S3 123.2(2) . . ?
C3 C2 S5 121.6(3) . . ?
C3 C2 S3 115.3(3) . . ?
O4 C13 C14 109.1(4) . . ?
O2 C21 C22 109.2(3) . . ?
O5 C14 C13 109.5(3) . . ?
S13 C7 S12 112.7(2) . . ?
S11 C7 S13 123.6(3) . . ?
S11 C7 S12 123.8(3) . . ?
S20 C12 S18 122.2(3) . . ?
C11 C12 S20 122.3(3) . . ?
C11 C12 S18 115.4(3) . . ?
O6 C16 C15 109.9(4) . . ?
S4 C3 S2 122.6(2) . . ?
C2 C3 S4 120.8(3) . . ?
C2 C3 S2 116.6(3) . . ?
O3 C22 C21 109.4(4) . . ?
S14 C8 S12 122.8(2) . . ?
C9 C8 S14 121.5(3) . . ?
C9 C8 S12 115.7(3) . . ?
S19 C11 S17 122.7(3) . . ?
C12 C11 S19 120.4(3) . . ?
C12 C11 S17 116.8(3) . . ?
O4 C24 C23 109.4(4) . . ?
O3 C23 C24 109.1(4) . . ?
O1 C18 C17 109.8(4) . . ?
S9 C6 S8 113.0(3) . . ?
S10 C6 S9 124.5(3) . . ?
S10 C6 S8 122.5(3) . . ?
O6 C17 C18 109.7(4) . . ?
S2 C1 S3 111.9(2) . . ?
S1 C1 S2 122.9(2) . . ?
S1 C1 S3 125.2(2) . . ?
C33 O10 C32 113.5(12) . . ?
O5 C15 C16 108.8(3) . . ?
S18 C10 S17 113.3(3) . . ?
S16 C10 S17 122.9(3) . . ?
S16 C10 S18 123.8(3) . . ?
O2 C20 C19 109.4(4) . . ?
O1 C19 C20 107.9(4) . . ?
C35 O11 C34 108.0(14) . . ?
O13 C38 C37 119(2) . . ?
O13 C39 C40 112.8(18) . . ?
O12 C37 C38 111.7(14) . . ?
O8 C40 C39 107.4(15) . . ?
O11 C35 C36 104.3(16) . . ?
C30 O9 C31 111.9(10) . . ?
C31 C32 O10 109.2(12) . . ?
O12 C36 C35 111.3(14) . . ?
O11 C34 C33 107.0(12) . . ?
C30 C29 O8 111.6(14) . . ?
O9 C30 C29 108.4(12) . . ?
O8A C29A C30A 104.3(13) . . ?
C36A O12A C37A 108(2) . . ?
C38A C37A O12A 110.7(16) . . ?
C35A C36A O12A 105(2) . . ?
O13A C38A C37A 108.0(19) . . ?
O11A C35A C36A 112.6(19) . . ?
C38A O13A C39A 108.5(16) . . ?
C34A O11A C35A 111.9(18) . . ?
O13A C39A C40A 103.0(17) . . ?
O11A C34A C33A 110(3) . . ?
O8A C40A C39A 109.6(16) . . ?
C29A O8A C40A 106.8(16) . . ?
C33A O10A C32A 118(2) . . ?
O9A C30A C29A 107.9(13) . . ?
O10A C32A C31A 114(2) . . ?
C30A O9A C31A 111(2) . . ?
O10 C33 C34 110.8(13) . . ?
C32 C31 O9 110.7(11) . . ?
O9A C31A C32A 111(2) . . ?
O10A C33A C34A 119(3) . . ?

_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 13.155
_oxdiff_exptl_absorpt_empirical_full_min 0.486
####################################################################### 
# 
# 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_18c6_nc2oc2n_lt_06_153_00_auto
_database_code_depnum_ccdc_archive 'CCDC 2384653'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2024-09-17 deposited with the CCDC.	2024-11-08 downloaded from the CCDC.
;
_audit_creation_date             2023-12-22
_audit_creation_method           
;
Olex2 1.5-ac5-023
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C6 Ni S10), C4 H14 N2 O, 2(C12 H24 O6)'
_chemical_formula_sum            'C40 H62 N2 Ni2 O13 S20'
_chemical_formula_weight         1537.53
_chemical_melting_point          ?
_chemical_oxdiff_formula         C40H62N2Ni2O13S20
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                   13.0985(4)
_cell_length_b                   14.4353(3)
_cell_length_c                   18.1439(5)
_cell_angle_alpha                90.560(2)
_cell_angle_beta                 100.266(2)
_cell_angle_gamma                104.728(2)
_cell_volume                     3259.35(15)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    16090
_cell_measurement_temperature    152.95(10)
_cell_measurement_theta_max      30.8950
_cell_measurement_theta_min      2.0190
_shelx_estimated_absorpt_T_max   0.903
_shelx_estimated_absorpt_T_min   0.479
_exptl_absorpt_coefficient_mu    1.273
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31225
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.67a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark black'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.678
_exptl_crystal_size_mid          0.545
_exptl_crystal_size_min          0.082
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_unetI/netI     0.0563
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.791
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            43335
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.791
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.921
_diffrn_reflns_theta_min         2.164
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      152.95(10)
_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 0.791
_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    1.46    --   -5.80 -99.00   0.00   90
  2  ω    -77.00   4.00   0.50    1.46    --   -5.80 -37.00 -90.00  162
  3  ω    -75.00 -43.00   0.50    1.46    --   -5.80 -57.00  30.00   64
  4  ω    -38.00   3.00   0.50    1.46    --   -5.80 -57.00  30.00   82
  5  ω    -15.00  68.00   0.50    1.46    --   -5.80  37.00-150.00  166
  6  ω    -67.00   7.00   0.50    1.46    --   -5.80 -37.00  30.00  148
  7  ω    -11.00  35.00   0.50    1.46    --    6.03 -99.00-150.00   92
;
_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      -0.0163039000
_diffrn_orient_matrix_UB_12      0.0074559000
_diffrn_orient_matrix_UB_13      -0.0384155000
_diffrn_orient_matrix_UB_21      -0.0353110000
_diffrn_orient_matrix_UB_22      -0.0467737000
_diffrn_orient_matrix_UB_23      -0.0050059000
_diffrn_orient_matrix_UB_31      -0.0416615000
_diffrn_orient_matrix_UB_32      0.0186148000
_diffrn_orient_matrix_UB_33      0.0091043000
_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                10396
_reflns_number_total             16329
_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 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.948
_refine_diff_density_min         -0.943
_refine_diff_density_rms         0.089
_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     862
_refine_ls_number_reflns         16329
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0978
_refine_ls_R_factor_gt           0.0532
_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)+(0.0612P)²+3.2129P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1232
_refine_ls_wR_factor_ref         0.1428
_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. Rigid body (RIGU) restrains
 C31A, O9A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(C29A)=Sof(H29C)=Sof(H29D)=Sof(O12A)=Sof(C37A)=Sof(H37C)=Sof(H37D)=
 Sof(C36A)=Sof(H36C)=Sof(H36D)=Sof(C38A)=Sof(H38C)=Sof(H38D)=Sof(C35A)=
 Sof(H35C)=Sof(H35D)=Sof(O13A)=Sof(O11A)=Sof(C39A)=Sof(H39C)=Sof(H39D)=
 Sof(C34A)=Sof(H34C)=Sof(H34D)=Sof(C40A)=Sof(H40C)=Sof(H40D)=Sof(O8A)=Sof(O10A)=
 Sof(C30A)=Sof(H30C)=Sof(H30D)=Sof(C32A)=Sof(H32C)=Sof(H32D)=Sof(O9A)=Sof(C31A)=
 Sof(H31C)=Sof(H31D)=Sof(C33A)=Sof(H33C)=Sof(H33D)=1-FVAR(1)
 Sof(O12)=Sof(O8)=Sof(O13)=Sof(O10)=Sof(O11)=Sof(C38)=Sof(H38A)=Sof(H38B)=
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C40)=Sof(H40A)=
 Sof(H40B)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(O9)=Sof(C32)=Sof(H32A)=Sof(H32B)=
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(C29)=Sof(H29A)=
 Sof(H29B)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C31)=
 Sof(H31A)=Sof(H31B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C27(H27A,H27B), C25(H25A,H25B), C28(H28A,H28B), C13(H13A,
 H13B), C21(H21A,H21B), C14(H14A,H14B), C16(H16A,H16B), C22(H22A,H22B),
 C24(H24A,H24B), C23(H23A,H23B), C18(H18A,H18B), C17(H17A,H17B), C15(H15A,H15B),
  C20(H20A,H20B), C19(H19A,H19B), C38(H38A,H38B), C39(H39A,H39B), C37(H37A,
 H37B), C40(H40A,H40B), C35(H35A,H35B), C32(H32A,H32B), C36(H36A,H36B),
 C34(H34A,H34B), C29(H29A,H29B), C30(H30A,H30B), C29A(H29C,H29D), C37A(H37C,
 H37D), C36A(H36C,H36D), C38A(H38C,H38D), C35A(H35C,H35D), C39A(H39C,H39D),
 C34A(H34C,H34D), C40A(H40C,H40D), C30A(H30C,H30D), C32A(H32C,H32D), C33(H33A,
 H33B), C31(H31A,H31B), C31A(H31C,H31D), C33A(H33C,H33D)
4.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(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 0.70116(3) 0.92146(3) 0.98447(3) 0.03280(12) Uani 1 1 d . . . . .
Ni2 Ni 0.500000 0.500000 1.000000 0.03541(16) Uani 1 2 d S . P . .
Ni3 Ni 0.500000 0.500000 0.500000 0.04206(17) Uani 1 2 d S . P . .
S4 S 0.53010(7) 0.90272(6) 0.95926(5) 0.0360(2) Uani 1 1 d . . . . .
S6 S 0.69710(7) 1.00048(7) 1.08501(6) 0.0397(2) Uani 1 1 d . . . . .
S5 S 0.70091(7) 0.83574(6) 0.88569(6) 0.0389(2) Uani 1 1 d . . . . .
S7 S 0.87266(7) 0.94095(7) 1.01239(6) 0.0402(2) Uani 1 1 d . . . . .
S15 S 0.59394(8) 0.64738(7) 1.00898(6) 0.0420(2) Uani 1 1 d . . . . .
S14 S 0.57679(8) 0.47012(7) 1.10955(6) 0.0416(2) Uani 1 1 d . . . . .
S13 S 0.76504(8) 0.76185(7) 1.13546(7) 0.0485(3) Uani 1 1 d . . . . .
S2 S 0.35971(7) 0.78934(7) 0.83391(6) 0.0417(2) Uani 1 1 d . . . . .
S9 S 1.03324(8) 1.02736(8) 1.15446(7) 0.0518(3) Uani 1 1 d . . . . .
S20 S 0.59375(9) 0.49394(8) 0.41459(6) 0.0515(3) Uani 1 1 d . . . . .
S19 S 0.63842(9) 0.57060(8) 0.58294(6) 0.0490(3) Uani 1 1 d . . . . .
S17 S 0.87532(9) 0.62808(8) 0.57533(6) 0.0535(3) Uani 1 1 d . . . . .
S12 S 0.74952(9) 0.59876(8) 1.22798(6) 0.0491(2) Uani 1 1 d . . . . .
S8 S 0.86946(9) 1.07885(8) 1.22140(7) 0.0530(3) Uani 1 1 d . . . . .
S11 S 0.91328(9) 0.78197(9) 1.28210(8) 0.0638(3) Uani 1 1 d . . . . .
S3 S 0.51469(8) 0.72031(7) 0.76894(7) 0.0492(3) Uani 1 1 d . . . . .
S18 S 0.83486(10) 0.55817(10) 0.42047(7) 0.0630(3) Uani 1 1 d . . . . .
S10 S 1.09039(12) 1.11736(9) 1.31020(8) 0.0749(4) Uani 1 1 d . . . . .
S1 S 0.28150(10) 0.65409(11) 0.70061(9) 0.0785(4) Uani 1 1 d . . . . .
S16 S 1.05924(12) 0.64410(13) 0.49761(9) 0.0899(5) Uani 1 1 d . . . . .
O7 O 0.2419(2) 0.67496(17) 0.30665(14) 0.0386(6) Uani 1 1 d . . . . .
O5 O 0.0789(2) 0.71765(19) 0.02881(16) 0.0474(7) Uani 1 1 d . . . . .
O4 O 0.2909(2) 0.73438(18) 0.09933(16) 0.0461(6) Uani 1 1 d . . . . .
O6 O -0.0919(2) 0.5755(2) 0.06676(17) 0.0525(7) Uani 1 1 d . . . . .
O2 O 0.1699(2) 0.42578(17) 0.21247(16) 0.0493(7) Uani 1 1 d . . . . .
O1 O -0.0351(2) 0.41651(19) 0.13908(17) 0.0534(7) Uani 1 1 d . . . . .
O3 O 0.3297(2) 0.56435(19) 0.15845(16) 0.0462(6) Uani 1 1 d . . . . .
N1 N 0.1202(2) 0.60037(19) 0.15486(17) 0.0343(6) Uani 1 1 d . . . . .
H1A H 0.101205 0.623675 0.109481 0.041 Uiso 1 1 calc R U . . .
H1B H 0.088206 0.536384 0.153320 0.041 Uiso 1 1 calc R U . . .
H1C H 0.192852 0.610237 0.165812 0.041 Uiso 1 1 calc R U . . .
O12 O 0.6470(18) 0.8507(16) 0.3671(11) 0.076(6) Uani 0.586(8) 1 d . . P A 1
N2 N 0.4303(3) 0.8149(2) 0.39545(18) 0.0419(7) Uani 1 1 d . . . . .
H2A H 0.392253 0.832606 0.353466 0.050 Uiso 1 1 calc R U . . .
H2B H 0.501831 0.839954 0.396799 0.050 Uiso 1 1 calc R U . . .
H2C H 0.411580 0.837151 0.436810 0.050 Uiso 1 1 calc R U . . .
O8 O 0.4265(15) 0.8624(14) 0.5546(11) 0.061(5) Uani 0.586(8) 1 d . . P A 1
O13 O 0.6028(8) 0.8113(7) 0.5122(6) 0.066(2) Uani 0.586(8) 1 d . . P A 1
C26 C 0.1303(3) 0.6306(3) 0.2914(2) 0.0435(9) Uani 1 1 d . . . . .
H26A H 0.094730 0.656168 0.327749 0.052 Uiso 1 1 calc R U . . .
H26B H 0.117510 0.560516 0.296263 0.052 Uiso 1 1 calc R U . . .
C9 C 0.6717(3) 0.6561(3) 1.0970(2) 0.0402(8) Uani 1 1 d . . . . .
C5 C 0.8277(3) 1.0235(3) 1.1313(2) 0.0414(9) Uani 1 1 d . . . . .
C27 C 0.2891(3) 0.6617(3) 0.3812(2) 0.0473(10) Uani 1 1 d . . . . .
H27A H 0.277281 0.592248 0.389066 0.057 Uiso 1 1 calc R U . . .
H27B H 0.255194 0.689823 0.417172 0.057 Uiso 1 1 calc R U . . .
C25 C 0.0850(3) 0.6506(3) 0.2135(2) 0.0476(10) Uani 1 1 d . . . . .
H25A H 0.005583 0.630729 0.205990 0.057 Uiso 1 1 calc R U . . .
H25B H 0.107035 0.720537 0.207520 0.057 Uiso 1 1 calc R U . . .
C28 C 0.4064(3) 0.7087(3) 0.3943(2) 0.0474(10) Uani 1 1 d . . . . .
H28A H 0.440921 0.689688 0.442779 0.057 Uiso 1 1 calc R U . . .
H28B H 0.437935 0.685739 0.354245 0.057 Uiso 1 1 calc R U . . .
C4 C 0.9045(3) 0.9986(3) 1.1000(2) 0.0434(9) Uani 1 1 d . . . . .
C2 C 0.5666(3) 0.7981(2) 0.8486(2) 0.0366(8) Uani 1 1 d . . . . .
C13 C 0.2663(4) 0.7909(3) 0.0395(3) 0.0557(11) Uani 1 1 d . . . . .
H13A H 0.265828 0.757896 -0.008658 0.067 Uiso 1 1 calc R U . . .
H13B H 0.321312 0.853158 0.044843 0.067 Uiso 1 1 calc R U . . .
C21 C 0.2709(4) 0.4110(3) 0.2067(2) 0.0549(11) Uani 1 1 d . . . . .
H21A H 0.267160 0.381105 0.156601 0.066 Uiso 1 1 calc R U . . .
H21B H 0.290954 0.367339 0.245114 0.066 Uiso 1 1 calc R U . . .
C14 C 0.1580(4) 0.8074(3) 0.0400(3) 0.0565(11) Uani 1 1 d . . . . .
H14A H 0.158093 0.839206 0.088664 0.068 Uiso 1 1 calc R U . . .
H14B H 0.141198 0.849882 -0.000322 0.068 Uiso 1 1 calc R U . . .
C7 C 0.8149(3) 0.7180(3) 1.2190(3) 0.0485(10) Uani 1 1 d . . . . .
C12 C 0.7220(3) 0.5444(3) 0.4625(2) 0.0458(9) Uani 1 1 d . . . . .
C16 C -0.1035(3) 0.6331(4) 0.0035(2) 0.0579(12) Uani 1 1 d . . . . .
H16A H -0.177794 0.640193 -0.007996 0.070 Uiso 1 1 calc R U . . .
H16B H -0.089592 0.601493 -0.040981 0.070 Uiso 1 1 calc R U . . .
C3 C 0.4923(3) 0.8289(2) 0.8796(2) 0.0352(8) Uani 1 1 d . . . . .
C22 C 0.3529(3) 0.5048(3) 0.2179(2) 0.0514(10) Uani 1 1 d . . . . .
H22A H 0.352976 0.536630 0.266489 0.062 Uiso 1 1 calc R U . . .
H22B H 0.425080 0.494519 0.219098 0.062 Uiso 1 1 calc R U . . .
C8 C 0.6646(3) 0.5791(3) 1.1400(2) 0.0411(9) Uani 1 1 d . . . . .
C11 C 0.7418(3) 0.5786(3) 0.5350(2) 0.0438(9) Uani 1 1 d . . . . .
C24 C 0.3862(3) 0.7051(3) 0.0962(3) 0.0553(11) Uani 1 1 d . . . . .
H24A H 0.446827 0.762075 0.095267 0.066 Uiso 1 1 calc R U . . .
H24B H 0.375748 0.664224 0.049872 0.066 Uiso 1 1 calc R U . . .
C23 C 0.4109(3) 0.6507(3) 0.1629(3) 0.0547(11) Uani 1 1 d . . . . .
H23A H 0.481388 0.636702 0.164660 0.066 Uiso 1 1 calc R U . . .
H23B H 0.414371 0.689277 0.209104 0.066 Uiso 1 1 calc R U . . .
C18 C -0.1427(3) 0.4265(3) 0.1204(3) 0.0653(14) Uani 1 1 d . . . . .
H18A H -0.158962 0.460963 0.162517 0.078 Uiso 1 1 calc R U . . .
H18B H -0.194192 0.362309 0.111959 0.078 Uiso 1 1 calc R U . . .
C6 C 1.0030(4) 1.0759(3) 1.2330(3) 0.0548(11) Uani 1 1 d . . . . .
C17 C -0.1547(3) 0.4809(4) 0.0513(3) 0.0628(13) Uani 1 1 d . . . . .
H17A H -0.131383 0.450227 0.010561 0.075 Uiso 1 1 calc R U . . .
H17B H -0.231032 0.480453 0.034656 0.075 Uiso 1 1 calc R U . . .
C1 C 0.3795(3) 0.7174(3) 0.7632(3) 0.0502(10) Uani 1 1 d . . . . .
O10 O 0.3000(8) 0.9293(6) 0.3077(5) 0.057(2) Uani 0.586(8) 1 d . . P A 1
C15 C -0.0266(4) 0.7288(3) 0.0204(3) 0.0591(12) Uani 1 1 d . . . . .
H15A H -0.039346 0.771111 -0.020957 0.071 Uiso 1 1 calc R U . . .
H15B H -0.036435 0.758479 0.067140 0.071 Uiso 1 1 calc R U . . .
C10 C 0.9298(4) 0.6125(3) 0.4971(3) 0.0580(11) Uani 1 1 d . . . . .
C20 C 0.0853(4) 0.3381(3) 0.2053(3) 0.0657(14) Uani 1 1 d . . . . .
H20A H 0.098941 0.298779 0.248578 0.079 Uiso 1 1 calc R U . . .
H20B H 0.083366 0.300553 0.158907 0.079 Uiso 1 1 calc R U . . .
C19 C -0.0182(4) 0.3615(3) 0.2027(3) 0.0686(14) Uani 1 1 d . . . . .
H19A H -0.077046 0.301911 0.198370 0.082 Uiso 1 1 calc R U . . .
H19B H -0.016816 0.398797 0.249109 0.082 Uiso 1 1 calc R U . . .
O11 O 0.4806(7) 0.8890(5) 0.2603(5) 0.0595(19) Uani 0.586(8) 1 d . . P A 1
C38 C 0.698(2) 0.8233(15) 0.4952(14) 0.104(8) Uani 0.586(8) 1 d . . P A 1
H38A H 0.736246 0.782517 0.526933 0.124 Uiso 0.586(8) 1 calc R U P A 1
H38B H 0.738891 0.890842 0.508558 0.124 Uiso 0.586(8) 1 calc R U P A 1
C39 C 0.595(2) 0.8392(16) 0.5840(14) 0.085(9) Uani 0.586(8) 1 d . . P A 1
H39A H 0.621151 0.909933 0.591051 0.103 Uiso 0.586(8) 1 calc R U P A 1
H39B H 0.642220 0.811442 0.620954 0.103 Uiso 0.586(8) 1 calc R U P A 1
C37 C 0.7013(10) 0.8013(9) 0.4166(10) 0.091(5) Uani 0.586(8) 1 d . . P A 1
H37A H 0.777194 0.816668 0.410224 0.109 Uiso 0.586(8) 1 calc R U P A 1
H37B H 0.670022 0.731694 0.404698 0.109 Uiso 0.586(8) 1 calc R U P A 1
C40 C 0.4881(10) 0.8110(9) 0.5997(6) 0.085(4) Uani 0.586(8) 1 d . . P A 1
H40A H 0.457194 0.741170 0.588384 0.103 Uiso 0.586(8) 1 calc R U P A 1
H40B H 0.489333 0.825452 0.653362 0.103 Uiso 0.586(8) 1 calc R U P A 1
C35 C 0.5886(15) 0.9172(14) 0.2524(13) 0.086(6) Uani 0.586(8) 1 d . . P A 1
H35A H 0.622081 0.983768 0.273455 0.104 Uiso 0.586(8) 1 calc R U P A 1
H35B H 0.593995 0.914443 0.198735 0.104 Uiso 0.586(8) 1 calc R U P A 1
O9 O 0.2496(7) 0.8705(6) 0.4468(5) 0.059(2) Uani 0.586(8) 1 d . . P A 1
C32 C 0.1921(15) 0.9008(15) 0.3222(9) 0.060(4) Uani 0.586(8) 1 d . . P A 1
H32A H 0.146217 0.934427 0.289229 0.072 Uiso 0.586(8) 1 calc R U P A 1
H32B H 0.162200 0.830907 0.310634 0.072 Uiso 0.586(8) 1 calc R U P A 1
C36 C 0.6454(10) 0.8479(10) 0.2950(9) 0.081(4) Uani 0.586(8) 1 d . . P A 1
H36A H 0.609131 0.781782 0.273952 0.097 Uiso 0.586(8) 1 calc R U P A 1
H36B H 0.720323 0.862888 0.286546 0.097 Uiso 0.586(8) 1 calc R U P A 1
C34 C 0.4199(13) 0.9487(9) 0.2214(7) 0.070(5) Uani 0.586(8) 1 d . . P A 1
H34A H 0.422754 0.944976 0.167294 0.084 Uiso 0.586(8) 1 calc R U P A 1
H34B H 0.451923 1.016207 0.240673 0.084 Uiso 0.586(8) 1 calc R U P A 1
C29 C 0.3173(10) 0.8390(8) 0.5684(6) 0.082(3) Uani 0.586(8) 1 d . . P A 1
H29A H 0.318306 0.852039 0.622240 0.099 Uiso 0.586(8) 1 calc R U P A 1
H29B H 0.282947 0.769946 0.555649 0.099 Uiso 0.586(8) 1 calc R U P A 1
C30 C 0.2559(16) 0.8963(12) 0.5231(8) 0.064(4) Uani 0.586(8) 1 d . . P A 1
H30A H 0.182882 0.883828 0.534952 0.077 Uiso 0.586(8) 1 calc R U P A 1
H30B H 0.291804 0.965433 0.533820 0.077 Uiso 0.586(8) 1 calc R U P A 1
C29A C 0.3323(12) 0.9111(8) 0.5525(8) 0.057(4) Uani 0.414(8) 1 d . . P A 2
H29C H 0.368466 0.980501 0.555156 0.069 Uiso 0.414(8) 1 calc R U P A 2
H29D H 0.307218 0.894993 0.600281 0.069 Uiso 0.414(8) 1 calc R U P A 2
O12A O 0.658(3) 0.8534(19) 0.3856(13) 0.048(4) Uani 0.414(8) 1 d . . P A 2
C37A C 0.7400(10) 0.8377(10) 0.4442(9) 0.046(3) Uani 0.414(8) 1 d . . P A 2
H37C H 0.794261 0.899266 0.460296 0.055 Uiso 0.414(8) 1 calc R U P A 2
H37D H 0.776516 0.792990 0.424953 0.055 Uiso 0.414(8) 1 calc R U P A 2
C36A C 0.7072(13) 0.8967(10) 0.3238(8) 0.065(4) Uani 0.414(8) 1 d . . P A 2
H36C H 0.741966 0.965714 0.336485 0.078 Uiso 0.414(8) 1 calc R U P A 2
H36D H 0.762528 0.864981 0.313964 0.078 Uiso 0.414(8) 1 calc R U P A 2
C38A C 0.6953(17) 0.7982(16) 0.5082(13) 0.047(4) Uani 0.414(8) 1 d . . P A 2
H38C H 0.752925 0.804336 0.552840 0.056 Uiso 0.414(8) 1 calc R U P A 2
H38D H 0.657435 0.729443 0.497415 0.056 Uiso 0.414(8) 1 calc R U P A 2
C35A C 0.6227(19) 0.8848(16) 0.2581(14) 0.065(5) Uani 0.414(8) 1 d . . P A 2
H35C H 0.653022 0.914665 0.215145 0.078 Uiso 0.414(8) 1 calc R U P A 2
H35D H 0.590043 0.815710 0.244440 0.078 Uiso 0.414(8) 1 calc R U P A 2
O13A O 0.6202(10) 0.8534(6) 0.5213(7) 0.044(2) Uani 0.414(8) 1 d . . P A 2
O11A O 0.5438(14) 0.9287(9) 0.2741(6) 0.067(3) Uani 0.414(8) 1 d . . P A 2
C39A C 0.577(2) 0.8210(19) 0.5897(16) 0.046(5) Uani 0.414(8) 1 d . . P A 2
H39C H 0.635581 0.831176 0.634297 0.055 Uiso 0.414(8) 1 calc R U P A 2
H39D H 0.537647 0.752299 0.583675 0.055 Uiso 0.414(8) 1 calc R U P A 2
C34A C 0.4660(18) 0.9271(13) 0.2107(13) 0.076(6) Uani 0.414(8) 1 d . . P A 2
H34C H 0.432406 0.859881 0.191436 0.091 Uiso 0.414(8) 1 calc R U P A 2
H34D H 0.500427 0.962084 0.171168 0.091 Uiso 0.414(8) 1 calc R U P A 2
C40A C 0.5030(12) 0.8838(7) 0.5960(7) 0.051(3) Uani 0.414(8) 1 d . . P A 2
H40C H 0.483778 0.879702 0.646476 0.062 Uiso 0.414(8) 1 calc R U P A 2
H40D H 0.540399 0.951363 0.590124 0.062 Uiso 0.414(8) 1 calc R U P A 2
O8A O 0.4052(17) 0.8547(17) 0.5390(13) 0.035(3) Uani 0.414(8) 1 d . . P A 2
O10A O 0.3221(12) 0.9118(8) 0.2793(9) 0.062(4) Uani 0.414(8) 1 d . . P A 2
C30A C 0.2369(16) 0.8854(13) 0.4858(14) 0.062(7) Uani 0.414(8) 1 d . . P A 2
H30C H 0.207098 0.814960 0.479350 0.075 Uiso 0.414(8) 1 calc R U P A 2
H30D H 0.179330 0.914620 0.495175 0.075 Uiso 0.414(8) 1 calc R U P A 2
C32A C 0.2315(17) 0.9396(13) 0.2911(10) 0.079(6) Uani 0.414(8) 1 d . . P A 2
H32C H 0.173943 0.920346 0.246219 0.095 Uiso 0.414(8) 1 calc R U P A 2
H32D H 0.249603 1.010279 0.299034 0.095 Uiso 0.414(8) 1 calc R U P A 2
O9A O 0.2732(6) 0.9197(6) 0.4231(6) 0.056(3) Uani 0.414(8) 1 d . . P A 2
C33 C 0.3081(9) 0.9191(8) 0.2312(6) 0.061(3) Uani 0.586(8) 1 d . . P A 1
H33A H 0.266486 0.958525 0.200926 0.073 Uiso 0.586(8) 1 calc R U P A 1
H33B H 0.276658 0.851189 0.212778 0.073 Uiso 0.586(8) 1 calc R U P A 1
C31 C 0.1911(10) 0.9229(7) 0.3980(7) 0.066(3) Uani 0.586(8) 1 d . . P A 1
H31A H 0.115921 0.907570 0.406031 0.079 Uiso 0.586(8) 1 calc R U P A 1
H31B H 0.223065 0.992521 0.409889 0.079 Uiso 0.586(8) 1 calc R U P A 1
C31A C 0.192(2) 0.893(2) 0.3589(15) 0.085(10) Uani 0.414(8) 1 d . . P A 2
H31C H 0.127986 0.914381 0.366859 0.102 Uiso 0.414(8) 1 calc R U P A 2
H31D H 0.170259 0.822814 0.350072 0.102 Uiso 0.414(8) 1 calc R U P A 2
C33A C 0.381(2) 0.9720(13) 0.2276(12) 0.076(7) Uani 0.414(8) 1 d . . P A 2
H33C H 0.414568 1.037481 0.250953 0.091 Uiso 0.414(8) 1 calc R U P A 2
H33D H 0.331452 0.976689 0.180679 0.091 Uiso 0.414(8) 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 S4 2.1510(9) . ?
Ni1 S6 2.1579(11) . ?
Ni1 S5 2.1669(11) . ?
Ni1 S7 2.1570(10) . ?
Ni2 S15 2.1581(10) 2_667 ?
Ni2 S15 2.1581(10) . ?
Ni2 S14 2.1618(10) 2_667 ?
Ni2 S14 2.1619(10) . ?
Ni3 S20 2.1558(11) 2_666 ?
Ni3 S20 2.1558(11) . ?
Ni3 S19 2.1560(11) 2_666 ?
Ni3 S19 2.1560(11) . ?
S4 C3 1.707(4) . ?
S6 C5 1.714(4) . ?
S5 C2 1.712(4) . ?
S7 C4 1.719(4) . ?
S15 C9 1.719(4) . ?
S14 C8 1.714(4) . ?
S13 C9 1.743(4) . ?
S13 C7 1.732(5) . ?
S2 C3 1.733(4) . ?
S2 C1 1.738(4) . ?
S9 C4 1.742(4) . ?
S9 C6 1.732(5) . ?
S20 C12 1.718(4) . ?
S19 C11 1.717(4) . ?
S17 C11 1.733(4) . ?
S17 C10 1.735(5) . ?
S12 C7 1.740(4) . ?
S12 C8 1.750(4) . ?
S8 C5 1.744(4) . ?
S8 C6 1.736(5) . ?
S11 C7 1.635(5) . ?
S3 C2 1.744(4) . ?
S3 C1 1.745(4) . ?
S18 C12 1.750(4) . ?
S18 C10 1.722(5) . ?
S10 C6 1.641(5) . ?
S1 C1 1.624(4) . ?
S16 C10 1.638(5) . ?
O7 C26 1.414(4) . ?
O7 C27 1.419(5) . ?
O5 C14 1.426(5) . ?
O5 C15 1.413(5) . ?
O4 C13 1.405(5) . ?
O4 C24 1.427(5) . ?
O6 C16 1.433(5) . ?
O6 C17 1.400(5) . ?
O2 C21 1.414(5) . ?
O2 C20 1.442(5) . ?
O1 C18 1.434(5) . ?
O1 C19 1.424(6) . ?
O3 C22 1.425(5) . ?
O3 C23 1.409(5) . ?
N1 C25 1.483(4) . ?
O12 C37 1.36(3) . ?
O12 C36 1.31(2) . ?
N2 C28 1.483(4) . ?
O8 C40 1.40(2) . ?
O8 C29 1.451(18) . ?
O13 C38 1.31(3) . ?
O13 C39 1.39(3) . ?
C26 C25 1.494(6) . ?
C9 C8 1.358(5) . ?
C5 C4 1.359(6) . ?
C27 C28 1.488(6) . ?
C2 C3 1.368(5) . ?
C13 C14 1.498(6) . ?
C21 C22 1.485(6) . ?
C12 C11 1.357(6) . ?
C16 C15 1.479(7) . ?
C24 C23 1.481(6) . ?
C18 C17 1.491(7) . ?
O10 C32 1.44(2) . ?
O10 C33 1.420(14) . ?
C20 C19 1.472(7) . ?
O11 C35 1.403(18) . ?
O11 C34 1.427(14) . ?
C38 C37 1.47(3) . ?
C39 C40 1.43(3) . ?
C35 C36 1.53(2) . ?
O9 C30 1.413(14) . ?
O9 C31 1.418(13) . ?
C32 C31 1.41(2) . ?
C34 C33 1.462(19) . ?
C29 C30 1.46(2) . ?
C29A O8A 1.45(2) . ?
C29A C30A 1.54(3) . ?
O12A C37A 1.43(3) . ?
O12A C36A 1.46(3) . ?
C37A C38A 1.45(3) . ?
C36A C35A 1.45(3) . ?
C38A O13A 1.462(19) . ?
C35A O11A 1.41(3) . ?
O13A C39A 1.48(3) . ?
O11A C34A 1.39(2) . ?
C39A C40A 1.51(2) . ?
C34A C33A 1.49(3) . ?
C40A O8A 1.46(3) . ?
O10A C32A 1.40(2) . ?
O10A C33A 1.47(3) . ?
C30A O9A 1.36(2) . ?
C32A C31A 1.51(4) . ?
O9A C31A 1.41(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
S4 Ni1 S6 85.60(4) . . ?
S4 Ni1 S5 93.32(4) . . ?
S4 Ni1 S7 178.69(5) . . ?
S6 Ni1 S5 177.17(4) . . ?
S7 Ni1 S6 93.18(4) . . ?
S7 Ni1 S5 87.89(4) . . ?
S15 Ni2 S15 180.0 2_667 . ?
S15 Ni2 S14 86.67(4) 2_667 . ?
S15 Ni2 S14 93.33(4) . . ?
S15 Ni2 S14 86.67(4) . 2_667 ?
S15 Ni2 S14 93.33(4) 2_667 2_667 ?
S14 Ni2 S14 180.0 2_667 . ?
S20 Ni3 S20 180.0 . 2_666 ?
S20 Ni3 S19 86.49(4) 2_666 . ?
S20 Ni3 S19 93.51(4) 2_666 2_666 ?
S20 Ni3 S19 86.49(4) . 2_666 ?
S20 Ni3 S19 93.51(4) . . ?
S19 Ni3 S19 180.00(5) 2_666 . ?
C3 S4 Ni1 102.43(12) . . ?
C5 S6 Ni1 101.96(14) . . ?
C2 S5 Ni1 101.68(13) . . ?
C4 S7 Ni1 102.27(13) . . ?
C9 S15 Ni2 102.09(13) . . ?
C8 S14 Ni2 101.94(14) . . ?
C7 S13 C9 97.7(2) . . ?
C3 S2 C1 97.85(18) . . ?
C6 S9 C4 97.6(2) . . ?
C12 S20 Ni3 101.64(14) . . ?
C11 S19 Ni3 102.24(15) . . ?
C11 S17 C10 97.3(2) . . ?
C7 S12 C8 97.5(2) . . ?
C6 S8 C5 97.3(2) . . ?
C2 S3 C1 97.89(18) . . ?
C10 S18 C12 97.3(2) . . ?
C26 O7 C27 111.5(3) . . ?
C15 O5 C14 112.2(3) . . ?
C13 O4 C24 111.8(3) . . ?
C17 O6 C16 112.2(4) . . ?
C21 O2 C20 113.4(3) . . ?
C19 O1 C18 113.4(4) . . ?
C23 O3 C22 111.9(3) . . ?
C36 O12 C37 124.1(19) . . ?
C40 O8 C29 110.8(15) . . ?
C38 O13 C39 119.1(17) . . ?
O7 C26 C25 108.7(3) . . ?
S15 C9 S13 122.7(2) . . ?
C8 C9 S15 121.1(3) . . ?
C8 C9 S13 116.2(3) . . ?
S6 C5 S8 122.1(2) . . ?
C4 C5 S6 121.6(3) . . ?
C4 C5 S8 116.2(3) . . ?
O7 C27 C28 109.5(3) . . ?
N1 C25 C26 113.3(3) . . ?
N2 C28 C27 112.7(3) . . ?
S7 C4 S9 123.5(2) . . ?
C5 C4 S7 120.6(3) . . ?
C5 C4 S9 115.9(3) . . ?
S5 C2 S3 123.2(2) . . ?
C3 C2 S5 121.4(3) . . ?
C3 C2 S3 115.4(3) . . ?
O4 C13 C14 109.0(3) . . ?
O2 C21 C22 109.1(3) . . ?
O5 C14 C13 109.3(3) . . ?
S13 C7 S12 112.7(2) . . ?
S11 C7 S13 123.4(3) . . ?
S11 C7 S12 123.9(3) . . ?
S20 C12 S18 122.4(2) . . ?
C11 C12 S20 121.9(3) . . ?
C11 C12 S18 115.7(3) . . ?
O6 C16 C15 109.6(4) . . ?
S4 C3 S2 122.4(2) . . ?
C2 C3 S4 121.0(3) . . ?
C2 C3 S2 116.6(3) . . ?
O3 C22 C21 109.8(3) . . ?
S14 C8 S12 122.6(2) . . ?
C9 C8 S14 121.6(3) . . ?
C9 C8 S12 115.8(3) . . ?
S19 C11 S17 122.9(2) . . ?
C12 C11 S19 120.6(3) . . ?
C12 C11 S17 116.5(3) . . ?
O4 C24 C23 109.0(3) . . ?
O3 C23 C24 108.9(4) . . ?
O1 C18 C17 109.9(4) . . ?
S9 C6 S8 112.9(2) . . ?
S10 C6 S9 124.5(3) . . ?
S10 C6 S8 122.6(3) . . ?
O6 C17 C18 109.3(4) . . ?
S2 C1 S3 112.2(2) . . ?
S1 C1 S2 122.8(2) . . ?
S1 C1 S3 124.9(2) . . ?
C33 O10 C32 114.7(10) . . ?
O5 C15 C16 108.6(3) . . ?
S18 C10 S17 113.3(3) . . ?
S16 C10 S17 122.9(3) . . ?
S16 C10 S18 123.8(3) . . ?
O2 C20 C19 109.2(3) . . ?
O1 C19 C20 107.8(4) . . ?
C35 O11 C34 111.6(12) . . ?
O13 C38 C37 116(2) . . ?
O13 C39 C40 114.3(18) . . ?
O12 C37 C38 113.4(14) . . ?
O8 C40 C39 107.5(15) . . ?
O11 C35 C36 107.2(14) . . ?
C30 O9 C31 112.1(10) . . ?
C31 C32 O10 110.5(12) . . ?
O12 C36 C35 114.3(15) . . ?
O11 C34 C33 110.8(10) . . ?
O8 C29 C30 109.8(13) . . ?
O9 C30 C29 108.0(12) . . ?
O8A C29A C30A 106.1(13) . . ?
C37A O12A C36A 110(2) . . ?
O12A C37A C38A 111.5(16) . . ?
C35A C36A O12A 107.8(18) . . ?
C37A C38A O13A 106.3(15) . . ?
O11A C35A C36A 109.0(19) . . ?
C38A O13A C39A 109.0(14) . . ?
C34A O11A C35A 111.3(15) . . ?
O13A C39A C40A 102.8(17) . . ?
O11A C34A C33A 112(2) . . ?
O8A C40A C39A 111.2(15) . . ?
C29A O8A C40A 108.7(15) . . ?
C32A O10A C33A 113.4(14) . . ?
O9A C30A C29A 108.1(13) . . ?
O10A C32A C31A 110.6(17) . . ?
C30A O9A C31A 111.3(18) . . ?
O10 C33 C34 111.3(10) . . ?
C32 C31 O9 111.1(11) . . ?
O9A C31A C32A 110.1(19) . . ?
O10A C33A C34A 108.3(17) . . ?

_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 3.034
_oxdiff_exptl_absorpt_empirical_full_min 0.527
####################################################################### 
# 
# 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_exp_1088_10_273_00_auto
_database_code_depnum_ccdc_archive 'CCDC 2384661'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2024-09-17 deposited with the CCDC.	2024-11-08 downloaded from the CCDC.
;
_audit_creation_date             2023-09-12
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '4(C3 Ni0.5 S5), C4 H14 N2 O, 2(C12 H24 O6)'
_chemical_formula_sum            'C40 H62 N2 Ni2 O13 S20'
_chemical_formula_weight         1537.53
_chemical_melting_point          ?
_chemical_oxdiff_formula         C24H32N2O6NiS10
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                   13.1803(5)
_cell_length_b                   14.6150(7)
_cell_length_c                   18.0399(7)
_cell_angle_alpha                89.343(3)
_cell_angle_beta                 79.432(3)
_cell_angle_gamma                76.004(4)
_cell_volume                     3312.7(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    16636
_cell_measurement_temperature    272.9(3)
_cell_measurement_theta_max      28.9430
_cell_measurement_theta_min      1.6190
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.252
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72149
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.67a (Rigaku Oxford Diffraction, 2022)
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    1.541
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.83
_exptl_crystal_size_mid          0.546
_exptl_crystal_size_min          0.188
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            39008
_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         26.369
_diffrn_reflns_theta_min         1.621
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      272.9(3)
_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    -94.00 -69.00   0.50    1.20    --  -20.89 153.00-153.00   50
  2  ω   -112.00 -57.00   0.50    1.20    --  -20.89-153.00 165.00  110
  3  ω    -65.00 -39.00   0.50    1.20    --  -20.89 120.00  48.00   52
  4  ω     42.00 102.00   0.50    1.20    --   21.12-153.00 165.00  120
  5  ω     23.00  76.00   0.50    1.20    --   21.12-120.00 -35.00  106
  6  ω     31.00  56.00   0.50    1.20    --  -20.89  19.00-180.00   50
  7  ω    -22.00  59.00   0.50    1.20    --  -20.89  19.00  30.00  162
  8  ω    -24.00  60.00   0.50    1.20    --  -20.89  19.00 -30.00  168
  9  ω    -17.00  36.00   0.50    1.20    --  -20.89 -99.00 120.00  106
 10  ω    -24.00  10.00   0.50    1.20    --  -20.89  19.00-180.00   68
 11  ω     60.00  86.00   0.50    1.20    --   21.12 178.00-150.00   52
 12  ω    -65.00  28.00   0.50    1.20    --   21.12 -19.00  30.00  186
 13  ω    -74.00  23.00   0.50    1.20    --   21.12 -19.00-180.00  194
;
_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      0.0063181000
_diffrn_orient_matrix_UB_12      -0.0010878000
_diffrn_orient_matrix_UB_13      -0.0399073000
_diffrn_orient_matrix_UB_21      0.0199837000
_diffrn_orient_matrix_UB_22      -0.0496827000
_diffrn_orient_matrix_UB_23      -0.0008604000
_diffrn_orient_matrix_UB_31      -0.0524134000
_diffrn_orient_matrix_UB_32      -0.0059276000
_diffrn_orient_matrix_UB_33      0.0028856000
_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                8833
_reflns_number_total             13558
_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 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     736
_refine_ls_number_reflns         13558
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0528
_refine_ls_restrained_S_all      1.045
_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)+(0.0636P)²+1.6503P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1338
_refine_ls_wR_factor_ref         0.1520
_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. Uiso/Uaniso restraints and constraints
O8 \\sim C40: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
within 2A
3. Rigid body (RIGU) restrains
 O13A, C38A, C39
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H35C)=Sof(H35D)=Sof(H39C)=Sof(H39D)=Sof(C37A)=Sof(H37C)=Sof(H37D)=
 Sof(C36A)=Sof(H36C)=Sof(H36D)=Sof(O13A)=Sof(C38A)=Sof(H38C)=Sof(H38D)=1-FVAR(1)
 Sof(O13)=Sof(H35A)=Sof(H35B)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H39A)=Sof(H39B)=
 Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C36)=Sof(H36A)=Sof(H36B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C17(H17A,
 H17B), C19(H19A,H19B), C15(H15A,H15B), C23(H23A,H23B), C20(H20A,H20B),
 C16(H16A,H16B), C18(H18A,H18B), C24(H24A,H24B), C13(H13A,H13B), C14(H14A,H14B),
  C22(H22A,H22B), C21(H21A,H21B), C35(H35A,H35B), C35(H35C,H35D), C40(H40A,
 H40B), C30(H30A,H30B), C34(H34A,H34B), C29(H29A,H29B), C38(H38A,H38B),
 C31(H31A,H31B), C39(H39A,H39B), C39(H39C,H39D), C33(H33A,H33B), C32(H32A,H32B),
  C37(H37A,H37B), C36(H36A,H36B), C37A(H37C,H37D), C36A(H36C,H36D), C38A(H38C,
 H38D)
5.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(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
Ni2 Ni 0.500000 0.500000 0.500000 0.05979(19) Uani 1 2 d S . P . .
Ni1 Ni 0.29949(3) 0.92231(3) 0.48605(3) 0.06039(15) Uani 1 1 d . . . . .
Ni3 Ni 0.500000 0.500000 0.000000 0.0749(2) Uani 1 2 d S . P . .
S2 S 0.46943(7) 0.90253(7) 0.46150(6) 0.0660(3) Uani 1 1 d . . . . .
S12 S 0.57925(8) 0.52989(8) 0.39016(6) 0.0703(3) Uani 1 1 d . . . . .
S7 S 0.30517(8) 0.99842(8) 0.58635(7) 0.0702(3) Uani 1 1 d . . . . .
S11 S 0.58629(8) 0.35368(8) 0.49171(6) 0.0712(3) Uani 1 1 d . . . . .
S1 S 0.29864(8) 0.83883(8) 0.38768(7) 0.0716(3) Uani 1 1 d . . . . .
S4 S 0.63736(8) 0.78992(8) 0.33807(7) 0.0718(3) Uani 1 1 d . . . . .
S6 S 0.12881(7) 0.94293(8) 0.51371(7) 0.0765(3) Uani 1 1 d . . . . .
S3 S 0.48209(9) 0.72603(9) 0.27218(8) 0.0825(3) Uani 1 1 d . . . . .
S14 S 0.74760(9) 0.40332(9) 0.27294(7) 0.0812(3) Uani 1 1 d . . . . .
S13 S 0.75306(10) 0.24126(8) 0.36591(8) 0.0821(3) Uani 1 1 d . . . . .
S16 S 0.63509(11) 0.42351(10) -0.08010(7) 0.0875(4) Uani 1 1 d . . . . .
S8 S -0.02920(9) 1.02898(10) 0.65478(10) 0.0996(5) Uani 1 1 d . . . . .
S9 S 0.13509(11) 1.07633(9) 0.72180(9) 0.0952(4) Uani 1 1 d . . . . .
S15 S 0.90222(11) 0.22196(11) 0.21984(10) 0.1046(5) Uani 1 1 d . . . . .
S17 S 0.59384(11) 0.51118(11) 0.08361(7) 0.0964(4) Uani 1 1 d . . . . .
S5 S 0.71306(12) 0.65779(12) 0.20596(10) 0.1097(5) Uani 1 1 d . . . . .
S18 S 0.86879(12) 0.36539(10) -0.07154(8) 0.0966(4) Uani 1 1 d . . . . .
S10 S -0.08473(14) 1.11735(11) 0.80927(12) 0.1389(8) Uani 1 1 d . . . . .
S19 S 0.83197(12) 0.44594(14) 0.07827(8) 0.1175(5) Uani 1 1 d . . . . .
O7 O 0.7619(2) 0.67129(18) 0.80935(15) 0.0648(7) Uani 1 1 d . . . . .
N1 N 0.8824(2) 0.5982(2) 0.65791(17) 0.0577(7) Uani 1 1 d . . . . .
H1A H 0.908710 0.616393 0.612691 0.069 Uiso 1 1 calc R U . . .
H1B H 0.811613 0.614423 0.665349 0.069 Uiso 1 1 calc R U . . .
H1C H 0.904775 0.535913 0.660248 0.069 Uiso 1 1 calc R U . . .
S20 S 1.05187(15) 0.3540(2) 0.00426(12) 0.1624(9) Uani 1 1 d . . . . .
O6 O 0.7214(3) 0.7342(2) 0.59709(19) 0.0937(10) Uani 1 1 d . . . . .
N2 N 0.5804(3) 0.8102(2) 0.89789(19) 0.0691(9) Uani 1 1 d . . . . .
H2A H 0.612077 0.827801 0.854039 0.083 Uiso 1 1 calc R U . . .
H2B H 0.607377 0.828940 0.935156 0.083 Uiso 1 1 calc R U . . .
H2C H 0.510840 0.836468 0.904985 0.083 Uiso 1 1 calc R U . . .
O1 O 0.6704(3) 0.5701(3) 0.65681(19) 0.0903(9) Uani 1 1 d . . . . .
O5 O 0.9339(3) 0.7134(3) 0.52892(18) 0.0952(10) Uani 1 1 d . . . . .
O3 O 1.0255(3) 0.4123(3) 0.6437(2) 0.1079(12) Uani 1 1 d . . . . .
O4 O 1.0940(3) 0.5667(3) 0.5699(2) 0.1064(12) Uani 1 1 d . . . . .
O2 O 0.8190(3) 0.4284(2) 0.71295(19) 0.0991(11) Uani 1 1 d . . . . .
C2 C 0.5056(3) 0.8308(3) 0.3830(2) 0.0591(9) Uani 1 1 d . . . . .
C8 C 0.6614(3) 0.4225(3) 0.3599(2) 0.0658(10) Uani 1 1 d . . . . .
C7 C 0.6640(3) 0.3455(3) 0.4043(3) 0.0671(10) Uani 1 1 d . . . . .
C1 C 0.4320(3) 0.8017(3) 0.3505(2) 0.0636(10) Uani 1 1 d . . . . .
C25 C 0.9190(3) 0.6446(3) 0.7167(2) 0.0732(11) Uani 1 1 d . . . . .
H25A H 0.901518 0.712221 0.710059 0.088 Uiso 1 1 calc R U . . .
H25B H 0.995763 0.623204 0.710319 0.088 Uiso 1 1 calc R U . . .
C5 C 0.1748(3) 1.0228(3) 0.6326(3) 0.0743(12) Uani 1 1 d . . . . .
C4 C 0.0991(3) 0.9983(3) 0.6006(3) 0.0742(12) Uani 1 1 d . . . . .
C26 C 0.8706(3) 0.6251(3) 0.7947(3) 0.0746(11) Uani 1 1 d . . . . .
H26A H 0.879062 0.557699 0.799970 0.090 Uiso 1 1 calc R U . . .
H26B H 0.906353 0.647306 0.830762 0.090 Uiso 1 1 calc R U . . .
C9 C 0.8069(3) 0.2849(3) 0.2823(3) 0.0788(12) Uani 1 1 d . . . . .
C3 C 0.6173(3) 0.7206(3) 0.2677(3) 0.0764(12) Uani 1 1 d . . . . .
C27 C 0.7136(4) 0.6574(3) 0.8837(3) 0.0774(12) Uani 1 1 d . . . . .
H27A H 0.748160 0.682205 0.919205 0.093 Uiso 1 1 calc R U . . .
H27B H 0.721921 0.590481 0.891563 0.093 Uiso 1 1 calc R U . . .
C11 C 0.7198(4) 0.4563(4) 0.0384(3) 0.0832(13) Uani 1 1 d . . . . .
C28 C 0.5986(4) 0.7060(3) 0.8970(3) 0.0822(13) Uani 1 1 d . . . . .
H28A H 0.566361 0.686259 0.857746 0.099 Uiso 1 1 calc R U . . .
H28B H 0.564012 0.687265 0.944959 0.099 Uiso 1 1 calc R U . . .
C6 C 0.0017(4) 1.0749(3) 0.7329(3) 0.0991(18) Uani 1 1 d . . . . .
C10 C 0.7380(4) 0.4179(3) -0.0327(3) 0.0787(12) Uani 1 1 d . . . . .
C17 C 0.6231(4) 0.7095(4) 0.5951(4) 0.112(2) Uani 1 1 d . . . . .
H17A H 0.629740 0.672581 0.549357 0.135 Uiso 1 1 calc R U . . .
H17B H 0.566728 0.766195 0.595275 0.135 Uiso 1 1 calc R U . . .
C19 C 0.6432(5) 0.5095(5) 0.7163(3) 0.108(2) Uani 1 1 d . . . . .
H19A H 0.572262 0.501501 0.716503 0.129 Uiso 1 1 calc R U . . .
H19B H 0.643457 0.538052 0.764539 0.129 Uiso 1 1 calc R U . . .
C15 C 0.8573(6) 0.8023(4) 0.5367(3) 0.124(2) Uani 1 1 d . . . . .
H15A H 0.875146 0.841375 0.494887 0.149 Uiso 1 1 calc R U . . .
H15B H 0.858009 0.834682 0.583137 0.149 Uiso 1 1 calc R U . . .
C23 C 1.1355(5) 0.4207(5) 0.6259(5) 0.143(3) Uani 1 1 d . . . . .
H23A H 1.183494 0.358354 0.618159 0.171 Uiso 1 1 calc R U . . .
H23B H 1.151652 0.452394 0.667541 0.171 Uiso 1 1 calc R U . . .
C20 C 0.7200(6) 0.4173(5) 0.7056(3) 0.125(3) Uani 1 1 d . . . . .
H20A H 0.697394 0.374506 0.742977 0.151 Uiso 1 1 calc R U . . .
H20B H 0.723639 0.390609 0.655944 0.151 Uiso 1 1 calc R U . . .
C16 C 0.7498(6) 0.7868(4) 0.5378(4) 0.119(2) Uani 1 1 d . . . . .
H16A H 0.698305 0.847304 0.541273 0.143 Uiso 1 1 calc R U . . .
H16B H 0.749355 0.754849 0.491045 0.143 Uiso 1 1 calc R U . . .
C18 C 0.5970(4) 0.6547(5) 0.6611(4) 0.114(2) Uani 1 1 d . . . . .
H18A H 0.596427 0.689580 0.706620 0.137 Uiso 1 1 calc R U . . .
H18B H 0.526717 0.644022 0.663323 0.137 Uiso 1 1 calc R U . . .
C24 C 1.1504(4) 0.4750(7) 0.5568(4) 0.140(3) Uani 1 1 d . . . . .
H24A H 1.225348 0.472686 0.540667 0.168 Uiso 1 1 calc R U . . .
H24B H 1.126711 0.446909 0.516674 0.168 Uiso 1 1 calc R U . . .
C13 C 1.1107(5) 0.6261(6) 0.5054(3) 0.123(3) Uani 1 1 d . . . . .
H13A H 1.097536 0.597808 0.460816 0.148 Uiso 1 1 calc R U . . .
H13B H 1.183728 0.631826 0.495555 0.148 Uiso 1 1 calc R U . . .
C14 C 1.0375(6) 0.7202(6) 0.5220(4) 0.132(3) Uani 1 1 d . . . . .
H14A H 1.047374 0.746436 0.568547 0.159 Uiso 1 1 calc R U . . .
H14B H 1.053006 0.762029 0.481713 0.159 Uiso 1 1 calc R U . . .
C22 C 1.0043(8) 0.3590(5) 0.7066(5) 0.158(4) Uani 1 1 d . . . . .
H22A H 1.003585 0.393484 0.752420 0.189 Uiso 1 1 calc R U . . .
H22B H 1.058442 0.300126 0.703435 0.189 Uiso 1 1 calc R U . . .
C12 C 0.9245(5) 0.3868(4) 0.0044(3) 0.1045(17) Uani 1 1 d . . . . .
C21 C 0.8992(8) 0.3403(4) 0.7071(4) 0.142(3) Uani 1 1 d . . . . .
H21A H 0.900796 0.305955 0.661088 0.171 Uiso 1 1 calc R U . . .
H21B H 0.881978 0.301839 0.749501 0.171 Uiso 1 1 calc R U . . .
O12 O 0.5753(4) 0.8589(3) 1.0535(2) 0.1046(11) Uani 1 1 d . . . . .
O10 O 0.3647(4) 0.8559(4) 0.8651(4) 0.1394(16) Uani 1 1 d . . . . .
O11 O 0.3891(4) 0.8359(4) 1.0095(3) 0.1395(17) Uani 1 1 d . . . . .
O8 O 0.7157(4) 0.9215(3) 0.8083(3) 0.1191(13) Uani 1 1 d . U . . .
O13 O 0.7563(11) 0.8613(9) 0.9495(7) 0.093(3) Uani 0.533(15) 1 d . . P A 1
O9 O 0.5345(4) 0.8956(3) 0.7586(3) 0.1321(15) Uani 1 1 d . . . . .
C35 C 0.4033(7) 0.8403(6) 1.0834(4) 0.127(2) Uani 1 1 d . . . . .
H35A H 0.364024 0.799327 1.112267 0.153 Uiso 0.533(15) 1 calc R U P A 1
H35B H 0.370342 0.904161 1.103045 0.153 Uiso 0.533(15) 1 calc R U P A 1
H35C H 0.429126 0.776429 1.099023 0.153 Uiso 0.467(15) 1 calc R U P A 2
H35D H 0.334481 0.866152 1.115056 0.153 Uiso 0.467(15) 1 calc R U P A 2
C40 C 0.8151(5) 0.8970(5) 0.8270(5) 0.121(2) Uani 1 1 d . U . . .
H40A H 0.858761 0.933639 0.796969 0.145 Uiso 1 1 calc R U . . .
H40B H 0.846248 0.831177 0.811986 0.145 Uiso 1 1 calc R U . . .
C30 C 0.6000(7) 0.9519(5) 0.7211(4) 0.141(3) Uani 1 1 d . . . . .
H30A H 0.571507 1.017131 0.738780 0.169 Uiso 1 1 calc R U . . .
H30B H 0.600954 0.948888 0.667282 0.169 Uiso 1 1 calc R U . . .
C34 C 0.3044(7) 0.8218(6) 0.9910(6) 0.159(3) Uani 1 1 d . . . . .
H34A H 0.244877 0.870907 1.016068 0.190 Uiso 1 1 calc R U . . .
H34B H 0.294516 0.762418 1.011879 0.190 Uiso 1 1 calc R U . . .
C29 C 0.7060(8) 0.9195(6) 0.7350(4) 0.148(3) Uani 1 1 d . . . . .
H29A H 0.734291 0.855250 0.715051 0.177 Uiso 1 1 calc R U . . .
H29B H 0.749664 0.957980 0.707302 0.177 Uiso 1 1 calc R U . . .
C38 C 0.7417(19) 0.8857(16) 1.0312(9) 0.106(7) Uani 0.533(15) 1 d . . P A 1
H38A H 0.810514 0.875260 1.046099 0.127 Uiso 0.533(15) 1 calc R U P A 1
H38B H 0.705722 0.951847 1.040691 0.127 Uiso 0.533(15) 1 calc R U P A 1
C31 C 0.4321(7) 0.9191(6) 0.7506(5) 0.157(3) Uani 1 1 d . . . . .
H31A H 0.430439 0.919165 0.697013 0.189 Uiso 1 1 calc R U . . .
H31B H 0.401044 0.983188 0.770331 0.189 Uiso 1 1 calc R U . . .
C39 C 0.8224(6) 0.9083(5) 0.9015(6) 0.140(3) Uani 1 1 d . . . . .
H39A H 0.802104 0.974986 0.915573 0.168 Uiso 0.533(15) 1 calc R U P A 1
H39B H 0.895596 0.883702 0.907471 0.168 Uiso 0.533(15) 1 calc R U P A 1
H39C H 0.883138 0.861253 0.912424 0.168 Uiso 0.467(15) 1 calc R U P A 2
H39D H 0.834810 0.969978 0.909136 0.168 Uiso 0.467(15) 1 calc R U P A 2
C33 C 0.2967(7) 0.8187(7) 0.9119(7) 0.184(4) Uani 1 1 d . . . . .
H33A H 0.307076 0.753365 0.896125 0.220 Uiso 1 1 calc R U . . .
H33B H 0.225011 0.851538 0.906950 0.220 Uiso 1 1 calc R U . . .
C32 C 0.3660(7) 0.8613(7) 0.7855(6) 0.169(4) Uani 1 1 d . . . . .
H32A H 0.391361 0.798279 0.762434 0.202 Uiso 1 1 calc R U . . .
H32B H 0.294060 0.886501 0.777041 0.202 Uiso 1 1 calc R U . . .
C37 C 0.6861(18) 0.8344(13) 1.0702(8) 0.136(6) Uani 0.533(15) 1 d . . P A 1
H37A H 0.683425 0.845144 1.123555 0.164 Uiso 0.533(15) 1 calc R U P A 1
H37B H 0.718962 0.768171 1.057644 0.164 Uiso 0.533(15) 1 calc R U P A 1
C36 C 0.5125(16) 0.8151(14) 1.0993(7) 0.159(8) Uani 0.533(15) 1 d . . P A 1
H36A H 0.510837 0.832560 1.151252 0.191 Uiso 0.533(15) 1 calc R U P A 1
H36B H 0.540920 0.747376 1.092583 0.191 Uiso 0.533(15) 1 calc R U P A 1
C37A C 0.6493(16) 0.9052(13) 1.0698(12) 0.123(6) Uani 0.467(15) 1 d . . P A 2
H37C H 0.669068 0.885710 1.117807 0.147 Uiso 0.467(15) 1 calc R U P A 2
H37D H 0.619658 0.972881 1.072673 0.147 Uiso 0.467(15) 1 calc R U P A 2
C36A C 0.4727(14) 0.8932(10) 1.0970(7) 0.108(6) Uani 0.467(15) 1 d . . P A 2
H36C H 0.477023 0.891405 1.150147 0.129 Uiso 0.467(15) 1 calc R U P A 2
H36D H 0.445186 0.958339 1.085183 0.129 Uiso 0.467(15) 1 calc R U P A 2
O13A O 0.7433(19) 0.9011(18) 0.9452(16) 0.174(10) Uani 0.467(15) 1 d . . P A 2
C38A C 0.747(4) 0.879(4) 1.006(3) 0.220(19) Uani 0.467(15) 1 d . . P A 2
H38C H 0.801680 0.903994 1.021714 0.263 Uiso 0.467(15) 1 calc R U P A 2
H38D H 0.771296 0.810951 1.004803 0.263 Uiso 0.467(15) 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
Ni2 S12 2.1563(10) 2_666 ?
Ni2 S12 2.1563(10) . ?
Ni2 S11 2.1581(11) . ?
Ni2 S11 2.1580(11) 2_666 ?
Ni1 S2 2.1500(10) . ?
Ni1 S7 2.1572(13) . ?
Ni1 S1 2.1682(13) . ?
Ni1 S6 2.1597(10) . ?
Ni3 S16 2.1537(14) 2_665 ?
Ni3 S16 2.1537(14) . ?
Ni3 S17 2.1493(12) . ?
Ni3 S17 2.1493(12) 2_665 ?
S2 C2 1.695(4) . ?
S12 C8 1.707(4) . ?
S7 C5 1.721(4) . ?
S11 C7 1.704(5) . ?
S1 C1 1.717(4) . ?
S4 C2 1.738(4) . ?
S4 C3 1.729(5) . ?
S6 C4 1.707(5) . ?
S3 C1 1.731(4) . ?
S3 C3 1.751(4) . ?
S14 C8 1.741(4) . ?
S14 C9 1.739(5) . ?
S13 C7 1.743(4) . ?
S13 C9 1.729(5) . ?
S16 C10 1.717(5) . ?
S8 C4 1.747(4) . ?
S8 C6 1.722(7) . ?
S9 C5 1.731(5) . ?
S9 C6 1.738(5) . ?
S15 C9 1.625(5) . ?
S17 C11 1.714(5) . ?
S5 C3 1.620(5) . ?
S18 C10 1.726(5) . ?
S18 C12 1.734(5) . ?
S10 C6 1.638(6) . ?
S19 C11 1.734(5) . ?
S19 C12 1.712(6) . ?
O7 C26 1.405(5) . ?
O7 C27 1.410(5) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C25 1.476(5) . ?
S20 C12 1.630(6) . ?
O6 C17 1.434(6) . ?
O6 C16 1.360(7) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
N2 C28 1.483(5) . ?
O1 C19 1.433(6) . ?
O1 C18 1.366(7) . ?
O5 C15 1.430(7) . ?
O5 C14 1.375(7) . ?
O3 C23 1.460(8) . ?
O3 C22 1.394(9) . ?
O4 C24 1.365(8) . ?
O4 C13 1.461(8) . ?
O2 C20 1.384(7) . ?
O2 C21 1.445(8) . ?
C2 C1 1.372(5) . ?
C8 C7 1.372(5) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C26 1.489(6) . ?
C5 C4 1.359(6) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 C28 1.487(6) . ?
C11 C10 1.363(6) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C18 1.461(8) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.467(9) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C16 1.484(9) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C24 1.478(10) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.473(10) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C21 1.474(10) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
O12 C37 1.502(19) . ?
O12 C36 1.330(16) . ?
O12 C37A 1.387(17) . ?
O12 C36A 1.410(16) . ?
O10 C33 1.327(10) . ?
O10 C32 1.434(10) . ?
O11 C35 1.385(8) . ?
O11 C34 1.284(9) . ?
O8 C40 1.375(7) . ?
O8 C29 1.353(8) . ?
O13 C38 1.49(2) . ?
O13 C39 1.408(15) . ?
O9 C30 1.413(8) . ?
O9 C31 1.345(8) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C35 H35C 0.9700 . ?
C35 H35D 0.9700 . ?
C35 C36 1.476(19) . ?
C35 C36A 1.386(16) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C40 C39 1.378(9) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 C29 1.430(10) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C34 C33 1.451(12) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C38 C37 1.29(3) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 C32 1.418(11) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C39 H39C 0.9700 . ?
C39 H39D 0.9700 . ?
C39 O13A 1.21(2) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37A H37C 0.9700 . ?
C37A H37D 0.9700 . ?
C37A C38A 1.53(5) . ?
C36A H36C 0.9700 . ?
C36A H36D 0.9700 . ?
O13A C38A 1.15(6) . ?
C38A H38C 0.9700 . ?
C38A H38D 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
S12 Ni2 S12 180.0 2_666 . ?
S12 Ni2 S11 86.75(4) . 2_666 ?
S12 Ni2 S11 86.75(4) 2_666 . ?
S12 Ni2 S11 93.25(4) 2_666 2_666 ?
S12 Ni2 S11 93.25(4) . . ?
S11 Ni2 S11 180.0 2_666 . ?
S2 Ni1 S7 85.45(4) . . ?
S2 Ni1 S1 93.23(4) . . ?
S2 Ni1 S6 178.53(5) . . ?
S7 Ni1 S1 176.85(5) . . ?
S7 Ni1 S6 93.16(5) . . ?
S6 Ni1 S1 88.13(5) . . ?
S16 Ni3 S16 180.0 2_665 . ?
S17 Ni3 S16 86.52(5) 2_665 . ?
S17 Ni3 S16 86.52(5) . 2_665 ?
S17 Ni3 S16 93.48(5) . . ?
S17 Ni3 S16 93.48(5) 2_665 2_665 ?
S17 Ni3 S17 180.0 . 2_665 ?
C2 S2 Ni1 102.48(12) . . ?
C8 S12 Ni2 102.24(15) . . ?
C5 S7 Ni1 102.15(17) . . ?
C7 S11 Ni2 102.19(14) . . ?
C1 S1 Ni1 101.87(14) . . ?
C3 S4 C2 98.5(2) . . ?
C4 S6 Ni1 101.99(14) . . ?
C1 S3 C3 98.0(2) . . ?
C9 S14 C8 98.0(2) . . ?
C9 S13 C7 98.2(2) . . ?
C10 S16 Ni3 102.16(17) . . ?
C6 S8 C4 97.9(2) . . ?
C5 S9 C6 96.9(3) . . ?
C11 S17 Ni3 102.19(16) . . ?
C10 S18 C12 97.4(3) . . ?
C12 S19 C11 98.1(3) . . ?
C26 O7 C27 111.4(3) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C25 N1 H1A 109.5 . . ?
C25 N1 H1B 109.5 . . ?
C25 N1 H1C 109.5 . . ?
C16 O6 C17 112.4(5) . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C28 N2 H2A 109.5 . . ?
C28 N2 H2B 109.5 . . ?
C28 N2 H2C 109.5 . . ?
C18 O1 C19 112.4(5) . . ?
C14 O5 C15 114.2(5) . . ?
C22 O3 C23 113.9(5) . . ?
C24 O4 C13 113.5(5) . . ?
C20 O2 C21 113.3(5) . . ?
S2 C2 S4 122.7(2) . . ?
C1 C2 S2 121.8(3) . . ?
C1 C2 S4 115.5(3) . . ?
S12 C8 S14 123.2(2) . . ?
C7 C8 S12 121.0(3) . . ?
C7 C8 S14 115.8(3) . . ?
S11 C7 S13 123.2(2) . . ?
C8 C7 S11 121.3(3) . . ?
C8 C7 S13 115.6(3) . . ?
S1 C1 S3 123.3(2) . . ?
C2 C1 S1 120.6(3) . . ?
C2 C1 S3 116.1(3) . . ?
N1 C25 H25A 109.0 . . ?
N1 C25 H25B 109.0 . . ?
N1 C25 C26 113.1(3) . . ?
H25A C25 H25B 107.8 . . ?
C26 C25 H25A 109.0 . . ?
C26 C25 H25B 109.0 . . ?
S7 C5 S9 122.0(3) . . ?
C4 C5 S7 120.6(4) . . ?
C4 C5 S9 117.4(3) . . ?
S6 C4 S8 123.5(3) . . ?
C5 C4 S6 121.8(3) . . ?
C5 C4 S8 114.7(4) . . ?
O7 C26 C25 109.4(3) . . ?
O7 C26 H26A 109.8 . . ?
O7 C26 H26B 109.8 . . ?
C25 C26 H26A 109.8 . . ?
C25 C26 H26B 109.8 . . ?
H26A C26 H26B 108.2 . . ?
S13 C9 S14 112.4(3) . . ?
S15 C9 S14 124.1(3) . . ?
S15 C9 S13 123.6(3) . . ?
S4 C3 S3 111.9(3) . . ?
S5 C3 S4 123.5(3) . . ?
S5 C3 S3 124.6(3) . . ?
O7 C27 H27A 109.6 . . ?
O7 C27 H27B 109.6 . . ?
O7 C27 C28 110.1(4) . . ?
H27A C27 H27B 108.2 . . ?
C28 C27 H27A 109.6 . . ?
C28 C27 H27B 109.6 . . ?
S17 C11 S19 123.4(3) . . ?
C10 C11 S17 121.3(4) . . ?
C10 C11 S19 115.3(4) . . ?
N2 C28 C27 112.3(3) . . ?
N2 C28 H28A 109.1 . . ?
N2 C28 H28B 109.1 . . ?
C27 C28 H28A 109.1 . . ?
C27 C28 H28B 109.1 . . ?
H28A C28 H28B 107.9 . . ?
S8 C6 S9 113.1(3) . . ?
S10 C6 S8 124.6(3) . . ?
S10 C6 S9 122.3(4) . . ?
S16 C10 S18 122.8(3) . . ?
C11 C10 S16 120.8(4) . . ?
C11 C10 S18 116.4(4) . . ?
O6 C17 H17A 109.8 . . ?
O6 C17 H17B 109.8 . . ?
O6 C17 C18 109.2(4) . . ?
H17A C17 H17B 108.3 . . ?
C18 C17 H17A 109.8 . . ?
C18 C17 H17B 109.8 . . ?
O1 C19 H19A 109.6 . . ?
O1 C19 H19B 109.6 . . ?
O1 C19 C20 110.1(5) . . ?
H19A C19 H19B 108.2 . . ?
C20 C19 H19A 109.6 . . ?
C20 C19 H19B 109.6 . . ?
O5 C15 H15A 109.8 . . ?
O5 C15 H15B 109.8 . . ?
O5 C15 C16 109.6(4) . . ?
H15A C15 H15B 108.2 . . ?
C16 C15 H15A 109.8 . . ?
C16 C15 H15B 109.8 . . ?
O3 C23 H23A 109.8 . . ?
O3 C23 H23B 109.8 . . ?
O3 C23 C24 109.5(4) . . ?
H23A C23 H23B 108.2 . . ?
C24 C23 H23A 109.8 . . ?
C24 C23 H23B 109.8 . . ?
O2 C20 C19 109.2(4) . . ?
O2 C20 H20A 109.8 . . ?
O2 C20 H20B 109.8 . . ?
C19 C20 H20A 109.8 . . ?
C19 C20 H20B 109.8 . . ?
H20A C20 H20B 108.3 . . ?
O6 C16 C15 111.0(5) . . ?
O6 C16 H16A 109.4 . . ?
O6 C16 H16B 109.4 . . ?
C15 C16 H16A 109.4 . . ?
C15 C16 H16B 109.4 . . ?
H16A C16 H16B 108.0 . . ?
O1 C18 C17 110.0(5) . . ?
O1 C18 H18A 109.7 . . ?
O1 C18 H18B 109.7 . . ?
C17 C18 H18A 109.7 . . ?
C17 C18 H18B 109.7 . . ?
H18A C18 H18B 108.2 . . ?
O4 C24 C23 110.5(5) . . ?
O4 C24 H24A 109.6 . . ?
O4 C24 H24B 109.6 . . ?
C23 C24 H24A 109.6 . . ?
C23 C24 H24B 109.6 . . ?
H24A C24 H24B 108.1 . . ?
O4 C13 H13A 109.9 . . ?
O4 C13 H13B 109.9 . . ?
O4 C13 C14 109.1(5) . . ?
H13A C13 H13B 108.3 . . ?
C14 C13 H13A 109.9 . . ?
C14 C13 H13B 109.9 . . ?
O5 C14 C13 110.0(5) . . ?
O5 C14 H14A 109.7 . . ?
O5 C14 H14B 109.7 . . ?
C13 C14 H14A 109.7 . . ?
C13 C14 H14B 109.7 . . ?
H14A C14 H14B 108.2 . . ?
O3 C22 H22A 110.3 . . ?
O3 C22 H22B 110.3 . . ?
O3 C22 C21 106.9(5) . . ?
H22A C22 H22B 108.6 . . ?
C21 C22 H22A 110.3 . . ?
C21 C22 H22B 110.3 . . ?
S19 C12 S18 112.9(3) . . ?
S20 C12 S18 122.9(4) . . ?
S20 C12 S19 124.2(3) . . ?
O2 C21 C22 109.9(5) . . ?
O2 C21 H21A 109.7 . . ?
O2 C21 H21B 109.7 . . ?
C22 C21 H21A 109.7 . . ?
C22 C21 H21B 109.7 . . ?
H21A C21 H21B 108.2 . . ?
C36 O12 C37 111.0(12) . . ?
C37A O12 C36A 113.4(11) . . ?
C33 O10 C32 123.2(7) . . ?
C34 O11 C35 123.6(6) . . ?
C29 O8 C40 119.7(6) . . ?
C39 O13 C38 115.0(11) . . ?
C31 O9 C30 116.3(6) . . ?
O11 C35 H35A 107.6 . . ?
O11 C35 H35B 107.6 . . ?
O11 C35 H35C 108.3 . . ?
O11 C35 H35D 108.3 . . ?
O11 C35 C36 119.0(7) . . ?
O11 C35 C36A 116.0(7) . . ?
H35A C35 H35B 107.0 . . ?
H35C C35 H35D 107.4 . . ?
C36 C35 H35A 107.6 . . ?
C36 C35 H35B 107.6 . . ?
C36A C35 H35C 108.3 . . ?
C36A C35 H35D 108.3 . . ?
O8 C40 H40A 107.8 . . ?
O8 C40 H40B 107.8 . . ?
O8 C40 C39 117.9(6) . . ?
H40A C40 H40B 107.2 . . ?
C39 C40 H40A 107.8 . . ?
C39 C40 H40B 107.8 . . ?
O9 C30 H30A 109.6 . . ?
O9 C30 H30B 109.6 . . ?
O9 C30 C29 110.2(5) . . ?
H30A C30 H30B 108.1 . . ?
C29 C30 H30A 109.6 . . ?
C29 C30 H30B 109.6 . . ?
O11 C34 H34A 107.4 . . ?
O11 C34 H34B 107.4 . . ?
O11 C34 C33 119.6(7) . . ?
H34A C34 H34B 107.0 . . ?
C33 C34 H34A 107.4 . . ?
C33 C34 H34B 107.4 . . ?
O8 C29 C30 115.4(7) . . ?
O8 C29 H29A 108.4 . . ?
O8 C29 H29B 108.4 . . ?
C30 C29 H29A 108.4 . . ?
C30 C29 H29B 108.4 . . ?
H29A C29 H29B 107.5 . . ?
O13 C38 H38A 109.7 . . ?
O13 C38 H38B 109.7 . . ?
H38A C38 H38B 108.2 . . ?
C37 C38 O13 109.8(14) . . ?
C37 C38 H38A 109.7 . . ?
C37 C38 H38B 109.7 . . ?
O9 C31 H31A 108.0 . . ?
O9 C31 H31B 108.0 . . ?
O9 C31 C32 117.1(7) . . ?
H31A C31 H31B 107.3 . . ?
C32 C31 H31A 108.0 . . ?
C32 C31 H31B 108.0 . . ?
O13 C39 H39A 109.4 . . ?
O13 C39 H39B 109.4 . . ?
C40 C39 O13 111.4(7) . . ?
C40 C39 H39A 109.4 . . ?
C40 C39 H39B 109.4 . . ?
C40 C39 H39C 109.0 . . ?
C40 C39 H39D 109.0 . . ?
H39A C39 H39B 108.0 . . ?
H39C C39 H39D 107.8 . . ?
O13A C39 C40 113.0(16) . . ?
O13A C39 H39C 109.0 . . ?
O13A C39 H39D 109.0 . . ?
O10 C33 C34 115.8(7) . . ?
O10 C33 H33A 108.3 . . ?
O10 C33 H33B 108.3 . . ?
C34 C33 H33A 108.3 . . ?
C34 C33 H33B 108.3 . . ?
H33A C33 H33B 107.4 . . ?
O10 C32 H32A 109.2 . . ?
O10 C32 H32B 109.2 . . ?
C31 C32 O10 111.9(7) . . ?
C31 C32 H32A 109.2 . . ?
C31 C32 H32B 109.2 . . ?
H32A C32 H32B 107.9 . . ?
O12 C37 H37A 109.8 . . ?
O12 C37 H37B 109.8 . . ?
C38 C37 O12 109.6(13) . . ?
C38 C37 H37A 109.8 . . ?
C38 C37 H37B 109.8 . . ?
H37A C37 H37B 108.2 . . ?
O12 C36 C35 110.9(11) . . ?
O12 C36 H36A 109.5 . . ?
O12 C36 H36B 109.5 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 108.0 . . ?
O12 C37A H37C 110.2 . . ?
O12 C37A H37D 110.2 . . ?
O12 C37A C38A 107(2) . . ?
H37C C37A H37D 108.5 . . ?
C38A C37A H37C 110.2 . . ?
C38A C37A H37D 110.2 . . ?
O12 C36A H36C 109.3 . . ?
O12 C36A H36D 109.3 . . ?
C35 C36A O12 111.6(10) . . ?
C35 C36A H36C 109.3 . . ?
C35 C36A H36D 109.3 . . ?
H36C C36A H36D 108.0 . . ?
C38A O13A C39 121(4) . . ?
C37A C38A H38C 106.8 . . ?
C37A C38A H38D 106.8 . . ?
O13A C38A C37A 122(4) . . ?
O13A C38A H38C 106.8 . . ?
O13A C38A H38D 106.8 . . ?
H38C C38A H38D 106.6 . . ?

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
Ni2 S12 C8 S14 -179.5(2) . . . . ?
Ni2 S12 C8 C7 -0.5(3) . . . . ?
Ni2 S11 C7 S13 179.86(19) . . . . ?
Ni2 S11 C7 C8 1.0(3) . . . . ?
Ni1 S2 C2 S4 -179.2(2) . . . . ?
Ni1 S2 C2 C1 1.2(3) . . . . ?
Ni1 S7 C5 S9 175.0(2) . . . . ?
Ni1 S7 C5 C4 -3.5(4) . . . . ?
Ni1 S1 C1 S3 176.7(2) . . . . ?
Ni1 S1 C1 C2 -2.7(3) . . . . ?
Ni1 S6 C4 S8 -177.0(2) . . . . ?
Ni1 S6 C4 C5 3.6(4) . . . . ?
Ni3 S16 C10 S18 -178.5(2) . . . . ?
Ni3 S16 C10 C11 0.8(4) . . . . ?
Ni3 S17 C11 S19 178.4(3) . . . . ?
Ni3 S17 C11 C10 -1.2(4) . . . . ?
S2 C2 C1 S1 1.1(5) . . . . ?
S2 C2 C1 S3 -178.3(2) . . . . ?
S12 C8 C7 S11 -0.4(5) . . . . ?
S12 C8 C7 S13 -179.3(2) . . . . ?
S7 C5 C4 S6 -0.1(5) . . . . ?
S7 C5 C4 S8 -179.5(2) . . . . ?
S4 C2 C1 S1 -178.5(2) . . . . ?
S4 C2 C1 S3 2.1(4) . . . . ?
S14 C8 C7 S11 178.6(2) . . . . ?
S14 C8 C7 S13 -0.3(4) . . . . ?
S9 C5 C4 S6 -178.7(2) . . . . ?
S9 C5 C4 S8 1.9(4) . . . . ?
S17 C11 C10 S16 0.3(6) . . . . ?
S17 C11 C10 S18 179.7(2) . . . . ?
S19 C11 C10 S16 -179.3(2) . . . . ?
S19 C11 C10 S18 0.0(5) . . . . ?
O7 C27 C28 N2 -68.4(5) . . . . ?
N1 C25 C26 O7 -69.7(4) . . . . ?
O6 C17 C18 O1 -66.0(6) . . . . ?
O1 C19 C20 O2 65.2(6) . . . . ?
O5 C15 C16 O6 61.1(7) . . . . ?
O3 C23 C24 O4 67.6(6) . . . . ?
O3 C22 C21 O2 -60.8(7) . . . . ?
O4 C13 C14 O5 -65.2(6) . . . . ?
C2 S4 C3 S3 1.7(3) . . . . ?
C2 S4 C3 S5 -177.8(3) . . . . ?
C8 S14 C9 S13 2.6(3) . . . . ?
C8 S14 C9 S15 -177.3(3) . . . . ?
C7 S13 C9 S14 -2.7(3) . . . . ?
C7 S13 C9 S15 177.2(3) . . . . ?
C1 S3 C3 S4 -0.8(3) . . . . ?
C1 S3 C3 S5 178.7(3) . . . . ?
C5 S9 C6 S8 -2.4(3) . . . . ?
C5 S9 C6 S10 179.9(3) . . . . ?
C4 S8 C6 S9 3.2(3) . . . . ?
C4 S8 C6 S10 -179.2(3) . . . . ?
C26 O7 C27 C28 -179.3(3) . . . . ?
C9 S14 C8 S12 177.6(2) . . . . ?
C9 S14 C8 C7 -1.4(3) . . . . ?
C9 S13 C7 S11 -177.1(2) . . . . ?
C9 S13 C7 C8 1.8(3) . . . . ?
C3 S4 C2 S2 178.1(3) . . . . ?
C3 S4 C2 C1 -2.3(3) . . . . ?
C3 S3 C1 S1 179.8(3) . . . . ?
C3 S3 C1 C2 -0.8(3) . . . . ?
C27 O7 C26 C25 -177.9(3) . . . . ?
C11 S19 C12 S18 0.0(4) . . . . ?
C11 S19 C12 S20 179.7(4) . . . . ?
C6 S8 C4 S6 177.5(3) . . . . ?
C6 S8 C4 C5 -3.1(4) . . . . ?
C6 S9 C5 S7 -178.3(3) . . . . ?
C6 S9 C5 C4 0.3(4) . . . . ?
C10 S18 C12 S19 -0.1(4) . . . . ?
C10 S18 C12 S20 -179.7(4) . . . . ?
C17 O6 C16 C15 -173.7(5) . . . . ?
C19 O1 C18 C17 -174.4(4) . . . . ?
C15 O5 C14 C13 -173.3(5) . . . . ?
C23 O3 C22 C21 -168.1(5) . . . . ?
C20 O2 C21 C22 173.5(5) . . . . ?
C16 O6 C17 C18 -179.0(5) . . . . ?
C18 O1 C19 C20 175.6(5) . . . . ?
C24 O4 C13 C14 173.5(5) . . . . ?
C13 O4 C24 C23 176.1(4) . . . . ?
C14 O5 C15 C16 175.7(5) . . . . ?
C22 O3 C23 C24 177.7(5) . . . . ?
C12 S18 C10 S16 179.3(3) . . . . ?
C12 S18 C10 C11 0.0(4) . . . . ?
C12 S19 C11 S17 -179.7(3) . . . . ?
C12 S19 C11 C10 0.0(4) . . . . ?
C21 O2 C20 C19 177.0(5) . . . . ?
O12 C37A C38A O13A 65(6) . . . . ?
O11 C35 C36 O12 48.6(18) . . . . ?
O11 C35 C36A O12 -58.8(14) . . . . ?
O11 C34 C33 O10 -17.7(15) . . . . ?
O8 C40 C39 O13 54.4(11) . . . . ?
O8 C40 C39 O13A 28.6(17) . . . . ?
O13 C38 C37 O12 -66(2) . . . . ?
O9 C30 C29 O8 -60.1(9) . . . . ?
O9 C31 C32 O10 57.0(11) . . . . ?
C35 O11 C34 C33 179.8(8) . . . . ?
C40 O8 C29 C30 -176.2(6) . . . . ?
C40 C39 O13A C38A 155(5) . . . . ?
C30 O9 C31 C32 177.7(8) . . . . ?
C34 O11 C35 C36 153.4(12) . . . . ?
C34 O11 C35 C36A -153.6(10) . . . . ?
C29 O8 C40 C39 174.0(7) . . . . ?
C38 O13 C39 C40 -167.8(12) . . . . ?
C31 O9 C30 C29 179.6(7) . . . . ?
C39 O13 C38 C37 -175.7(17) . . . . ?
C39 O13A C38A C37A 156(3) . . . . ?
C33 O10 C32 C31 169.1(8) . . . . ?
C32 O10 C33 C34 -178.1(8) . . . . ?
C37 O12 C36 C35 179.3(11) . . . . ?
C36 O12 C37 C38 -172.7(15) . . . . ?
C37A O12 C36A C35 -175.2(12) . . . . ?
C36A O12 C37A C38A -166(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 2.907
_oxdiff_exptl_absorpt_empirical_full_min 0.521
####################################################################### 
# 
# 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_exp_1088_11_293_00_auto
_database_code_depnum_ccdc_archive 'CCDC 2384662'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2024-09-17 deposited with the CCDC.	2024-11-08 downloaded from the CCDC.
;
_audit_creation_date             2023-09-12
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '4(C3 Ni0.5 S5), C4 H14 N2 O, 2(C12 H24 O6)'
_chemical_formula_sum            'C40 H62 N2 Ni2 O13 S20'
_chemical_formula_weight         1537.53
_chemical_melting_point          ?
_chemical_oxdiff_formula         C24H32N2O6NiS10
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                   13.1866(5)
_cell_length_b                   14.6416(5)
_cell_length_c                   18.0448(7)
_cell_angle_alpha                89.198(3)
_cell_angle_beta                 79.443(3)
_cell_angle_gamma                76.205(3)
_cell_volume                     3324.6(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    16158
_cell_measurement_temperature    293.0(2)
_cell_measurement_theta_max      29.0810
_cell_measurement_theta_min      1.6180
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.248
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80751
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.67a (Rigaku Oxford Diffraction, 2022)
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    1.536
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.698
_exptl_crystal_size_mid          0.564
_exptl_crystal_size_min          0.177
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            39226
_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         1.618
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293.0(2)
_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    -94.00 -69.00   0.50    1.20    --  -20.89 153.00-153.00   50
  2  ω   -112.00 -57.00   0.50    1.20    --  -20.89-153.00 165.00  110
  3  ω    -65.00 -39.00   0.50    1.20    --  -20.89 120.00  48.00   52
  4  ω     42.00 102.00   0.50    1.20    --   21.12-153.00 165.00  120
  5  ω     23.00  76.00   0.50    1.20    --   21.12-120.00 -35.00  106
  6  ω     31.00  56.00   0.50    1.20    --  -20.89  19.00-180.00   50
  7  ω    -22.00  59.00   0.50    1.20    --  -20.89  19.00  30.00  162
  8  ω    -24.00  60.00   0.50    1.20    --  -20.89  19.00 -30.00  168
  9  ω    -17.00  36.00   0.50    1.20    --  -20.89 -99.00 120.00  106
 10  ω    -24.00  10.00   0.50    1.20    --  -20.89  19.00-180.00   68
 11  ω     60.00  86.00   0.50    1.20    --   21.12 178.00-150.00   52
 12  ω    -65.00  28.00   0.50    1.20    --   21.12 -19.00  30.00  186
 13  ω    -74.00  23.00   0.50    1.20    --   21.12 -19.00-180.00  194
;
_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      0.0062159000
_diffrn_orient_matrix_UB_12      -0.0013210000
_diffrn_orient_matrix_UB_13      -0.0398851000
_diffrn_orient_matrix_UB_21      0.0197030000
_diffrn_orient_matrix_UB_22      -0.0495396000
_diffrn_orient_matrix_UB_23      -0.0005505000
_diffrn_orient_matrix_UB_31      -0.0524393000
_diffrn_orient_matrix_UB_32      -0.0058981000
_diffrn_orient_matrix_UB_33      0.0030297000
_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                8445
_reflns_number_total             13618
_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 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     736
_refine_ls_number_reflns         13618
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0516
_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)+(0.0641P)²+1.4696P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1297
_refine_ls_wR_factor_ref         0.1497
_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. Uiso/Uaniso restraints and constraints
C36 \\sim C35: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
O8 \\sim C40: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
within 2A
3. Rigid body (RIGU) restrains
 C38A, O13A, C39
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C22, O3, C23
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H35C)=Sof(H35D)=Sof(H39C)=Sof(H39D)=Sof(C37A)=Sof(H37C)=Sof(H37D)=
 Sof(C36A)=Sof(H36C)=Sof(H36D)=Sof(O13A)=Sof(C38A)=Sof(H38C)=Sof(H38D)=1-FVAR(1)
 Sof(O13)=Sof(H35A)=Sof(H35B)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H39A)=Sof(H39B)=
 Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C36)=Sof(H36A)=Sof(H36B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C17(H17A,
 H17B), C19(H19A,H19B), C15(H15A,H15B), C23(H23A,H23B), C20(H20A,H20B),
 C16(H16A,H16B), C18(H18A,H18B), C24(H24A,H24B), C13(H13A,H13B), C14(H14A,H14B),
  C22(H22A,H22B), C21(H21A,H21B), C35(H35A,H35B), C35(H35C,H35D), C40(H40A,
 H40B), C30(H30A,H30B), C34(H34A,H34B), C29(H29A,H29B), C38(H38A,H38B),
 C31(H31A,H31B), C39(H39A,H39B), C39(H39C,H39D), C33(H33A,H33B), C32(H32A,H32B),
  C37(H37A,H37B), C36(H36A,H36B), C37A(H37C,H37D), C36A(H36C,H36D), C38A(H38C,
 H38D)
5.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(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
Ni2 Ni 0.500000 0.500000 0.500000 0.06354(19) Uani 1 2 d S . P . .
Ni1 Ni 0.29950(3) 0.92248(3) 0.48633(3) 0.06450(16) Uani 1 1 d . . . . .
Ni3 Ni 0.500000 0.500000 0.000000 0.0810(2) Uani 1 2 d S . P . .
S2 S 0.46940(7) 0.90245(7) 0.46169(7) 0.0707(3) Uani 1 1 d . . . . .
S12 S 0.57957(8) 0.53000(8) 0.39019(6) 0.0753(3) Uani 1 1 d . . . . .
S7 S 0.30535(8) 0.99837(8) 0.58645(7) 0.0747(3) Uani 1 1 d . . . . .
S11 S 0.58536(8) 0.35399(8) 0.49172(6) 0.0755(3) Uani 1 1 d . . . . .
S1 S 0.29856(8) 0.83932(8) 0.38804(7) 0.0766(3) Uani 1 1 d . . . . .
S4 S 0.63690(8) 0.79005(8) 0.33852(7) 0.0761(3) Uani 1 1 d . . . . .
S6 S 0.12903(7) 0.94307(8) 0.51402(8) 0.0822(3) Uani 1 1 d . . . . .
S3 S 0.48154(9) 0.72696(9) 0.27263(8) 0.0870(3) Uani 1 1 d . . . . .
S14 S 0.74749(9) 0.40375(9) 0.27303(7) 0.0861(3) Uani 1 1 d . . . . .
S13 S 0.75168(9) 0.24168(8) 0.36598(8) 0.0868(3) Uani 1 1 d . . . . .
S16 S 0.63479(12) 0.42281(10) -0.07965(7) 0.0944(4) Uani 1 1 d . . . . .
S8 S -0.02878(9) 1.02910(10) 0.65488(10) 0.1065(5) Uani 1 1 d . . . . .
S9 S 0.13533(11) 1.07632(10) 0.72172(9) 0.1010(4) Uani 1 1 d . . . . .
S15 S 0.90124(11) 0.22258(11) 0.21997(10) 0.1113(5) Uani 1 1 d . . . . .
S17 S 0.59422(12) 0.51137(12) 0.08326(7) 0.1039(4) Uani 1 1 d . . . . .
S5 S 0.71227(12) 0.65844(12) 0.20651(9) 0.1143(5) Uani 1 1 d . . . . .
S18 S 0.86812(12) 0.36459(11) -0.07120(8) 0.1051(4) Uani 1 1 d . . . . .
S10 S -0.08437(15) 1.11742(12) 0.80915(12) 0.1486(8) Uani 1 1 d . . . . .
S19 S 0.83186(13) 0.44641(15) 0.07791(8) 0.1271(6) Uani 1 1 d . . . . .
O7 O 0.7619(2) 0.67072(18) 0.80961(15) 0.0695(7) Uani 1 1 d . . . . .
N1 N 0.8823(2) 0.5980(2) 0.65831(17) 0.0610(7) Uani 1 1 d . . . . .
H1A H 0.908564 0.616672 0.613209 0.073 Uiso 1 1 calc R U . . .
H1B H 0.811684 0.614197 0.665857 0.073 Uiso 1 1 calc R U . . .
H1C H 0.904448 0.535815 0.660304 0.073 Uiso 1 1 calc R U . . .
S20 S 1.05123(16) 0.3538(2) 0.00411(12) 0.1740(10) Uani 1 1 d . . . . .
O6 O 0.7233(3) 0.7339(2) 0.59691(19) 0.0990(10) Uani 1 1 d . . . . .
N2 N 0.5810(3) 0.8097(2) 0.89794(19) 0.0740(9) Uani 1 1 d . . . . .
H2A H 0.611973 0.827514 0.853882 0.089 Uiso 1 1 calc R U . . .
H2B H 0.608730 0.828376 0.934817 0.089 Uiso 1 1 calc R U . . .
H2C H 0.511562 0.835731 0.905571 0.089 Uiso 1 1 calc R U . . .
O1 O 0.6709(3) 0.5704(3) 0.65661(19) 0.0974(10) Uani 1 1 d . . . . .
O5 O 0.9355(3) 0.7122(3) 0.52935(18) 0.1031(11) Uani 1 1 d . . . . .
O3 O 1.0245(3) 0.4121(3) 0.6439(2) 0.1170(13) Uani 1 1 d . . . . .
O4 O 1.0941(3) 0.5654(4) 0.5706(2) 0.1152(13) Uani 1 1 d . . . . .
O2 O 0.8181(3) 0.4285(2) 0.71278(19) 0.1062(11) Uani 1 1 d . . . . .
C2 C 0.5053(3) 0.8313(3) 0.3832(2) 0.0629(9) Uani 1 1 d . . . . .
C8 C 0.6611(3) 0.4225(3) 0.3598(2) 0.0692(10) Uani 1 1 d . . . . .
C7 C 0.6631(3) 0.3459(3) 0.4044(2) 0.0702(11) Uani 1 1 d . . . . .
C1 C 0.4314(3) 0.8024(3) 0.3512(2) 0.0672(10) Uani 1 1 d . . . . .
C25 C 0.9195(3) 0.6435(3) 0.7174(2) 0.0784(12) Uani 1 1 d . . . . .
H25A H 0.903220 0.710918 0.710594 0.094 Uiso 1 1 calc R U . . .
H25B H 0.996062 0.621441 0.711163 0.094 Uiso 1 1 calc R U . . .
C5 C 0.1747(3) 1.0227(3) 0.6328(3) 0.0770(12) Uani 1 1 d . . . . .
C4 C 0.0989(3) 0.9986(3) 0.6008(3) 0.0790(12) Uani 1 1 d . . . . .
C26 C 0.8706(3) 0.6244(3) 0.7954(2) 0.0781(12) Uani 1 1 d . . . . .
H26A H 0.878654 0.557260 0.801070 0.094 Uiso 1 1 calc R U . . .
H26B H 0.906267 0.646754 0.831449 0.094 Uiso 1 1 calc R U . . .
C9 C 0.8054(3) 0.2856(3) 0.2829(3) 0.0825(12) Uani 1 1 d . . . . .
C3 C 0.6167(3) 0.7212(3) 0.2681(3) 0.0811(12) Uani 1 1 d . . . . .
C27 C 0.7133(4) 0.6574(3) 0.8843(3) 0.0842(12) Uani 1 1 d . . . . .
H27A H 0.747910 0.682236 0.919697 0.101 Uiso 1 1 calc R U . . .
H27B H 0.721061 0.590653 0.892698 0.101 Uiso 1 1 calc R U . . .
C11 C 0.7193(4) 0.4567(4) 0.0383(3) 0.0876(13) Uani 1 1 d . . . . .
C28 C 0.5991(4) 0.7058(3) 0.8972(3) 0.0870(13) Uani 1 1 d . . . . .
H28A H 0.564226 0.687007 0.945028 0.104 Uiso 1 1 calc R U . . .
H28B H 0.567079 0.686128 0.857803 0.104 Uiso 1 1 calc R U . . .
C6 C 0.0019(4) 1.0753(3) 0.7327(4) 0.1085(19) Uani 1 1 d . . . . .
C10 C 0.7374(4) 0.4175(3) -0.0326(3) 0.0844(13) Uani 1 1 d . . . . .
C17 C 0.6243(4) 0.7098(5) 0.5952(4) 0.121(2) Uani 1 1 d . . . . .
H17A H 0.630064 0.673705 0.549272 0.146 Uiso 1 1 calc R U . . .
H17B H 0.568364 0.766591 0.595851 0.146 Uiso 1 1 calc R U . . .
C19 C 0.6429(5) 0.5100(6) 0.7159(3) 0.119(2) Uani 1 1 d . . . . .
H19A H 0.571863 0.502343 0.715900 0.143 Uiso 1 1 calc R U . . .
H19B H 0.643299 0.538079 0.764200 0.143 Uiso 1 1 calc R U . . .
C15 C 0.8585(7) 0.8019(4) 0.5364(4) 0.131(2) Uani 1 1 d . . . . .
H15A H 0.876465 0.840274 0.494076 0.157 Uiso 1 1 calc R U . . .
H15B H 0.859854 0.834851 0.582364 0.157 Uiso 1 1 calc R U . . .
C23 C 1.1349(5) 0.4196(5) 0.6265(5) 0.157(3) Uani 1 1 d . . . . .
H23A H 1.182242 0.357321 0.618776 0.188 Uiso 1 1 calc R U . . .
H23B H 1.151363 0.450886 0.668207 0.188 Uiso 1 1 calc R U . . .
C20 C 0.7190(7) 0.4180(5) 0.7050(3) 0.137(3) Uani 1 1 d . . . . .
H20A H 0.695982 0.374972 0.742092 0.164 Uiso 1 1 calc R U . . .
H20B H 0.722660 0.391930 0.655214 0.164 Uiso 1 1 calc R U . . .
C16 C 0.7513(6) 0.7869(4) 0.5383(4) 0.128(2) Uani 1 1 d . . . . .
H16A H 0.700253 0.847368 0.542526 0.154 Uiso 1 1 calc R U . . .
H16B H 0.749784 0.755991 0.491471 0.154 Uiso 1 1 calc R U . . .
C18 C 0.5986(4) 0.6548(6) 0.6602(4) 0.125(2) Uani 1 1 d . . . . .
H18A H 0.597913 0.689414 0.705833 0.150 Uiso 1 1 calc R U . . .
H18B H 0.528258 0.644290 0.662310 0.150 Uiso 1 1 calc R U . . .
C24 C 1.1497(4) 0.4740(7) 0.5575(4) 0.154(3) Uani 1 1 d . . . . .
H24A H 1.224651 0.471648 0.541252 0.185 Uiso 1 1 calc R U . . .
H24B H 1.125627 0.446332 0.517515 0.185 Uiso 1 1 calc R U . . .
C13 C 1.1114(5) 0.6249(7) 0.5058(3) 0.137(3) Uani 1 1 d . . . . .
H13A H 1.098202 0.596771 0.461266 0.165 Uiso 1 1 calc R U . . .
H13B H 1.184373 0.630665 0.496127 0.165 Uiso 1 1 calc R U . . .
C14 C 1.0386(7) 0.7185(6) 0.5224(4) 0.145(3) Uani 1 1 d . . . . .
H14A H 1.048746 0.744589 0.568795 0.175 Uiso 1 1 calc R U . . .
H14B H 1.054267 0.760340 0.482009 0.175 Uiso 1 1 calc R U . . .
C22 C 1.0028(8) 0.3589(5) 0.7065(5) 0.169(3) Uani 1 1 d . . . . .
H22A H 1.002046 0.393097 0.752270 0.203 Uiso 1 1 calc R U . . .
H22B H 1.056641 0.300193 0.703389 0.203 Uiso 1 1 calc R U . . .
C12 C 0.9242(5) 0.3861(4) 0.0047(3) 0.1149(18) Uani 1 1 d . . . . .
C21 C 0.8983(8) 0.3402(4) 0.7068(4) 0.157(3) Uani 1 1 d . . . . .
H21A H 0.899683 0.306298 0.660699 0.188 Uiso 1 1 calc R U . . .
H21B H 0.880911 0.301544 0.749071 0.188 Uiso 1 1 calc R U . . .
O12 O 0.5741(4) 0.8590(3) 1.0542(2) 0.1128(12) Uani 1 1 d . . . . .
O10 O 0.3662(4) 0.8562(4) 0.8639(4) 0.1480(17) Uani 1 1 d . . . . .
O11 O 0.3892(4) 0.8368(4) 1.0089(3) 0.1472(17) Uani 1 1 d . . . . .
O8 O 0.7174(4) 0.9207(3) 0.8090(3) 0.1233(13) Uani 1 1 d . U . . .
O13 O 0.7576(11) 0.8614(9) 0.9499(7) 0.096(4) Uani 0.539(16) 1 d . . P A 1
O9 O 0.5362(4) 0.8958(3) 0.7582(2) 0.1350(14) Uani 1 1 d . . . . .
C35 C 0.4026(7) 0.8414(6) 1.0830(4) 0.137(3) Uani 1 1 d . U . . .
H35A H 0.362583 0.800919 1.111914 0.165 Uiso 0.539(16) 1 calc R U P A 1
H35B H 0.370424 0.905239 1.102236 0.165 Uiso 0.539(16) 1 calc R U P A 1
H35C H 0.333552 0.866634 1.114258 0.165 Uiso 0.461(16) 1 calc R U P A 2
H35D H 0.428603 0.777814 1.098776 0.165 Uiso 0.461(16) 1 calc R U P A 2
C40 C 0.8159(5) 0.8964(5) 0.8283(5) 0.125(2) Uani 1 1 d . U . . .
H40A H 0.859505 0.933801 0.798972 0.150 Uiso 1 1 calc R U . . .
H40B H 0.847344 0.831146 0.812729 0.150 Uiso 1 1 calc R U . . .
C30 C 0.6023(7) 0.9509(5) 0.7208(4) 0.145(3) Uani 1 1 d . . . . .
H30A H 0.573421 1.016179 0.737334 0.174 Uiso 1 1 calc R U . . .
H30B H 0.604291 0.946646 0.666961 0.174 Uiso 1 1 calc R U . . .
C34 C 0.3045(7) 0.8229(6) 0.9897(6) 0.169(3) Uani 1 1 d . . . . .
H34A H 0.245214 0.872451 1.013757 0.203 Uiso 1 1 calc R U . . .
H34B H 0.293356 0.764157 1.011192 0.203 Uiso 1 1 calc R U . . .
C29 C 0.7077(8) 0.9203(6) 0.7357(5) 0.156(3) Uani 1 1 d . . . . .
H29A H 0.737484 0.856874 0.714864 0.187 Uiso 1 1 calc R U . . .
H29B H 0.750286 0.960290 0.708911 0.187 Uiso 1 1 calc R U . . .
C38 C 0.7441(19) 0.8827(17) 1.0299(10) 0.113(7) Uani 0.539(16) 1 d . . P A 1
H38A H 0.813335 0.867669 1.044419 0.135 Uiso 0.539(16) 1 calc R U P A 1
H38B H 0.714303 0.949701 1.039031 0.135 Uiso 0.539(16) 1 calc R U P A 1
C31 C 0.4344(8) 0.9192(6) 0.7493(5) 0.171(3) Uani 1 1 d . . . . .
H31A H 0.433462 0.918985 0.695686 0.206 Uiso 1 1 calc R U . . .
H31B H 0.403410 0.983140 0.768710 0.206 Uiso 1 1 calc R U . . .
C39 C 0.8225(6) 0.9065(6) 0.9034(6) 0.150(3) Uani 1 1 d . . . . .
H39A H 0.895349 0.881308 0.909610 0.179 Uiso 0.539(16) 1 calc R U P A 1
H39B H 0.803169 0.972883 0.917681 0.179 Uiso 0.539(16) 1 calc R U P A 1
H39C H 0.881367 0.857767 0.914495 0.179 Uiso 0.461(16) 1 calc R U P A 2
H39D H 0.838284 0.966734 0.910948 0.179 Uiso 0.461(16) 1 calc R U P A 2
C33 C 0.2983(8) 0.8187(8) 0.9110(8) 0.198(5) Uani 1 1 d . . . . .
H33A H 0.309692 0.753174 0.895799 0.238 Uiso 1 1 calc R U . . .
H33B H 0.226799 0.850304 0.905299 0.238 Uiso 1 1 calc R U . . .
C32 C 0.3681(7) 0.8612(7) 0.7842(6) 0.177(4) Uani 1 1 d . . . . .
H32A H 0.393554 0.798359 0.761498 0.212 Uiso 1 1 calc R U . . .
H32B H 0.296404 0.886097 0.775427 0.212 Uiso 1 1 calc R U . . .
C37 C 0.684(2) 0.8381(17) 1.0717(9) 0.153(7) Uani 0.539(16) 1 d . . P A 1
H37A H 0.679743 0.855136 1.124188 0.184 Uiso 0.539(16) 1 calc R U P A 1
H37B H 0.715366 0.771065 1.064851 0.184 Uiso 0.539(16) 1 calc R U P A 1
C36 C 0.5119(17) 0.8154(15) 1.0988(8) 0.182(9) Uani 0.539(16) 1 d . U P A 1
H36A H 0.510610 0.831770 1.150877 0.219 Uiso 0.539(16) 1 calc R U P A 1
H36B H 0.539900 0.747913 1.091467 0.219 Uiso 0.539(16) 1 calc R U P A 1
C37A C 0.6487(18) 0.9058(13) 1.0697(14) 0.129(7) Uani 0.461(16) 1 d . . P A 2
H37C H 0.665229 0.890698 1.119312 0.155 Uiso 0.461(16) 1 calc R U P A 2
H37D H 0.622251 0.973356 1.067681 0.155 Uiso 0.461(16) 1 calc R U P A 2
C36A C 0.4710(14) 0.8948(11) 1.0969(7) 0.109(6) Uani 0.461(16) 1 d . . P A 2
H36C H 0.474206 0.894175 1.150131 0.130 Uiso 0.461(16) 1 calc R U P A 2
H36D H 0.444300 0.959494 1.083751 0.130 Uiso 0.461(16) 1 calc R U P A 2
O13A O 0.7395(19) 0.9020(17) 0.9495(18) 0.180(10) Uani 0.461(16) 1 d . . P A 2
C38A C 0.747(4) 0.870(4) 1.008(3) 0.29(3) Uani 0.461(16) 1 d . . P A 2
H38C H 0.808049 0.885648 1.023853 0.354 Uiso 0.461(16) 1 calc R U P A 2
H38D H 0.761437 0.802506 1.003212 0.354 Uiso 0.461(16) 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
Ni2 S12 2.1572(11) 2_666 ?
Ni2 S12 2.1573(11) . ?
Ni2 S11 2.1586(11) . ?
Ni2 S11 2.1586(11) 2_666 ?
Ni1 S2 2.1513(10) . ?
Ni1 S7 2.1570(13) . ?
Ni1 S1 2.1689(13) . ?
Ni1 S6 2.1595(10) . ?
Ni3 S16 2.1572(14) 2_665 ?
Ni3 S16 2.1572(14) . ?
Ni3 S17 2.1490(12) . ?
Ni3 S17 2.1490(12) 2_665 ?
S2 C2 1.696(4) . ?
S12 C8 1.713(4) . ?
S7 C5 1.727(4) . ?
S11 C7 1.705(4) . ?
S1 C1 1.713(4) . ?
S4 C2 1.739(4) . ?
S4 C3 1.729(5) . ?
S6 C4 1.710(5) . ?
S3 C1 1.738(4) . ?
S3 C3 1.751(4) . ?
S14 C8 1.742(4) . ?
S14 C9 1.738(5) . ?
S13 C7 1.748(4) . ?
S13 C9 1.722(5) . ?
S16 C10 1.711(5) . ?
S8 C4 1.743(4) . ?
S8 C6 1.720(7) . ?
S9 C5 1.731(5) . ?
S9 C6 1.737(5) . ?
S15 C9 1.638(5) . ?
S17 C11 1.708(5) . ?
S5 C3 1.622(5) . ?
S18 C10 1.730(5) . ?
S18 C12 1.737(6) . ?
S10 C6 1.641(6) . ?
S19 C11 1.737(5) . ?
S19 C12 1.714(6) . ?
O7 C26 1.409(5) . ?
O7 C27 1.415(5) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C25 1.478(5) . ?
S20 C12 1.627(6) . ?
O6 C17 1.437(6) . ?
O6 C16 1.353(7) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
N2 C28 1.483(5) . ?
O1 C19 1.430(6) . ?
O1 C18 1.364(7) . ?
O5 C15 1.446(7) . ?
O5 C14 1.367(7) . ?
O3 C23 1.462(8) . ?
O3 C22 1.388(9) . ?
O4 C24 1.364(9) . ?
O4 C13 1.465(8) . ?
O2 C20 1.384(8) . ?
O2 C21 1.453(8) . ?
C2 C1 1.368(5) . ?
C8 C7 1.368(5) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C26 1.489(6) . ?
C5 C4 1.357(6) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 C28 1.480(6) . ?
C11 C10 1.367(6) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C18 1.448(8) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.467(9) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C16 1.476(9) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C24 1.477(10) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.472(10) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C21 1.467(10) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
O12 C37 1.50(2) . ?
O12 C36 1.312(18) . ?
O12 C37A 1.39(2) . ?
O12 C36A 1.416(15) . ?
O10 C33 1.330(10) . ?
O10 C32 1.434(10) . ?
O11 C35 1.385(8) . ?
O11 C34 1.290(10) . ?
O8 C40 1.369(7) . ?
O8 C29 1.353(8) . ?
O13 C38 1.45(2) . ?
O13 C39 1.365(15) . ?
O9 C30 1.403(8) . ?
O9 C31 1.343(9) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C35 H35C 0.9700 . ?
C35 H35D 0.9700 . ?
C35 C36 1.48(2) . ?
C35 C36A 1.383(16) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C40 C39 1.386(9) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 C29 1.428(10) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C34 C33 1.440(12) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C38 C37 1.28(3) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 C32 1.421(11) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C39 H39C 0.9700 . ?
C39 H39D 0.9700 . ?
C39 O13A 1.26(2) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37A H37C 0.9700 . ?
C37A H37D 0.9700 . ?
C37A C38A 1.54(6) . ?
C36A H36C 0.9700 . ?
C36A H36D 0.9700 . ?
O13A C38A 1.16(7) . ?
C38A H38C 0.9700 . ?
C38A H38D 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
S12 Ni2 S12 180.0 2_666 . ?
S12 Ni2 S11 86.82(4) . 2_666 ?
S12 Ni2 S11 86.82(4) 2_666 . ?
S12 Ni2 S11 93.18(4) 2_666 2_666 ?
S12 Ni2 S11 93.18(4) . . ?
S11 Ni2 S11 180.0 2_666 . ?
S2 Ni1 S7 85.64(4) . . ?
S2 Ni1 S1 93.00(4) . . ?
S2 Ni1 S6 178.56(6) . . ?
S7 Ni1 S1 176.88(5) . . ?
S7 Ni1 S6 93.04(5) . . ?
S6 Ni1 S1 88.29(5) . . ?
S16 Ni3 S16 180.0 2_665 . ?
S17 Ni3 S16 86.68(5) 2_665 . ?
S17 Ni3 S16 86.68(5) . 2_665 ?
S17 Ni3 S16 93.32(5) . . ?
S17 Ni3 S16 93.32(5) 2_665 2_665 ?
S17 Ni3 S17 180.0 . 2_665 ?
C2 S2 Ni1 102.66(12) . . ?
C8 S12 Ni2 102.28(14) . . ?
C5 S7 Ni1 102.20(17) . . ?
C7 S11 Ni2 102.28(14) . . ?
C1 S1 Ni1 101.88(14) . . ?
C3 S4 C2 98.6(2) . . ?
C4 S6 Ni1 102.31(14) . . ?
C1 S3 C3 98.2(2) . . ?
C9 S14 C8 97.6(2) . . ?
C9 S13 C7 98.0(2) . . ?
C10 S16 Ni3 102.26(18) . . ?
C6 S8 C4 98.0(2) . . ?
C5 S9 C6 96.8(3) . . ?
C11 S17 Ni3 102.20(16) . . ?
C10 S18 C12 97.5(3) . . ?
C12 S19 C11 98.4(3) . . ?
C26 O7 C27 111.3(3) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C25 N1 H1A 109.5 . . ?
C25 N1 H1B 109.5 . . ?
C25 N1 H1C 109.5 . . ?
C16 O6 C17 112.4(5) . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C28 N2 H2A 109.5 . . ?
C28 N2 H2B 109.5 . . ?
C28 N2 H2C 109.5 . . ?
C18 O1 C19 112.7(5) . . ?
C14 O5 C15 114.5(5) . . ?
C22 O3 C23 113.6(6) . . ?
C24 O4 C13 113.3(6) . . ?
C20 O2 C21 113.5(5) . . ?
S2 C2 S4 122.8(2) . . ?
C1 C2 S2 121.4(3) . . ?
C1 C2 S4 115.8(3) . . ?
S12 C8 S14 123.1(2) . . ?
C7 C8 S12 120.9(3) . . ?
C7 C8 S14 116.0(3) . . ?
S11 C7 S13 123.2(2) . . ?
C8 C7 S11 121.4(3) . . ?
C8 C7 S13 115.4(3) . . ?
S1 C1 S3 123.3(2) . . ?
C2 C1 S1 121.0(3) . . ?
C2 C1 S3 115.7(3) . . ?
N1 C25 H25A 108.9 . . ?
N1 C25 H25B 108.9 . . ?
N1 C25 C26 113.4(3) . . ?
H25A C25 H25B 107.7 . . ?
C26 C25 H25A 108.9 . . ?
C26 C25 H25B 108.9 . . ?
S7 C5 S9 121.9(3) . . ?
C4 C5 S7 120.7(4) . . ?
C4 C5 S9 117.4(3) . . ?
S6 C4 S8 123.8(3) . . ?
C5 C4 S6 121.5(3) . . ?
C5 C4 S8 114.7(4) . . ?
O7 C26 C25 109.4(3) . . ?
O7 C26 H26A 109.8 . . ?
O7 C26 H26B 109.8 . . ?
C25 C26 H26A 109.8 . . ?
C25 C26 H26B 109.8 . . ?
H26A C26 H26B 108.2 . . ?
S13 C9 S14 112.8(3) . . ?
S15 C9 S14 123.7(3) . . ?
S15 C9 S13 123.5(3) . . ?
S4 C3 S3 111.7(3) . . ?
S5 C3 S4 123.6(3) . . ?
S5 C3 S3 124.8(3) . . ?
O7 C27 H27A 109.7 . . ?
O7 C27 H27B 109.7 . . ?
O7 C27 C28 110.0(4) . . ?
H27A C27 H27B 108.2 . . ?
C28 C27 H27A 109.7 . . ?
C28 C27 H27B 109.7 . . ?
S17 C11 S19 123.5(3) . . ?
C10 C11 S17 121.5(4) . . ?
C10 C11 S19 115.0(4) . . ?
N2 C28 H28A 109.1 . . ?
N2 C28 H28B 109.1 . . ?
C27 C28 N2 112.7(4) . . ?
C27 C28 H28A 109.1 . . ?
C27 C28 H28B 109.1 . . ?
H28A C28 H28B 107.8 . . ?
S8 C6 S9 113.0(3) . . ?
S10 C6 S8 124.6(3) . . ?
S10 C6 S9 122.3(4) . . ?
S16 C10 S18 122.9(3) . . ?
C11 C10 S16 120.7(4) . . ?
C11 C10 S18 116.4(4) . . ?
O6 C17 H17A 109.8 . . ?
O6 C17 H17B 109.8 . . ?
O6 C17 C18 109.2(4) . . ?
H17A C17 H17B 108.3 . . ?
C18 C17 H17A 109.8 . . ?
C18 C17 H17B 109.8 . . ?
O1 C19 H19A 109.7 . . ?
O1 C19 H19B 109.7 . . ?
O1 C19 C20 109.8(5) . . ?
H19A C19 H19B 108.2 . . ?
C20 C19 H19A 109.7 . . ?
C20 C19 H19B 109.7 . . ?
O5 C15 H15A 109.7 . . ?
O5 C15 H15B 109.7 . . ?
O5 C15 C16 109.8(4) . . ?
H15A C15 H15B 108.2 . . ?
C16 C15 H15A 109.7 . . ?
C16 C15 H15B 109.7 . . ?
O3 C23 H23A 109.9 . . ?
O3 C23 H23B 109.9 . . ?
O3 C23 C24 108.8(5) . . ?
H23A C23 H23B 108.3 . . ?
C24 C23 H23A 109.9 . . ?
C24 C23 H23B 109.9 . . ?
O2 C20 C19 109.2(5) . . ?
O2 C20 H20A 109.8 . . ?
O2 C20 H20B 109.8 . . ?
C19 C20 H20A 109.8 . . ?
C19 C20 H20B 109.8 . . ?
H20A C20 H20B 108.3 . . ?
O6 C16 C15 111.4(5) . . ?
O6 C16 H16A 109.3 . . ?
O6 C16 H16B 109.3 . . ?
C15 C16 H16A 109.3 . . ?
C15 C16 H16B 109.3 . . ?
H16A C16 H16B 108.0 . . ?
O1 C18 C17 110.8(5) . . ?
O1 C18 H18A 109.5 . . ?
O1 C18 H18B 109.5 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
O4 C24 C23 110.6(6) . . ?
O4 C24 H24A 109.5 . . ?
O4 C24 H24B 109.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 108.1 . . ?
O4 C13 H13A 109.9 . . ?
O4 C13 H13B 109.9 . . ?
O4 C13 C14 109.0(5) . . ?
H13A C13 H13B 108.3 . . ?
C14 C13 H13A 109.9 . . ?
C14 C13 H13B 109.9 . . ?
O5 C14 C13 110.3(5) . . ?
O5 C14 H14A 109.6 . . ?
O5 C14 H14B 109.6 . . ?
C13 C14 H14A 109.6 . . ?
C13 C14 H14B 109.6 . . ?
H14A C14 H14B 108.1 . . ?
O3 C22 H22A 110.3 . . ?
O3 C22 H22B 110.3 . . ?
O3 C22 C21 107.1(6) . . ?
H22A C22 H22B 108.6 . . ?
C21 C22 H22A 110.3 . . ?
C21 C22 H22B 110.3 . . ?
S19 C12 S18 112.7(3) . . ?
S20 C12 S18 122.7(4) . . ?
S20 C12 S19 124.6(4) . . ?
O2 C21 C22 109.8(5) . . ?
O2 C21 H21A 109.7 . . ?
O2 C21 H21B 109.7 . . ?
C22 C21 H21A 109.7 . . ?
C22 C21 H21B 109.7 . . ?
H21A C21 H21B 108.2 . . ?
C36 O12 C37 112.0(13) . . ?
C37A O12 C36A 113.4(12) . . ?
C33 O10 C32 123.5(7) . . ?
C34 O11 C35 123.7(7) . . ?
C29 O8 C40 120.2(6) . . ?
C39 O13 C38 115.8(12) . . ?
C31 O9 C30 116.4(6) . . ?
O11 C35 H35A 107.7 . . ?
O11 C35 H35B 107.7 . . ?
O11 C35 H35C 108.3 . . ?
O11 C35 H35D 108.3 . . ?
O11 C35 C36 118.3(8) . . ?
H35A C35 H35B 107.1 . . ?
H35C C35 H35D 107.4 . . ?
C36 C35 H35A 107.7 . . ?
C36 C35 H35B 107.7 . . ?
C36A C35 O11 115.9(7) . . ?
C36A C35 H35C 108.3 . . ?
C36A C35 H35D 108.3 . . ?
O8 C40 H40A 107.8 . . ?
O8 C40 H40B 107.8 . . ?
O8 C40 C39 118.1(6) . . ?
H40A C40 H40B 107.1 . . ?
C39 C40 H40A 107.8 . . ?
C39 C40 H40B 107.8 . . ?
O9 C30 H30A 109.4 . . ?
O9 C30 H30B 109.4 . . ?
O9 C30 C29 111.1(6) . . ?
H30A C30 H30B 108.0 . . ?
C29 C30 H30A 109.4 . . ?
C29 C30 H30B 109.4 . . ?
O11 C34 H34A 107.4 . . ?
O11 C34 H34B 107.4 . . ?
O11 C34 C33 119.6(8) . . ?
H34A C34 H34B 107.0 . . ?
C33 C34 H34A 107.4 . . ?
C33 C34 H34B 107.4 . . ?
O8 C29 C30 116.2(7) . . ?
O8 C29 H29A 108.2 . . ?
O8 C29 H29B 108.2 . . ?
C30 C29 H29A 108.2 . . ?
C30 C29 H29B 108.2 . . ?
H29A C29 H29B 107.4 . . ?
O13 C38 H38A 108.8 . . ?
O13 C38 H38B 108.8 . . ?
H38A C38 H38B 107.7 . . ?
C37 C38 O13 113.9(15) . . ?
C37 C38 H38A 108.8 . . ?
C37 C38 H38B 108.8 . . ?
O9 C31 H31A 108.1 . . ?
O9 C31 H31B 108.1 . . ?
O9 C31 C32 116.7(7) . . ?
H31A C31 H31B 107.3 . . ?
C32 C31 H31A 108.1 . . ?
C32 C31 H31B 108.1 . . ?
O13 C39 C40 112.1(8) . . ?
O13 C39 H39A 109.2 . . ?
O13 C39 H39B 109.2 . . ?
C40 C39 H39A 109.2 . . ?
C40 C39 H39B 109.2 . . ?
C40 C39 H39C 108.6 . . ?
C40 C39 H39D 108.6 . . ?
H39A C39 H39B 107.9 . . ?
H39C C39 H39D 107.6 . . ?
O13A C39 C40 114.4(16) . . ?
O13A C39 H39C 108.6 . . ?
O13A C39 H39D 108.6 . . ?
O10 C33 C34 116.2(7) . . ?
O10 C33 H33A 108.2 . . ?
O10 C33 H33B 108.2 . . ?
C34 C33 H33A 108.2 . . ?
C34 C33 H33B 108.2 . . ?
H33A C33 H33B 107.4 . . ?
O10 C32 H32A 109.2 . . ?
O10 C32 H32B 109.2 . . ?
C31 C32 O10 111.9(7) . . ?
C31 C32 H32A 109.2 . . ?
C31 C32 H32B 109.2 . . ?
H32A C32 H32B 107.9 . . ?
O12 C37 H37A 109.1 . . ?
O12 C37 H37B 109.1 . . ?
C38 C37 O12 112.3(14) . . ?
C38 C37 H37A 109.1 . . ?
C38 C37 H37B 109.1 . . ?
H37A C37 H37B 107.9 . . ?
O12 C36 C35 110.9(12) . . ?
O12 C36 H36A 109.5 . . ?
O12 C36 H36B 109.5 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 108.1 . . ?
O12 C37A H37C 110.7 . . ?
O12 C37A H37D 110.7 . . ?
O12 C37A C38A 105(3) . . ?
H37C C37A H37D 108.8 . . ?
C38A C37A H37C 110.7 . . ?
C38A C37A H37D 110.7 . . ?
O12 C36A H36C 109.5 . . ?
O12 C36A H36D 109.5 . . ?
C35 C36A O12 110.6(10) . . ?
C35 C36A H36C 109.5 . . ?
C35 C36A H36D 109.5 . . ?
H36C C36A H36D 108.1 . . ?
C38A O13A C39 119(4) . . ?
C37A C38A H38C 108.7 . . ?
C37A C38A H38D 108.7 . . ?
O13A C38A C37A 114(5) . . ?
O13A C38A H38C 108.7 . . ?
O13A C38A H38D 108.7 . . ?
H38C C38A H38D 107.6 . . ?

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
Ni2 S12 C8 S14 -179.2(2) . . . . ?
Ni2 S12 C8 C7 -0.7(3) . . . . ?
Ni2 S11 C7 S13 179.86(19) . . . . ?
Ni2 S11 C7 C8 1.0(3) . . . . ?
Ni1 S2 C2 S4 -178.93(19) . . . . ?
Ni1 S2 C2 C1 0.8(3) . . . . ?
Ni1 S7 C5 S9 175.2(2) . . . . ?
Ni1 S7 C5 C4 -3.8(4) . . . . ?
Ni1 S1 C1 S3 176.8(2) . . . . ?
Ni1 S1 C1 C2 -3.0(3) . . . . ?
Ni1 S6 C4 S8 -176.9(2) . . . . ?
Ni1 S6 C4 C5 3.2(4) . . . . ?
Ni3 S16 C10 S18 -178.5(2) . . . . ?
Ni3 S16 C10 C11 0.6(4) . . . . ?
Ni3 S17 C11 S19 178.4(3) . . . . ?
Ni3 S17 C11 C10 -1.6(4) . . . . ?
S2 C2 C1 S1 1.6(5) . . . . ?
S2 C2 C1 S3 -178.2(2) . . . . ?
S12 C8 C7 S11 -0.2(5) . . . . ?
S12 C8 C7 S13 -179.2(2) . . . . ?
S7 C5 C4 S6 0.4(5) . . . . ?
S7 C5 C4 S8 -179.5(2) . . . . ?
S4 C2 C1 S1 -178.7(2) . . . . ?
S4 C2 C1 S3 1.5(4) . . . . ?
S14 C8 C7 S11 178.5(2) . . . . ?
S14 C8 C7 S13 -0.5(4) . . . . ?
S9 C5 C4 S6 -178.6(2) . . . . ?
S9 C5 C4 S8 1.5(4) . . . . ?
S17 C11 C10 S16 0.7(6) . . . . ?
S17 C11 C10 S18 179.9(2) . . . . ?
S19 C11 C10 S16 -179.3(2) . . . . ?
S19 C11 C10 S18 -0.1(5) . . . . ?
O7 C27 C28 N2 -68.9(5) . . . . ?
N1 C25 C26 O7 -69.0(4) . . . . ?
O6 C17 C18 O1 -65.4(6) . . . . ?
O1 C19 C20 O2 65.4(6) . . . . ?
O5 C15 C16 O6 59.6(7) . . . . ?
O3 C23 C24 O4 67.6(7) . . . . ?
O3 C22 C21 O2 -61.0(8) . . . . ?
O4 C13 C14 O5 -65.0(6) . . . . ?
C2 S4 C3 S3 1.4(3) . . . . ?
C2 S4 C3 S5 -177.8(3) . . . . ?
C8 S14 C9 S13 2.5(3) . . . . ?
C8 S14 C9 S15 -177.4(3) . . . . ?
C7 S13 C9 S14 -2.7(3) . . . . ?
C7 S13 C9 S15 177.2(3) . . . . ?
C1 S3 C3 S4 -0.8(3) . . . . ?
C1 S3 C3 S5 178.5(3) . . . . ?
C5 S9 C6 S8 -2.1(3) . . . . ?
C5 S9 C6 S10 179.5(3) . . . . ?
C4 S8 C6 S9 2.8(3) . . . . ?
C4 S8 C6 S10 -178.9(3) . . . . ?
C26 O7 C27 C28 -179.4(3) . . . . ?
C9 S14 C8 S12 177.4(2) . . . . ?
C9 S14 C8 C7 -1.2(3) . . . . ?
C9 S13 C7 S11 -177.0(2) . . . . ?
C9 S13 C7 C8 2.0(3) . . . . ?
C3 S4 C2 S2 177.9(2) . . . . ?
C3 S4 C2 C1 -1.8(3) . . . . ?
C3 S3 C1 S1 179.8(2) . . . . ?
C3 S3 C1 C2 -0.4(3) . . . . ?
C27 O7 C26 C25 -177.8(3) . . . . ?
C11 S19 C12 S18 0.5(4) . . . . ?
C11 S19 C12 S20 179.1(4) . . . . ?
C6 S8 C4 S6 177.5(3) . . . . ?
C6 S8 C4 C5 -2.6(4) . . . . ?
C6 S9 C5 S7 -178.6(3) . . . . ?
C6 S9 C5 C4 0.4(4) . . . . ?
C10 S18 C12 S19 -0.5(4) . . . . ?
C10 S18 C12 S20 -179.2(4) . . . . ?
C17 O6 C16 C15 -173.6(5) . . . . ?
C19 O1 C18 C17 -174.2(4) . . . . ?
C15 O5 C14 C13 -172.8(5) . . . . ?
C23 O3 C22 C21 -167.7(5) . . . . ?
C20 O2 C21 C22 173.2(6) . . . . ?
C16 O6 C17 C18 -178.8(5) . . . . ?
C18 O1 C19 C20 175.3(5) . . . . ?
C24 O4 C13 C14 173.2(5) . . . . ?
C13 O4 C24 C23 176.0(5) . . . . ?
C14 O5 C15 C16 176.1(5) . . . . ?
C22 O3 C23 C24 177.7(6) . . . . ?
C12 S18 C10 S16 179.6(3) . . . . ?
C12 S18 C10 C11 0.4(4) . . . . ?
C12 S19 C11 S17 179.8(3) . . . . ?
C12 S19 C11 C10 -0.2(4) . . . . ?
C21 O2 C20 C19 177.0(5) . . . . ?
O12 C37A C38A O13A 75(6) . . . . ?
O11 C35 C36 O12 49.5(19) . . . . ?
O11 C35 C36A O12 -59.9(14) . . . . ?
O11 C34 C33 O10 -19.0(15) . . . . ?
O8 C40 C39 O13 53.5(11) . . . . ?
O8 C40 C39 O13A 25.9(16) . . . . ?
O13 C38 C37 O12 -60(3) . . . . ?
O9 C30 C29 O8 -57.9(9) . . . . ?
O9 C31 C32 O10 57.0(12) . . . . ?
C35 O11 C34 C33 -179.6(9) . . . . ?
C40 O8 C29 C30 -177.1(6) . . . . ?
C40 C39 O13A C38A 148(5) . . . . ?
C30 O9 C31 C32 177.3(8) . . . . ?
C34 O11 C35 C36 153.1(12) . . . . ?
C34 O11 C35 C36A -152.8(11) . . . . ?
C29 O8 C40 C39 173.9(7) . . . . ?
C38 O13 C39 C40 -168.8(12) . . . . ?
C31 O9 C30 C29 178.9(7) . . . . ?
C39 O13 C38 C37 -179(2) . . . . ?
C39 O13A C38A C37A 155(2) . . . . ?
C33 O10 C32 C31 169.4(9) . . . . ?
C32 O10 C33 C34 -177.5(9) . . . . ?
C37 O12 C36 C35 176.8(13) . . . . ?
C36 O12 C37 C38 -178.0(18) . . . . ?
C37A O12 C36A C35 -175.6(13) . . . . ?
C36A O12 C37A C38A -169(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 2.273
_oxdiff_exptl_absorpt_empirical_full_min 0.516
####################################################################### 
# 
# 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_exp_1088_09_253_00_auto
_database_code_depnum_ccdc_archive 'CCDC 2384660'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2024-09-17 deposited with the CCDC.	2024-11-08 downloaded from the CCDC.
;
_audit_creation_date             2023-09-12
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '4(C3 Ni0.5 S5), C4 H14 N2 O, 2(C12 H24 O6)'
_chemical_formula_sum            'C40 H62 N2 Ni2 O13 S20'
_chemical_formula_weight         1537.53
_chemical_melting_point          ?
_chemical_oxdiff_formula         C24H32N2O6NiS10
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                   13.1660(5)
_cell_length_b                   14.5697(6)
_cell_length_c                   18.0721(7)
_cell_angle_alpha                89.590(3)
_cell_angle_beta                 79.483(3)
_cell_angle_gamma                76.032(3)
_cell_volume                     3305.2(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    17510
_cell_measurement_temperature    252.9(3)
_cell_measurement_theta_max      29.4110
_cell_measurement_theta_min      1.6190
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.255
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87535
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.67a (Rigaku Oxford Diffraction, 2022)
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    1.545
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.818
_exptl_crystal_size_mid          0.535
_exptl_crystal_size_min          0.185
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            38905
_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         1.622
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      252.9(3)
_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    -94.00 -69.00   0.50    1.20    --  -20.89 153.00-153.00   50
  2  ω   -112.00 -57.00   0.50    1.20    --  -20.89-153.00 165.00  110
  3  ω    -65.00 -39.00   0.50    1.20    --  -20.89 120.00  48.00   52
  4  ω     42.00 102.00   0.50    1.20    --   21.12-153.00 165.00  120
  5  ω     23.00  76.00   0.50    1.20    --   21.12-120.00 -35.00  106
  6  ω     31.00  56.00   0.50    1.20    --  -20.89  19.00-180.00   50
  7  ω    -22.00  59.00   0.50    1.20    --  -20.89  19.00  30.00  162
  8  ω    -24.00  60.00   0.50    1.20    --  -20.89  19.00 -30.00  168
  9  ω    -17.00  36.00   0.50    1.20    --  -20.89 -99.00 120.00  106
 10  ω    -24.00  10.00   0.50    1.20    --  -20.89  19.00-180.00   68
 11  ω     60.00  86.00   0.50    1.20    --   21.12 178.00-150.00   52
 12  ω    -65.00  28.00   0.50    1.20    --   21.12 -19.00  30.00  186
 13  ω    -74.00  23.00   0.50    1.20    --   21.12 -19.00-180.00  194
;
_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      0.0026018000
_diffrn_orient_matrix_UB_12      0.0018587000
_diffrn_orient_matrix_UB_13      -0.0395148000
_diffrn_orient_matrix_UB_21      0.0211771000
_diffrn_orient_matrix_UB_22      -0.0497083000
_diffrn_orient_matrix_UB_23      -0.0036646000
_diffrn_orient_matrix_UB_31      -0.0523212000
_diffrn_orient_matrix_UB_32      -0.0067884000
_diffrn_orient_matrix_UB_33      0.0045901000
_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                9063
_reflns_number_total             13529
_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 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.068
_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     736
_refine_ls_number_reflns         13529
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0514
_refine_ls_restrained_S_all      1.035
_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)+(0.0590P)²+2.4471P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1276
_refine_ls_wR_factor_ref         0.1458
_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. Uiso/Uaniso restraints and constraints
O8 \\sim C40: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
within 2A
3. Rigid body (RIGU) restrains
 O13A, C38A, C39
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H35C)=Sof(H35D)=Sof(H39C)=Sof(H39D)=Sof(C37A)=Sof(H37C)=Sof(H37D)=
 Sof(C36A)=Sof(H36C)=Sof(H36D)=Sof(O13A)=Sof(C38A)=Sof(H38C)=Sof(H38D)=1-FVAR(1)
 Sof(O13)=Sof(H35A)=Sof(H35B)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H39A)=Sof(H39B)=
 Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C36)=Sof(H36A)=Sof(H36B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C17(H17A,
 H17B), C19(H19A,H19B), C15(H15A,H15B), C23(H23A,H23B), C20(H20A,H20B),
 C16(H16A,H16B), C18(H18A,H18B), C24(H24A,H24B), C13(H13A,H13B), C14(H14A,H14B),
  C22(H22A,H22B), C21(H21A,H21B), C35(H35A,H35B), C35(H35C,H35D), C40(H40A,
 H40B), C30(H30A,H30B), C34(H34A,H34B), C29(H29A,H29B), C38(H38A,H38B),
 C31(H31A,H31B), C39(H39A,H39B), C39(H39C,H39D), C33(H33A,H33B), C32(H32A,H32B),
  C37(H37A,H37B), C36(H36A,H36B), C37A(H37C,H37D), C36A(H36C,H36D), C38A(H38C,
 H38D)
5.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(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
Ni2 Ni 0.500000 0.500000 0.500000 0.05585(18) Uani 1 2 d S . P . .
Ni1 Ni 0.29944(3) 0.92214(3) 0.48580(3) 0.05567(15) Uani 1 1 d . . . . .
Ni3 Ni 0.500000 0.500000 0.000000 0.0686(2) Uani 1 2 d S . P . .
S2 S 0.46961(7) 0.90248(7) 0.46114(6) 0.0613(3) Uani 1 1 d . . . . .
S12 S 0.57891(8) 0.52980(8) 0.39010(6) 0.0658(3) Uani 1 1 d . . . . .
S7 S 0.30509(8) 0.99853(8) 0.58617(6) 0.0651(3) Uani 1 1 d . . . . .
S11 S 0.58727(8) 0.35350(8) 0.49165(6) 0.0666(3) Uani 1 1 d . . . . .
S1 S 0.29871(8) 0.83835(8) 0.38744(7) 0.0661(3) Uani 1 1 d . . . . .
S4 S 0.63783(8) 0.78978(8) 0.33747(7) 0.0663(3) Uani 1 1 d . . . . .
S6 S 0.12865(7) 0.94273(8) 0.51357(7) 0.0708(3) Uani 1 1 d . . . . .
S3 S 0.48263(9) 0.72509(9) 0.27178(7) 0.0766(3) Uani 1 1 d . . . . .
S14 S 0.74788(9) 0.40295(9) 0.27270(7) 0.0760(3) Uani 1 1 d . . . . .
S13 S 0.75463(9) 0.24066(8) 0.36578(8) 0.0766(3) Uani 1 1 d . . . . .
S16 S 0.63548(11) 0.42429(9) -0.08048(7) 0.0806(3) Uani 1 1 d . . . . .
S8 S -0.02976(9) 1.02885(10) 0.65483(9) 0.0918(4) Uani 1 1 d . . . . .
S9 S 0.13473(10) 1.07642(9) 0.72192(8) 0.0877(4) Uani 1 1 d . . . . .
S15 S 0.90369(10) 0.22121(11) 0.21947(9) 0.0983(4) Uani 1 1 d . . . . .
S17 S 0.59369(11) 0.51050(11) 0.08392(7) 0.0882(4) Uani 1 1 d . . . . .
S5 S 0.71387(12) 0.65710(12) 0.20535(9) 0.1040(5) Uani 1 1 d . . . . .
S18 S 0.86970(11) 0.36616(10) -0.07214(7) 0.0890(4) Uani 1 1 d . . . . .
S10 S -0.08517(14) 1.11741(11) 0.80953(12) 0.1288(7) Uani 1 1 d . . . . .
S19 S 0.83233(12) 0.44549(14) 0.07855(8) 0.1076(5) Uani 1 1 d . . . . .
O7 O 0.7617(2) 0.67177(18) 0.80889(15) 0.0615(7) Uani 1 1 d . . . . .
N1 N 0.8820(2) 0.5985(2) 0.65738(17) 0.0542(7) Uani 1 1 d . . . . .
H1A H 0.907898 0.617275 0.611760 0.065 Uiso 1 1 calc R U . . .
H1B H 0.810320 0.614469 0.665323 0.065 Uiso 1 1 calc R U . . .
H1C H 0.905248 0.535327 0.659320 0.065 Uiso 1 1 calc R U . . .
S20 S 1.05270(15) 0.35428(19) 0.00408(11) 0.1484(8) Uani 1 1 d . . . . .
O6 O 0.7198(3) 0.7346(2) 0.59739(19) 0.0866(9) Uani 1 1 d . . . . .
N2 N 0.5792(3) 0.8110(2) 0.89774(19) 0.0644(8) Uani 1 1 d . . . . .
H2A H 0.609300 0.828843 0.852932 0.077 Uiso 1 1 calc R U . . .
H2B H 0.608088 0.830441 0.934397 0.077 Uiso 1 1 calc R U . . .
H2C H 0.508659 0.837110 0.906356 0.077 Uiso 1 1 calc R U . . .
O1 O 0.6703(2) 0.5694(3) 0.65713(18) 0.0823(9) Uani 1 1 d . . . . .
O5 O 0.9321(3) 0.7139(2) 0.52895(18) 0.0882(10) Uani 1 1 d . . . . .
O3 O 1.0268(3) 0.4132(2) 0.6430(2) 0.0988(11) Uani 1 1 d . . . . .
O4 O 1.0936(3) 0.5681(3) 0.5695(2) 0.0993(12) Uani 1 1 d . . . . .
O2 O 0.8208(3) 0.4278(2) 0.71285(18) 0.0888(10) Uani 1 1 d . . . . .
C2 C 0.5058(3) 0.8305(2) 0.3826(2) 0.0543(9) Uani 1 1 d . . . . .
C8 C 0.6622(3) 0.4214(3) 0.3600(2) 0.0609(10) Uani 1 1 d . . . . .
C7 C 0.6652(3) 0.3449(3) 0.4040(2) 0.0614(10) Uani 1 1 d . . . . .
C1 C 0.4326(3) 0.8008(3) 0.3502(2) 0.0594(10) Uani 1 1 d . . . . .
C25 C 0.9189(3) 0.6452(3) 0.7160(2) 0.0689(11) Uani 1 1 d . . . . .
H25A H 0.901001 0.713739 0.709499 0.083 Uiso 1 1 calc R U . . .
H25B H 0.996571 0.623670 0.709306 0.083 Uiso 1 1 calc R U . . .
C5 C 0.1744(3) 1.0226(3) 0.6327(3) 0.0677(11) Uani 1 1 d . . . . .
C4 C 0.0986(3) 0.9983(3) 0.6003(3) 0.0692(12) Uani 1 1 d . . . . .
C26 C 0.8709(3) 0.6256(3) 0.7942(2) 0.0684(11) Uani 1 1 d . . . . .
H26A H 0.879791 0.557310 0.799424 0.082 Uiso 1 1 calc R U . . .
H26B H 0.906988 0.648522 0.830475 0.082 Uiso 1 1 calc R U . . .
C9 C 0.8078(3) 0.2841(3) 0.2824(3) 0.0750(12) Uani 1 1 d . . . . .
C3 C 0.6180(3) 0.7198(3) 0.2668(3) 0.0726(12) Uani 1 1 d . . . . .
C27 C 0.7136(4) 0.6578(3) 0.8834(3) 0.0744(12) Uani 1 1 d . . . . .
H27A H 0.748579 0.683112 0.919194 0.089 Uiso 1 1 calc R U . . .
H27B H 0.722302 0.589923 0.891202 0.089 Uiso 1 1 calc R U . . .
C11 C 0.7197(4) 0.4568(3) 0.0383(2) 0.0747(12) Uani 1 1 d . . . . .
C28 C 0.5985(4) 0.7062(3) 0.8970(3) 0.0769(12) Uani 1 1 d . . . . .
H28A H 0.563962 0.687324 0.945439 0.092 Uiso 1 1 calc R U . . .
H28B H 0.565837 0.685560 0.857575 0.092 Uiso 1 1 calc R U . . .
C6 C 0.0013(4) 1.0749(3) 0.7327(3) 0.0931(17) Uani 1 1 d . . . . .
C10 C 0.7382(4) 0.4187(3) -0.0331(2) 0.0712(11) Uani 1 1 d . . . . .
C17 C 0.6218(4) 0.7091(4) 0.5959(4) 0.107(2) Uani 1 1 d . . . . .
H17A H 0.628464 0.671699 0.549628 0.129 Uiso 1 1 calc R U . . .
H17B H 0.564456 0.766340 0.596365 0.129 Uiso 1 1 calc R U . . .
C19 C 0.6437(4) 0.5089(5) 0.7166(3) 0.0979(18) Uani 1 1 d . . . . .
H19A H 0.571969 0.500518 0.717154 0.117 Uiso 1 1 calc R U . . .
H19B H 0.644253 0.538134 0.765190 0.117 Uiso 1 1 calc R U . . .
C15 C 0.8550(6) 0.8027(4) 0.5369(3) 0.112(2) Uani 1 1 d . . . . .
H15A H 0.873174 0.842373 0.494911 0.135 Uiso 1 1 calc R U . . .
H15B H 0.855744 0.835631 0.583838 0.135 Uiso 1 1 calc R U . . .
C23 C 1.1365(5) 0.4218(5) 0.6249(5) 0.132(3) Uani 1 1 d . . . . .
H23A H 1.185288 0.358753 0.616693 0.158 Uiso 1 1 calc R U . . .
H23B H 1.153193 0.453950 0.666959 0.158 Uiso 1 1 calc R U . . .
C20 C 0.7212(6) 0.4163(5) 0.7056(3) 0.111(2) Uani 1 1 d . . . . .
H20A H 0.698652 0.372837 0.743178 0.133 Uiso 1 1 calc R U . . .
H20B H 0.724806 0.389121 0.655454 0.133 Uiso 1 1 calc R U . . .
C16 C 0.7476(5) 0.7879(4) 0.5378(4) 0.1069(19) Uani 1 1 d . . . . .
H16A H 0.695675 0.849268 0.541787 0.128 Uiso 1 1 calc R U . . .
H16B H 0.746818 0.755608 0.490619 0.128 Uiso 1 1 calc R U . . .
C18 C 0.5961(4) 0.6539(5) 0.6614(4) 0.1045(18) Uani 1 1 d . . . . .
H18A H 0.594766 0.689482 0.707498 0.125 Uiso 1 1 calc R U . . .
H18B H 0.525306 0.642478 0.663323 0.125 Uiso 1 1 calc R U . . .
C24 C 1.1505(4) 0.4767(6) 0.5560(4) 0.129(3) Uani 1 1 d . . . . .
H24A H 1.226113 0.474987 0.539479 0.155 Uiso 1 1 calc R U . . .
H24B H 1.126535 0.448113 0.515490 0.155 Uiso 1 1 calc R U . . .
C13 C 1.1097(4) 0.6276(6) 0.5056(3) 0.117(2) Uani 1 1 d . . . . .
H13A H 1.097364 0.598214 0.460479 0.140 Uiso 1 1 calc R U . . .
H13B H 1.183232 0.634147 0.496028 0.140 Uiso 1 1 calc R U . . .
C14 C 1.0358(6) 0.7213(5) 0.5213(3) 0.118(2) Uani 1 1 d . . . . .
H14A H 1.045873 0.749289 0.567770 0.142 Uiso 1 1 calc R U . . .
H14B H 1.050934 0.762913 0.480083 0.142 Uiso 1 1 calc R U . . .
C22 C 1.0062(7) 0.3593(5) 0.7060(4) 0.143(3) Uani 1 1 d . . . . .
H22A H 1.004983 0.394466 0.752332 0.172 Uiso 1 1 calc R U . . .
H22B H 1.061411 0.299955 0.702684 0.172 Uiso 1 1 calc R U . . .
C12 C 0.9256(4) 0.3868(4) 0.0041(3) 0.0964(16) Uani 1 1 d . . . . .
C21 C 0.9022(7) 0.3398(4) 0.7063(4) 0.130(3) Uani 1 1 d . . . . .
H21A H 0.904086 0.305209 0.659541 0.156 Uiso 1 1 calc R U . . .
H21B H 0.885336 0.300260 0.748622 0.156 Uiso 1 1 calc R U . . .
O12 O 0.5764(4) 0.8594(3) 1.0533(2) 0.0959(10) Uani 1 1 d . . . . .
O10 O 0.3630(4) 0.8549(3) 0.8662(3) 0.1308(16) Uani 1 1 d . . . . .
O11 O 0.3894(4) 0.8349(4) 1.0106(3) 0.1314(16) Uani 1 1 d . . . . .
O8 O 0.7140(4) 0.9216(3) 0.8075(3) 0.1139(13) Uani 1 1 d . U . . .
O13 O 0.7560(10) 0.8635(8) 0.9496(6) 0.085(3) Uani 0.557(14) 1 d . . P A 1
O9 O 0.5322(4) 0.8952(3) 0.7589(2) 0.1267(15) Uani 1 1 d . . . . .
C35 C 0.4048(6) 0.8393(5) 1.0841(4) 0.118(2) Uani 1 1 d . . . . .
H35A H 0.365651 0.797460 1.113209 0.141 Uiso 0.557(14) 1 calc R U P A 1
H35B H 0.371070 0.903902 1.104255 0.141 Uiso 0.557(14) 1 calc R U P A 1
H35C H 0.335407 0.864660 1.116658 0.141 Uiso 0.443(14) 1 calc R U P A 2
H35D H 0.432353 0.774700 1.099346 0.141 Uiso 0.443(14) 1 calc R U P A 2
C40 C 0.8144(5) 0.8977(4) 0.8262(4) 0.112(2) Uani 1 1 d . U . . .
H40A H 0.846809 0.831229 0.810493 0.135 Uiso 1 1 calc R U . . .
H40B H 0.857879 0.935619 0.796323 0.135 Uiso 1 1 calc R U . . .
C30 C 0.5977(7) 0.9516(5) 0.7212(4) 0.133(3) Uani 1 1 d . . . . .
H30A H 0.568313 1.017837 0.738721 0.160 Uiso 1 1 calc R U . . .
H30B H 0.598708 0.947784 0.666940 0.160 Uiso 1 1 calc R U . . .
C34 C 0.3044(7) 0.8204(6) 0.9924(6) 0.148(3) Uani 1 1 d . . . . .
H34A H 0.244269 0.870075 1.018174 0.178 Uiso 1 1 calc R U . . .
H34B H 0.294910 0.760209 1.013377 0.178 Uiso 1 1 calc R U . . .
C29 C 0.7042(8) 0.9203(6) 0.7351(5) 0.145(3) Uani 1 1 d . . . . .
H29A H 0.733938 0.855439 0.714248 0.174 Uiso 1 1 calc R U . . .
H29B H 0.747390 0.960226 0.707683 0.174 Uiso 1 1 calc R U . . .
C38 C 0.7446(18) 0.8861(15) 1.0280(10) 0.100(7) Uani 0.557(14) 1 d . . P A 1
H38A H 0.815212 0.873095 1.041841 0.119 Uiso 0.557(14) 1 calc R U P A 1
H38B H 0.711275 0.953683 1.037970 0.119 Uiso 0.557(14) 1 calc R U P A 1
C31 C 0.4294(7) 0.9185(6) 0.7516(5) 0.154(3) Uani 1 1 d . . . . .
H31A H 0.427132 0.918178 0.697682 0.185 Uiso 1 1 calc R U . . .
H31B H 0.398437 0.983721 0.771369 0.185 Uiso 1 1 calc R U . . .
C39 C 0.8215(6) 0.9088(5) 0.9008(5) 0.136(3) Uani 1 1 d . . . . .
H39A H 0.801849 0.976473 0.914849 0.163 Uiso 0.557(14) 1 calc R U P A 1
H39B H 0.895476 0.883470 0.906631 0.163 Uiso 0.557(14) 1 calc R U P A 1
H39C H 0.879947 0.858861 0.913025 0.163 Uiso 0.443(14) 1 calc R U P A 2
H39D H 0.837121 0.969963 0.908942 0.163 Uiso 0.443(14) 1 calc R U P A 2
C33 C 0.2954(7) 0.8174(7) 0.9137(7) 0.176(4) Uani 1 1 d . . . . .
H33A H 0.305799 0.751086 0.897649 0.211 Uiso 1 1 calc R U . . .
H33B H 0.222621 0.850475 0.909331 0.211 Uiso 1 1 calc R U . . .
C32 C 0.3628(7) 0.8615(7) 0.7869(6) 0.169(4) Uani 1 1 d . . . . .
H32A H 0.387003 0.797786 0.763081 0.202 Uiso 1 1 calc R U . . .
H32B H 0.289847 0.888102 0.779289 0.202 Uiso 1 1 calc R U . . .
C37 C 0.6850(16) 0.8353(13) 1.0705(7) 0.133(6) Uani 0.557(14) 1 d . . P A 1
H37A H 0.681736 0.849229 1.123989 0.159 Uiso 0.557(14) 1 calc R U P A 1
H37B H 0.717109 0.767586 1.060073 0.159 Uiso 0.557(14) 1 calc R U P A 1
C36 C 0.5128(13) 0.8150(12) 1.0994(7) 0.143(7) Uani 0.557(14) 1 d . . P A 1
H36A H 0.511179 0.832888 1.151828 0.171 Uiso 0.557(14) 1 calc R U P A 1
H36B H 0.541858 0.746401 1.092555 0.171 Uiso 0.557(14) 1 calc R U P A 1
C37A C 0.6520(16) 0.9076(12) 1.0682(12) 0.116(7) Uani 0.443(14) 1 d . . P A 2
H37C H 0.670042 0.891680 1.117701 0.139 Uiso 0.443(14) 1 calc R U P A 2
H37D H 0.622879 0.976162 1.067914 0.139 Uiso 0.443(14) 1 calc R U P A 2
C36A C 0.4728(13) 0.8931(10) 1.0966(7) 0.091(5) Uani 0.443(14) 1 d . . P A 2
H36C H 0.477121 0.892796 1.150178 0.110 Uiso 0.443(14) 1 calc R U P A 2
H36D H 0.444042 0.958674 1.084061 0.110 Uiso 0.443(14) 1 calc R U P A 2
O13A O 0.7387(16) 0.9051(15) 0.9420(16) 0.163(10) Uani 0.443(14) 1 d . . P A 2
C38A C 0.749(4) 0.877(4) 1.008(3) 0.23(2) Uani 0.443(14) 1 d . . P A 2
H38C H 0.806863 0.901148 1.022231 0.271 Uiso 0.443(14) 1 calc R U P A 2
H38D H 0.772011 0.808149 1.005394 0.271 Uiso 0.443(14) 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
Ni2 S12 2.1598(10) 2_666 ?
Ni2 S12 2.1598(10) . ?
Ni2 S11 2.1578(11) 2_666 ?
Ni2 S11 2.1578(11) . ?
Ni1 S2 2.1512(10) . ?
Ni1 S7 2.1570(13) . ?
Ni1 S1 2.1663(13) . ?
Ni1 S6 2.1594(10) . ?
Ni3 S16 2.1540(13) . ?
Ni3 S16 2.1541(13) 2_665 ?
Ni3 S17 2.1501(12) . ?
Ni3 S17 2.1501(12) 2_665 ?
S2 C2 1.696(4) . ?
S12 C8 1.718(4) . ?
S7 C5 1.726(4) . ?
S11 C7 1.710(4) . ?
S1 C1 1.722(4) . ?
S4 C2 1.741(4) . ?
S4 C3 1.735(5) . ?
S6 C4 1.705(5) . ?
S3 C1 1.729(4) . ?
S3 C3 1.750(4) . ?
S14 C8 1.745(4) . ?
S14 C9 1.743(5) . ?
S13 C7 1.740(4) . ?
S13 C9 1.726(5) . ?
S16 C10 1.713(5) . ?
S8 C4 1.750(4) . ?
S8 C6 1.720(7) . ?
S9 C5 1.732(5) . ?
S9 C6 1.737(5) . ?
S15 C9 1.630(5) . ?
S17 C11 1.711(5) . ?
S5 C3 1.615(5) . ?
S18 C10 1.734(5) . ?
S18 C12 1.735(5) . ?
S10 C6 1.643(6) . ?
S19 C11 1.741(5) . ?
S19 C12 1.719(6) . ?
O7 C26 1.409(5) . ?
O7 C27 1.415(5) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N1 H1C 0.9000 . ?
N1 C25 1.476(5) . ?
S20 C12 1.626(6) . ?
O6 C17 1.431(6) . ?
O6 C16 1.370(6) . ?
N2 H2A 0.9000 . ?
N2 H2B 0.9000 . ?
N2 H2C 0.9000 . ?
N2 C28 1.486(5) . ?
O1 C19 1.432(6) . ?
O1 C18 1.368(7) . ?
O5 C15 1.429(7) . ?
O5 C14 1.378(7) . ?
O3 C23 1.458(7) . ?
O3 C22 1.402(8) . ?
O4 C24 1.359(8) . ?
O4 C13 1.456(7) . ?
O2 C20 1.391(7) . ?
O2 C21 1.448(7) . ?
C2 C1 1.367(5) . ?
C8 C7 1.361(5) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 C26 1.494(6) . ?
C5 C4 1.360(6) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 C28 1.485(6) . ?
C11 C10 1.364(6) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 C18 1.460(8) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 C20 1.472(8) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 C16 1.479(8) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 C24 1.483(10) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 C14 1.467(9) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 C21 1.463(10) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
O12 C37 1.476(17) . ?
O12 C36 1.347(14) . ?
O12 C37A 1.411(16) . ?
O12 C36A 1.417(15) . ?
O10 C33 1.333(10) . ?
O10 C32 1.436(10) . ?
O11 C35 1.385(8) . ?
O11 C34 1.286(9) . ?
O8 C40 1.386(7) . ?
O8 C29 1.339(8) . ?
O13 C38 1.43(2) . ?
O13 C39 1.393(13) . ?
O9 C30 1.415(8) . ?
O9 C31 1.344(8) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C35 H35D 0.9800 . ?
C35 C36 1.457(16) . ?
C35 C36A 1.373(15) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 C39 1.381(9) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 C29 1.435(10) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 C33 1.451(11) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 C37 1.34(3) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 C32 1.416(11) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C39 H39D 0.9800 . ?
C39 O13A 1.21(2) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C37A H37C 0.9800 . ?
C37A H37D 0.9800 . ?
C37A C38A 1.50(5) . ?
C36A H36C 0.9800 . ?
C36A H36D 0.9800 . ?
O13A C38A 1.27(6) . ?
C38A H38C 0.9800 . ?
C38A H38D 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
S12 Ni2 S12 180.0 . 2_666 ?
S11 Ni2 S12 86.76(4) . 2_666 ?
S11 Ni2 S12 93.24(4) . . ?
S11 Ni2 S12 86.76(4) 2_666 . ?
S11 Ni2 S12 93.24(4) 2_666 2_666 ?
S11 Ni2 S11 180.0 . 2_666 ?
S2 Ni1 S7 85.49(4) . . ?
S2 Ni1 S1 93.17(4) . . ?
S2 Ni1 S6 178.51(5) . . ?
S7 Ni1 S1 176.81(5) . . ?
S7 Ni1 S6 93.09(5) . . ?
S6 Ni1 S1 88.21(5) . . ?
S16 Ni3 S16 180.0 . 2_665 ?
S17 Ni3 S16 93.52(5) 2_665 2_665 ?
S17 Ni3 S16 93.52(5) . . ?
S17 Ni3 S16 86.48(5) . 2_665 ?
S17 Ni3 S16 86.48(5) 2_665 . ?
S17 Ni3 S17 180.0 . 2_665 ?
C2 S2 Ni1 102.46(12) . . ?
C8 S12 Ni2 102.01(14) . . ?
C5 S7 Ni1 102.18(17) . . ?
C7 S11 Ni2 102.28(14) . . ?
C1 S1 Ni1 101.92(14) . . ?
C3 S4 C2 98.5(2) . . ?
C4 S6 Ni1 102.18(14) . . ?
C1 S3 C3 98.2(2) . . ?
C9 S14 C8 97.3(2) . . ?
C9 S13 C7 98.2(2) . . ?
C10 S16 Ni3 102.11(17) . . ?
C6 S8 C4 97.9(2) . . ?
C5 S9 C6 96.7(3) . . ?
C11 S17 Ni3 102.04(16) . . ?
C10 S18 C12 97.5(2) . . ?
C12 S19 C11 98.1(2) . . ?
C26 O7 C27 111.2(3) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C25 N1 H1A 109.5 . . ?
C25 N1 H1B 109.5 . . ?
C25 N1 H1C 109.5 . . ?
C16 O6 C17 112.6(4) . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C28 N2 H2A 109.5 . . ?
C28 N2 H2B 109.5 . . ?
C28 N2 H2C 109.5 . . ?
C18 O1 C19 112.4(5) . . ?
C14 O5 C15 114.1(5) . . ?
C22 O3 C23 113.8(5) . . ?
C24 O4 C13 113.3(5) . . ?
C20 O2 C21 113.7(5) . . ?
S2 C2 S4 122.6(2) . . ?
C1 C2 S2 122.0(3) . . ?
C1 C2 S4 115.4(3) . . ?
S12 C8 S14 122.5(2) . . ?
C7 C8 S12 121.2(3) . . ?
C7 C8 S14 116.3(3) . . ?
S11 C7 S13 123.2(2) . . ?
C8 C7 S11 121.2(3) . . ?
C8 C7 S13 115.6(3) . . ?
S1 C1 S3 123.3(2) . . ?
C2 C1 S1 120.4(3) . . ?
C2 C1 S3 116.3(3) . . ?
N1 C25 H25A 109.0 . . ?
N1 C25 H25B 109.0 . . ?
N1 C25 C26 113.1(3) . . ?
H25A C25 H25B 107.8 . . ?
C26 C25 H25A 109.0 . . ?
C26 C25 H25B 109.0 . . ?
S7 C5 S9 122.0(3) . . ?
C4 C5 S7 120.4(4) . . ?
C4 C5 S9 117.6(3) . . ?
S6 C4 S8 123.7(3) . . ?
C5 C4 S6 121.8(3) . . ?
C5 C4 S8 114.4(4) . . ?
O7 C26 C25 109.2(3) . . ?
O7 C26 H26A 109.8 . . ?
O7 C26 H26B 109.8 . . ?
C25 C26 H26A 109.8 . . ?
C25 C26 H26B 109.8 . . ?
H26A C26 H26B 108.3 . . ?
S13 C9 S14 112.6(3) . . ?
S15 C9 S14 123.6(3) . . ?
S15 C9 S13 123.8(3) . . ?
S4 C3 S3 111.6(3) . . ?
S5 C3 S4 123.4(3) . . ?
S5 C3 S3 125.1(3) . . ?
O7 C27 H27A 109.7 . . ?
O7 C27 H27B 109.7 . . ?
O7 C27 C28 110.0(4) . . ?
H27A C27 H27B 108.2 . . ?
C28 C27 H27A 109.7 . . ?
C28 C27 H27B 109.7 . . ?
S17 C11 S19 123.3(3) . . ?
C10 C11 S17 121.4(4) . . ?
C10 C11 S19 115.3(4) . . ?
N2 C28 H28A 109.1 . . ?
N2 C28 H28B 109.1 . . ?
C27 C28 N2 112.7(3) . . ?
C27 C28 H28A 109.1 . . ?
C27 C28 H28B 109.1 . . ?
H28A C28 H28B 107.8 . . ?
S8 C6 S9 113.3(3) . . ?
S10 C6 S8 124.6(3) . . ?
S10 C6 S9 122.1(4) . . ?
S16 C10 S18 122.8(3) . . ?
C11 C10 S16 120.9(4) . . ?
C11 C10 S18 116.3(4) . . ?
O6 C17 H17A 109.7 . . ?
O6 C17 H17B 109.7 . . ?
O6 C17 C18 109.7(4) . . ?
H17A C17 H17B 108.2 . . ?
C18 C17 H17A 109.7 . . ?
C18 C17 H17B 109.7 . . ?
O1 C19 H19A 109.7 . . ?
O1 C19 H19B 109.7 . . ?
O1 C19 C20 110.0(4) . . ?
H19A C19 H19B 108.2 . . ?
C20 C19 H19A 109.7 . . ?
C20 C19 H19B 109.7 . . ?
O5 C15 H15A 109.6 . . ?
O5 C15 H15B 109.6 . . ?
O5 C15 C16 110.1(4) . . ?
H15A C15 H15B 108.1 . . ?
C16 C15 H15A 109.6 . . ?
C16 C15 H15B 109.6 . . ?
O3 C23 H23A 109.8 . . ?
O3 C23 H23B 109.8 . . ?
O3 C23 C24 109.3(4) . . ?
H23A C23 H23B 108.3 . . ?
C24 C23 H23A 109.8 . . ?
C24 C23 H23B 109.8 . . ?
O2 C20 C19 109.2(4) . . ?
O2 C20 H20A 109.8 . . ?
O2 C20 H20B 109.8 . . ?
C19 C20 H20A 109.8 . . ?
C19 C20 H20B 109.8 . . ?
H20A C20 H20B 108.3 . . ?
O6 C16 C15 110.4(5) . . ?
O6 C16 H16A 109.6 . . ?
O6 C16 H16B 109.6 . . ?
C15 C16 H16A 109.6 . . ?
C15 C16 H16B 109.6 . . ?
H16A C16 H16B 108.1 . . ?
O1 C18 C17 110.1(5) . . ?
O1 C18 H18A 109.6 . . ?
O1 C18 H18B 109.6 . . ?
C17 C18 H18A 109.6 . . ?
C17 C18 H18B 109.6 . . ?
H18A C18 H18B 108.2 . . ?
O4 C24 C23 110.4(5) . . ?
O4 C24 H24A 109.6 . . ?
O4 C24 H24B 109.6 . . ?
C23 C24 H24A 109.6 . . ?
C23 C24 H24B 109.6 . . ?
H24A C24 H24B 108.1 . . ?
O4 C13 H13A 109.7 . . ?
O4 C13 H13B 109.7 . . ?
O4 C13 C14 109.8(5) . . ?
H13A C13 H13B 108.2 . . ?
C14 C13 H13A 109.7 . . ?
C14 C13 H13B 109.7 . . ?
O5 C14 C13 110.3(5) . . ?
O5 C14 H14A 109.6 . . ?
O5 C14 H14B 109.6 . . ?
C13 C14 H14A 109.6 . . ?
C13 C14 H14B 109.6 . . ?
H14A C14 H14B 108.1 . . ?
O3 C22 H22A 110.4 . . ?
O3 C22 H22B 110.4 . . ?
O3 C22 C21 106.7(5) . . ?
H22A C22 H22B 108.6 . . ?
C21 C22 H22A 110.4 . . ?
C21 C22 H22B 110.4 . . ?
S19 C12 S18 112.8(3) . . ?
S20 C12 S18 123.1(3) . . ?
S20 C12 S19 124.1(3) . . ?
O2 C21 C22 110.0(5) . . ?
O2 C21 H21A 109.7 . . ?
O2 C21 H21B 109.7 . . ?
C22 C21 H21A 109.7 . . ?
C22 C21 H21B 109.7 . . ?
H21A C21 H21B 108.2 . . ?
C36 O12 C37 110.5(10) . . ?
C37A O12 C36A 114.7(11) . . ?
C33 O10 C32 123.7(7) . . ?
C34 O11 C35 123.7(6) . . ?
C29 O8 C40 119.8(6) . . ?
C39 O13 C38 115.8(11) . . ?
C31 O9 C30 116.6(6) . . ?
O11 C35 H35A 107.5 . . ?
O11 C35 H35B 107.5 . . ?
O11 C35 H35C 108.4 . . ?
O11 C35 H35D 108.4 . . ?
O11 C35 C36 119.3(7) . . ?
H35A C35 H35B 107.0 . . ?
H35C C35 H35D 107.5 . . ?
C36 C35 H35A 107.5 . . ?
C36 C35 H35B 107.5 . . ?
C36A C35 O11 115.4(7) . . ?
C36A C35 H35C 108.4 . . ?
C36A C35 H35D 108.4 . . ?
O8 C40 H40A 107.9 . . ?
O8 C40 H40B 107.9 . . ?
H40A C40 H40B 107.2 . . ?
C39 C40 O8 117.8(6) . . ?
C39 C40 H40A 107.9 . . ?
C39 C40 H40B 107.9 . . ?
O9 C30 H30A 109.5 . . ?
O9 C30 H30B 109.5 . . ?
O9 C30 C29 110.6(5) . . ?
H30A C30 H30B 108.1 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
O11 C34 H34A 107.4 . . ?
O11 C34 H34B 107.4 . . ?
O11 C34 C33 119.8(7) . . ?
H34A C34 H34B 106.9 . . ?
C33 C34 H34A 107.4 . . ?
C33 C34 H34B 107.4 . . ?
O8 C29 C30 115.6(7) . . ?
O8 C29 H29A 108.4 . . ?
O8 C29 H29B 108.4 . . ?
C30 C29 H29A 108.4 . . ?
C30 C29 H29B 108.4 . . ?
H29A C29 H29B 107.4 . . ?
O13 C38 H38A 109.4 . . ?
O13 C38 H38B 109.4 . . ?
H38A C38 H38B 108.0 . . ?
C37 C38 O13 111.3(13) . . ?
C37 C38 H38A 109.4 . . ?
C37 C38 H38B 109.4 . . ?
O9 C31 H31A 107.9 . . ?
O9 C31 H31B 107.9 . . ?
O9 C31 C32 117.7(7) . . ?
H31A C31 H31B 107.2 . . ?
C32 C31 H31A 107.9 . . ?
C32 C31 H31B 107.9 . . ?
O13 C39 H39A 109.0 . . ?
O13 C39 H39B 109.0 . . ?
C40 C39 O13 113.0(7) . . ?
C40 C39 H39A 109.0 . . ?
C40 C39 H39B 109.0 . . ?
C40 C39 H39C 109.5 . . ?
C40 C39 H39D 109.5 . . ?
H39A C39 H39B 107.8 . . ?
H39C C39 H39D 108.1 . . ?
O13A C39 C40 110.8(15) . . ?
O13A C39 H39C 109.5 . . ?
O13A C39 H39D 109.5 . . ?
O10 C33 C34 116.0(6) . . ?
O10 C33 H33A 108.3 . . ?
O10 C33 H33B 108.3 . . ?
C34 C33 H33A 108.3 . . ?
C34 C33 H33B 108.3 . . ?
H33A C33 H33B 107.4 . . ?
O10 C32 H32A 109.1 . . ?
O10 C32 H32B 109.1 . . ?
C31 C32 O10 112.4(7) . . ?
C31 C32 H32A 109.1 . . ?
C31 C32 H32B 109.1 . . ?
H32A C32 H32B 107.9 . . ?
O12 C37 H37A 109.8 . . ?
O12 C37 H37B 109.8 . . ?
C38 C37 O12 109.5(12) . . ?
C38 C37 H37A 109.8 . . ?
C38 C37 H37B 109.8 . . ?
H37A C37 H37B 108.2 . . ?
O12 C36 C35 111.3(10) . . ?
O12 C36 H36A 109.4 . . ?
O12 C36 H36B 109.4 . . ?
C35 C36 H36A 109.4 . . ?
C35 C36 H36B 109.4 . . ?
H36A C36 H36B 108.0 . . ?
O12 C37A H37C 110.2 . . ?
O12 C37A H37D 110.2 . . ?
O12 C37A C38A 108(2) . . ?
H37C C37A H37D 108.5 . . ?
C38A C37A H37C 110.2 . . ?
C38A C37A H37D 110.2 . . ?
O12 C36A H36C 109.2 . . ?
O12 C36A H36D 109.2 . . ?
C35 C36A O12 112.2(10) . . ?
C35 C36A H36C 109.2 . . ?
C35 C36A H36D 109.2 . . ?
H36C C36A H36D 107.9 . . ?
C39 O13A C38A 114(3) . . ?
C37A C38A H38C 108.3 . . ?
C37A C38A H38D 108.3 . . ?
O13A C38A C37A 116(4) . . ?
O13A C38A H38C 108.3 . . ?
O13A C38A H38D 108.3 . . ?
H38C C38A H38D 107.4 . . ?

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
Ni2 S12 C8 S14 -179.70(19) . . . . ?
Ni2 S12 C8 C7 -0.2(3) . . . . ?
Ni2 S11 C7 S13 179.83(19) . . . . ?
Ni2 S11 C7 C8 1.3(3) . . . . ?
Ni1 S2 C2 S4 -179.33(19) . . . . ?
Ni1 S2 C2 C1 0.9(3) . . . . ?
Ni1 S7 C5 S9 175.1(2) . . . . ?
Ni1 S7 C5 C4 -4.0(4) . . . . ?
Ni1 S1 C1 S3 176.8(2) . . . . ?
Ni1 S1 C1 C2 -3.0(3) . . . . ?
Ni1 S6 C4 S8 -176.8(2) . . . . ?
Ni1 S6 C4 C5 3.2(4) . . . . ?
Ni3 S16 C10 S18 -178.8(2) . . . . ?
Ni3 S16 C10 C11 0.8(4) . . . . ?
Ni3 S17 C11 S19 178.9(3) . . . . ?
Ni3 S17 C11 C10 -1.7(4) . . . . ?
S2 C2 C1 S1 1.5(5) . . . . ?
S2 C2 C1 S3 -178.3(2) . . . . ?
S12 C8 C7 S11 -0.8(5) . . . . ?
S12 C8 C7 S13 -179.4(2) . . . . ?
S7 C5 C4 S6 0.6(5) . . . . ?
S7 C5 C4 S8 -179.5(2) . . . . ?
S4 C2 C1 S1 -178.2(2) . . . . ?
S4 C2 C1 S3 1.9(4) . . . . ?
S14 C8 C7 S11 178.8(2) . . . . ?
S14 C8 C7 S13 0.1(4) . . . . ?
S9 C5 C4 S6 -178.5(2) . . . . ?
S9 C5 C4 S8 1.4(4) . . . . ?
S17 C11 C10 S16 0.7(6) . . . . ?
S17 C11 C10 S18 -179.7(2) . . . . ?
S19 C11 C10 S16 -179.9(2) . . . . ?
S19 C11 C10 S18 -0.3(5) . . . . ?
O7 C27 C28 N2 -68.1(5) . . . . ?
N1 C25 C26 O7 -69.5(4) . . . . ?
O6 C17 C18 O1 -65.5(6) . . . . ?
O1 C19 C20 O2 65.5(5) . . . . ?
O5 C15 C16 O6 60.9(6) . . . . ?
O3 C23 C24 O4 67.3(6) . . . . ?
O3 C22 C21 O2 -61.2(7) . . . . ?
O4 C13 C14 O5 -64.1(6) . . . . ?
C2 S4 C3 S3 1.6(3) . . . . ?
C2 S4 C3 S5 -177.7(3) . . . . ?
C8 S14 C9 S13 2.6(3) . . . . ?
C8 S14 C9 S15 -177.2(3) . . . . ?
C7 S13 C9 S14 -2.6(3) . . . . ?
C7 S13 C9 S15 177.2(3) . . . . ?
C1 S3 C3 S4 -0.8(3) . . . . ?
C1 S3 C3 S5 178.5(3) . . . . ?
C5 S9 C6 S8 -2.3(3) . . . . ?
C5 S9 C6 S10 179.7(3) . . . . ?
C4 S8 C6 S9 2.9(3) . . . . ?
C4 S8 C6 S10 -179.2(3) . . . . ?
C26 O7 C27 C28 -179.3(3) . . . . ?
C9 S14 C8 S12 177.8(2) . . . . ?
C9 S14 C8 C7 -1.7(3) . . . . ?
C9 S13 C7 S11 -177.1(2) . . . . ?
C9 S13 C7 C8 1.6(3) . . . . ?
C3 S4 C2 S2 178.1(2) . . . . ?
C3 S4 C2 C1 -2.2(3) . . . . ?
C3 S3 C1 S1 179.5(3) . . . . ?
C3 S3 C1 C2 -0.7(3) . . . . ?
C27 O7 C26 C25 -178.0(3) . . . . ?
C11 S19 C12 S18 -0.3(4) . . . . ?
C11 S19 C12 S20 179.4(4) . . . . ?
C6 S8 C4 S6 177.3(3) . . . . ?
C6 S8 C4 C5 -2.6(4) . . . . ?
C6 S9 C5 S7 -178.5(3) . . . . ?
C6 S9 C5 C4 0.5(4) . . . . ?
C10 S18 C12 S19 0.1(4) . . . . ?
C10 S18 C12 S20 -179.6(4) . . . . ?
C17 O6 C16 C15 -173.3(5) . . . . ?
C19 O1 C18 C17 -174.9(4) . . . . ?
C15 O5 C14 C13 -174.0(5) . . . . ?
C23 O3 C22 C21 -167.6(5) . . . . ?
C20 O2 C21 C22 173.7(5) . . . . ?
C16 O6 C17 C18 -179.1(5) . . . . ?
C18 O1 C19 C20 175.2(4) . . . . ?
C24 O4 C13 C14 172.9(4) . . . . ?
C13 O4 C24 C23 176.0(4) . . . . ?
C14 O5 C15 C16 174.9(5) . . . . ?
C22 O3 C23 C24 177.8(5) . . . . ?
C12 S18 C10 S16 179.7(3) . . . . ?
C12 S18 C10 C11 0.1(4) . . . . ?
C12 S19 C11 S17 179.8(3) . . . . ?
C12 S19 C11 C10 0.4(4) . . . . ?
C21 O2 C20 C19 177.4(4) . . . . ?
O12 C37A C38A O13A 68(5) . . . . ?
O11 C35 C36 O12 48.4(16) . . . . ?
O11 C35 C36A O12 -60.0(13) . . . . ?
O11 C34 C33 O10 -17.6(14) . . . . ?
O8 C40 C39 O13 53.1(10) . . . . ?
O8 C40 C39 O13A 24.9(15) . . . . ?
O13 C38 C37 O12 -63(2) . . . . ?
O9 C30 C29 O8 -58.9(9) . . . . ?
O9 C31 C32 O10 56.0(12) . . . . ?
C35 O11 C34 C33 179.8(8) . . . . ?
C40 O8 C29 C30 -176.4(6) . . . . ?
C40 C39 O13A C38A 154(4) . . . . ?
C30 O9 C31 C32 178.2(8) . . . . ?
C34 O11 C35 C36 153.5(11) . . . . ?
C34 O11 C35 C36A -152.9(10) . . . . ?
C29 O8 C40 C39 173.9(7) . . . . ?
C38 O13 C39 C40 -169.1(11) . . . . ?
C31 O9 C30 C29 178.7(7) . . . . ?
C39 O13 C38 C37 -176.7(15) . . . . ?
C39 O13A C38A C37A 156(3) . . . . ?
C33 O10 C32 C31 169.6(8) . . . . ?
C32 O10 C33 C34 -177.4(8) . . . . ?
C37 O12 C36 C35 179.0(11) . . . . ?
C36 O12 C37 C38 -175.2(14) . . . . ?
C37A O12 C36A C35 -175.3(11) . . . . ?
C36A O12 C37A C38A -168(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 2.957
_oxdiff_exptl_absorpt_empirical_full_min 0.550
####################################################################### 
# 
# 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_18c6_nc2oc2n_lt_09_183_00_auto
_database_code_depnum_ccdc_archive 'CCDC 2384656'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2024-09-17 deposited with the CCDC.	2024-11-08 downloaded from the CCDC.
;
_audit_creation_date             2023-12-22
_audit_creation_method           
;
Olex2 1.5-ac5-023
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C6 Ni S10), C4 H14 N2 O, 2(C12 H24 O6)'
_chemical_formula_sum            'C40 H62 N2 Ni2 O13 S20'
_chemical_formula_weight         1537.53
_chemical_melting_point          ?
_chemical_oxdiff_formula         C40H62N2Ni2O13S20
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                   13.1130(4)
_cell_length_b                   14.4648(3)
_cell_length_c                   18.1307(5)
_cell_angle_alpha                90.322(2)
_cell_angle_beta                 100.339(2)
_cell_angle_gamma                104.569(2)
_cell_volume                     3269.70(15)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    15073
_cell_measurement_temperature    183.00(14)
_cell_measurement_theta_max      31.0710
_cell_measurement_theta_min      2.0330
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.269
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.279
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.67a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark black'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-18 1 10 0.1992
0 -20 1 0.2466
17 0 -10 0.3022
0 20 -1 0.2622
-1 1 -25 0.0522
4 -3 24 0.0019

_exptl_crystal_size_max          0.587
_exptl_crystal_size_mid          0.51
_exptl_crystal_size_min          0.116
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-17.5353 0.5922 10.4471 -0.0999 0.5420 0.8344
0.1661 -19.7779 0.7492 -0.1695 0.9133 -0.3704
17.3240 0.4213 -10.3643 0.1074 -0.5822 -0.8059
-0.0319 19.7421 -0.8278 0.1700 -0.9160 0.3635
-0.5012 1.0542 -25.0122 0.9786 0.0771 -0.1908
3.6120 -3.2451 23.7169 -0.9969 -0.0784 0.0089

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_unetI/netI     0.0591
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.792
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            43704
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.792
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.932
_diffrn_reflns_theta_min         2.162
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      183.00(14)
_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 0.792
_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    1.46    --   -5.80 -99.00   0.00   90
  2  ω    -77.00   4.00   0.50    1.46    --   -5.80 -37.00 -90.00  162
  3  ω    -75.00 -43.00   0.50    1.46    --   -5.80 -57.00  30.00   64
  4  ω    -38.00   3.00   0.50    1.46    --   -5.80 -57.00  30.00   82
  5  ω    -15.00  68.00   0.50    1.46    --   -5.80  37.00-150.00  166
  6  ω    -67.00   7.00   0.50    1.46    --   -5.80 -37.00  30.00  148
  7  ω    -11.00  35.00   0.50    1.46    --    6.03 -99.00-150.00   92
;
_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      -0.0169968000
_diffrn_orient_matrix_UB_12      0.0069681000
_diffrn_orient_matrix_UB_13      -0.0384904000
_diffrn_orient_matrix_UB_21      -0.0350755000
_diffrn_orient_matrix_UB_22      -0.0466354000
_diffrn_orient_matrix_UB_23      -0.0043466000
_diffrn_orient_matrix_UB_31      -0.0414414000
_diffrn_orient_matrix_UB_32      0.0187322000
_diffrn_orient_matrix_UB_33      0.0092479000
_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                9900
_reflns_number_total             16409
_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 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.848
_refine_diff_density_min         -0.732
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     862
_refine_ls_number_reflns         16409
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0551
_refine_ls_restrained_S_all      1.029
_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)+(0.0626P)²+2.5604P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1263
_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 N(H,H,H) groups
2. Rigid body (RIGU) restrains
 C31A, O9A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C38, O13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C33A, O10A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(C29A)=Sof(H29C)=Sof(H29D)=Sof(O12A)=Sof(C37A)=Sof(H37C)=Sof(H37D)=
 Sof(C36A)=Sof(H36C)=Sof(H36D)=Sof(C38A)=Sof(H38C)=Sof(H38D)=Sof(C35A)=
 Sof(H35C)=Sof(H35D)=Sof(O13A)=Sof(O11A)=Sof(C39A)=Sof(H39C)=Sof(H39D)=
 Sof(C34A)=Sof(H34C)=Sof(H34D)=Sof(C40A)=Sof(H40C)=Sof(H40D)=Sof(O8A)=Sof(O10A)=
 Sof(C30A)=Sof(H30C)=Sof(H30D)=Sof(C32A)=Sof(H32C)=Sof(H32D)=Sof(O9A)=Sof(C31A)=
 Sof(H31C)=Sof(H31D)=Sof(C33A)=Sof(H33C)=Sof(H33D)=1-FVAR(1)
 Sof(O12)=Sof(O8)=Sof(O13)=Sof(O10)=Sof(O11)=Sof(C38)=Sof(H38A)=Sof(H38B)=
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C40)=Sof(H40A)=
 Sof(H40B)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(O9)=Sof(C32)=Sof(H32A)=Sof(H32B)=
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(C29)=Sof(H29A)=
 Sof(H29B)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C31)=
 Sof(H31A)=Sof(H31B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C27(H27A,H27B), C25(H25A,H25B), C28(H28A,H28B), C13(H13A,
 H13B), C21(H21A,H21B), C14(H14A,H14B), C16(H16A,H16B), C22(H22A,H22B),
 C24(H24A,H24B), C23(H23A,H23B), C18(H18A,H18B), C17(H17A,H17B), C15(H15A,H15B),
  C20(H20A,H20B), C19(H19A,H19B), C38(H38A,H38B), C39(H39A,H39B), C37(H37A,
 H37B), C40(H40A,H40B), C35(H35A,H35B), C32(H32A,H32B), C36(H36A,H36B),
 C34(H34A,H34B), C29(H29A,H29B), C30(H30A,H30B), C29A(H29C,H29D), C37A(H37C,
 H37D), C36A(H36C,H36D), C38A(H38C,H38D), C35A(H35C,H35D), C39A(H39C,H39D),
 C34A(H34C,H34D), C40A(H40C,H40D), C30A(H30C,H30D), C32A(H32C,H32D), C33(H33A,
 H33B), C31(H31A,H31B), C31A(H31C,H31D), C33A(H33C,H33D)
4.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(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 0.70094(3) 0.92154(3) 0.98481(3) 0.03911(13) Uani 1 1 d . . . . .
Ni2 Ni 0.500000 0.500000 1.000000 0.04191(17) Uani 1 2 d S . P . .
Ni3 Ni 0.500000 0.500000 0.500000 0.04989(19) Uani 1 2 d S . P . .
S4 S 0.53022(7) 0.90268(6) 0.95967(6) 0.0426(2) Uani 1 1 d . . . . .
S6 S 0.69652(7) 0.99972(7) 1.08527(6) 0.0470(2) Uani 1 1 d . . . . .
S5 S 0.70100(7) 0.83649(7) 0.88618(6) 0.0464(2) Uani 1 1 d . . . . .
S7 S 0.87225(7) 0.94137(7) 1.01264(6) 0.0486(2) Uani 1 1 d . . . . .
S15 S 0.59226(8) 0.64729(7) 1.00891(6) 0.0496(2) Uani 1 1 d . . . . .
S14 S 0.57714(8) 0.47007(7) 1.10954(6) 0.0491(2) Uani 1 1 d . . . . .
S13 S 0.76243(9) 0.76134(7) 1.13509(7) 0.0572(3) Uani 1 1 d . . . . .
S2 S 0.36047(7) 0.78958(7) 0.83478(6) 0.0485(2) Uani 1 1 d . . . . .
S9 S 1.03236(8) 1.02766(8) 1.15442(8) 0.0628(3) Uani 1 1 d . . . . .
S20 S 0.59371(10) 0.49280(9) 0.41497(7) 0.0618(3) Uani 1 1 d . . . . .
S19 S 0.63771(10) 0.57177(8) 0.58229(6) 0.0583(3) Uani 1 1 d . . . . .
S17 S 0.87400(10) 0.62957(8) 0.57444(7) 0.0637(3) Uani 1 1 d . . . . .
S12 S 0.74879(9) 0.59827(8) 1.22772(7) 0.0576(3) Uani 1 1 d . . . . .
S8 S 0.86837(10) 1.07803(8) 1.22144(7) 0.0630(3) Uani 1 1 d . . . . .
S11 S 0.91075(10) 0.78129(9) 1.28162(9) 0.0749(4) Uani 1 1 d . . . . .
S3 S 0.51534(8) 0.72158(8) 0.76972(7) 0.0567(3) Uani 1 1 d . . . . .
S18 S 0.83396(11) 0.55725(11) 0.42056(7) 0.0755(4) Uani 1 1 d . . . . .
S10 S 1.08902(13) 1.11723(9) 1.30977(9) 0.0909(5) Uani 1 1 d . . . . .
S1 S 0.28259(11) 0.65479(11) 0.70196(9) 0.0859(5) Uani 1 1 d . . . . .
S16 S 1.05733(13) 0.64450(15) 0.49702(10) 0.1062(6) Uani 1 1 d . . . . .
O7 O 0.2409(2) 0.67420(17) 0.30714(15) 0.0452(6) Uani 1 1 d . . . . .
O5 O 0.0765(2) 0.7168(2) 0.02889(17) 0.0577(7) Uani 1 1 d . . . . .
O4 O 0.2887(2) 0.73458(19) 0.09913(17) 0.0568(7) Uani 1 1 d . . . . .
O6 O -0.0922(2) 0.5742(2) 0.06731(18) 0.0653(8) Uani 1 1 d . . . . .
O2 O 0.1719(3) 0.42637(18) 0.21244(17) 0.0607(8) Uani 1 1 d . . . . .
O1 O -0.0334(3) 0.4157(2) 0.13990(18) 0.0662(9) Uani 1 1 d . . . . .
O3 O 0.3298(2) 0.5655(2) 0.15831(16) 0.0560(7) Uani 1 1 d . . . . .
N1 N 0.1196(2) 0.59984(19) 0.15545(17) 0.0410(7) Uani 1 1 d . . . . .
H1A H 0.098912 0.622171 0.109841 0.049 Uiso 1 1 calc R U . . .
H1B H 0.089441 0.535815 0.154747 0.049 Uiso 1 1 calc R U . . .
H1C H 0.192307 0.611156 0.165789 0.049 Uiso 1 1 calc R U . . .
O12 O 0.6443(19) 0.8506(14) 0.3631(9) 0.089(6) Uani 0.609(9) 1 d . . P A 1
N2 N 0.4278(3) 0.8139(2) 0.39600(19) 0.0494(8) Uani 1 1 d . . . . .
H2A H 0.391703 0.831633 0.352988 0.059 Uiso 1 1 calc R U . . .
H2B H 0.499461 0.839359 0.399323 0.059 Uiso 1 1 calc R U . . .
H2C H 0.406204 0.835756 0.436240 0.059 Uiso 1 1 calc R U . . .
O8 O 0.4291(14) 0.8630(13) 0.5560(10) 0.071(5) Uani 0.609(9) 1 d . . P A 1
O13 O 0.6031(8) 0.8136(7) 0.5110(6) 0.076(3) Uani 0.609(9) 1 d . . P A 1
C26 C 0.1301(3) 0.6295(3) 0.2918(2) 0.0507(10) Uani 1 1 d . . . . .
H26A H 0.094241 0.654370 0.328255 0.061 Uiso 1 1 calc R U . . .
H26B H 0.118224 0.559662 0.296721 0.061 Uiso 1 1 calc R U . . .
C9 C 0.6700(3) 0.6559(3) 1.0968(2) 0.0457(9) Uani 1 1 d . . . . .
C5 C 0.8270(3) 1.0231(3) 1.1315(2) 0.0483(9) Uani 1 1 d . . . . .
C27 C 0.2881(4) 0.6605(3) 0.3818(2) 0.0564(11) Uani 1 1 d . . . . .
H27A H 0.276982 0.591306 0.389690 0.068 Uiso 1 1 calc R U . . .
H27B H 0.253666 0.688017 0.417827 0.068 Uiso 1 1 calc R U . . .
C25 C 0.0839(3) 0.6493(3) 0.2140(2) 0.0554(11) Uani 1 1 d . . . . .
H25A H 0.004718 0.628958 0.206782 0.066 Uiso 1 1 calc R U . . .
H25B H 0.104984 0.719140 0.207862 0.066 Uiso 1 1 calc R U . . .
C28 C 0.4048(4) 0.7081(3) 0.3951(3) 0.0579(11) Uani 1 1 d . . . . .
H28A H 0.439407 0.689183 0.443776 0.069 Uiso 1 1 calc R U . . .
H28B H 0.436795 0.685496 0.355236 0.069 Uiso 1 1 calc R U . . .
C4 C 0.9038(3) 0.9984(3) 1.1000(2) 0.0504(10) Uani 1 1 d . . . . .
C2 C 0.5666(3) 0.7991(2) 0.8490(2) 0.0429(8) Uani 1 1 d . . . . .
C13 C 0.2632(4) 0.7904(3) 0.0394(3) 0.0690(13) Uani 1 1 d . . . . .
H13A H 0.263239 0.757571 -0.008654 0.083 Uiso 1 1 calc R U . . .
H13B H 0.317672 0.852645 0.044493 0.083 Uiso 1 1 calc R U . . .
C21 C 0.2727(4) 0.4122(3) 0.2065(3) 0.0687(14) Uani 1 1 d . . . . .
H21A H 0.269104 0.382906 0.156356 0.082 Uiso 1 1 calc R U . . .
H21B H 0.293102 0.368426 0.244898 0.082 Uiso 1 1 calc R U . . .
C14 C 0.1552(4) 0.8065(3) 0.0393(3) 0.0705(14) Uani 1 1 d . . . . .
H14A H 0.154926 0.838698 0.087624 0.085 Uiso 1 1 calc R U . . .
H14B H 0.138060 0.848302 -0.001581 0.085 Uiso 1 1 calc R U . . .
C7 C 0.8129(3) 0.7175(3) 1.2185(3) 0.0585(11) Uani 1 1 d . . . . .
C12 C 0.7214(4) 0.5442(3) 0.4623(2) 0.0544(10) Uani 1 1 d . . . . .
C16 C -0.1045(4) 0.6326(4) 0.0040(3) 0.0720(14) Uani 1 1 d . . . . .
H16A H -0.178725 0.639865 -0.006976 0.086 Uiso 1 1 calc R U . . .
H16B H -0.091298 0.601282 -0.040791 0.086 Uiso 1 1 calc R U . . .
C3 C 0.4927(3) 0.8293(2) 0.8802(2) 0.0402(8) Uani 1 1 d . . . . .
C22 C 0.3534(4) 0.5055(4) 0.2179(3) 0.0644(12) Uani 1 1 d . . . . .
H22A H 0.353013 0.536795 0.266488 0.077 Uiso 1 1 calc R U . . .
H22B H 0.425698 0.495703 0.219140 0.077 Uiso 1 1 calc R U . . .
C8 C 0.6639(3) 0.5790(3) 1.1399(2) 0.0467(9) Uani 1 1 d . . . . .
C11 C 0.7412(3) 0.5794(3) 0.5345(2) 0.0521(10) Uani 1 1 d . . . . .
C24 C 0.3847(3) 0.7063(3) 0.0966(3) 0.0674(13) Uani 1 1 d . . . . .
H24A H 0.444704 0.763566 0.096193 0.081 Uiso 1 1 calc R U . . .
H24B H 0.375315 0.666310 0.050121 0.081 Uiso 1 1 calc R U . . .
C23 C 0.4092(4) 0.6516(4) 0.1628(3) 0.0687(13) Uani 1 1 d . . . . .
H23A H 0.480091 0.638249 0.164714 0.082 Uiso 1 1 calc R U . . .
H23B H 0.412093 0.689427 0.209113 0.082 Uiso 1 1 calc R U . . .
C18 C -0.1417(4) 0.4258(4) 0.1211(3) 0.0825(17) Uani 1 1 d . . . . .
H18A H -0.158249 0.459544 0.163347 0.099 Uiso 1 1 calc R U . . .
H18B H -0.192885 0.361809 0.112281 0.099 Uiso 1 1 calc R U . . .
C6 C 1.0017(4) 1.0755(3) 1.2330(3) 0.0679(13) Uani 1 1 d . . . . .
C17 C -0.1530(4) 0.4808(4) 0.0526(3) 0.0783(15) Uani 1 1 d . . . . .
H17A H -0.129149 0.450575 0.011950 0.094 Uiso 1 1 calc R U . . .
H17B H -0.229356 0.479938 0.035539 0.094 Uiso 1 1 calc R U . . .
C1 C 0.3802(3) 0.7180(3) 0.7641(3) 0.0555(11) Uani 1 1 d . . . . .
O10 O 0.2957(10) 0.9295(7) 0.3082(6) 0.067(2) Uani 0.609(9) 1 d . . P A 1
C15 C -0.0281(4) 0.7274(4) 0.0204(3) 0.0749(15) Uani 1 1 d . . . . .
H15A H -0.041087 0.769619 -0.021111 0.090 Uiso 1 1 calc R U . . .
H15B H -0.037935 0.757139 0.067100 0.090 Uiso 1 1 calc R U . . .
C10 C 0.9290(4) 0.6128(4) 0.4969(3) 0.0684(13) Uani 1 1 d . . . . .
C20 C 0.0881(5) 0.3385(3) 0.2055(3) 0.0821(17) Uani 1 1 d . . . . .
H20A H 0.102729 0.299116 0.248668 0.099 Uiso 1 1 calc R U . . .
H20B H 0.086214 0.301597 0.158923 0.099 Uiso 1 1 calc R U . . .
C19 C -0.0152(5) 0.3607(3) 0.2035(3) 0.0866(18) Uani 1 1 d . . . . .
H19A H -0.073244 0.300972 0.199402 0.104 Uiso 1 1 calc R U . . .
H19B H -0.013864 0.397530 0.250029 0.104 Uiso 1 1 calc R U . . .
O11 O 0.4741(8) 0.8883(6) 0.2588(6) 0.072(2) Uani 0.609(9) 1 d . . P A 1
C38 C 0.706(2) 0.8267(13) 0.4950(18) 0.096(7) Uani 0.609(9) 1 d . . P A 1
H38A H 0.744036 0.785251 0.525845 0.116 Uiso 0.609(9) 1 calc R U P A 1
H38B H 0.746964 0.894088 0.507310 0.116 Uiso 0.609(9) 1 calc R U P A 1
C39 C 0.5978(17) 0.8437(12) 0.5830(12) 0.103(9) Uani 0.609(9) 1 d . . P A 1
H39A H 0.621834 0.914392 0.588322 0.123 Uiso 0.609(9) 1 calc R U P A 1
H39B H 0.647358 0.818063 0.620146 0.123 Uiso 0.609(9) 1 calc R U P A 1
C37 C 0.6979(11) 0.8025(11) 0.4137(12) 0.118(7) Uani 0.609(9) 1 d . . P A 1
H37A H 0.771634 0.813028 0.403762 0.142 Uiso 0.609(9) 1 calc R U P A 1
H37B H 0.662833 0.733356 0.404116 0.142 Uiso 0.609(9) 1 calc R U P A 1
C40 C 0.4896(12) 0.8125(9) 0.5995(6) 0.105(4) Uani 0.609(9) 1 d . . P A 1
H40A H 0.459829 0.743026 0.587454 0.126 Uiso 0.609(9) 1 calc R U P A 1
H40B H 0.490723 0.825602 0.653379 0.126 Uiso 0.609(9) 1 calc R U P A 1
C35 C 0.5805(19) 0.921(2) 0.2509(16) 0.112(9) Uani 0.609(9) 1 d . . P A 1
H35A H 0.611861 0.986410 0.273780 0.135 Uiso 0.609(9) 1 calc R U P A 1
H35B H 0.586224 0.921215 0.197145 0.135 Uiso 0.609(9) 1 calc R U P A 1
O9 O 0.2485(9) 0.8692(7) 0.4476(5) 0.071(2) Uani 0.609(9) 1 d . . P A 1
C32 C 0.1885(14) 0.8985(14) 0.3231(9) 0.071(4) Uani 0.609(9) 1 d . . P A 1
H32A H 0.140955 0.930131 0.289510 0.085 Uiso 0.609(9) 1 calc R U P A 1
H32B H 0.161335 0.828580 0.312460 0.085 Uiso 0.609(9) 1 calc R U P A 1
C36 C 0.6393(12) 0.8489(12) 0.2925(11) 0.100(5) Uani 0.609(9) 1 d . . P A 1
H36A H 0.601742 0.783391 0.271496 0.120 Uiso 0.609(9) 1 calc R U P A 1
H36B H 0.713102 0.863277 0.282219 0.120 Uiso 0.609(9) 1 calc R U P A 1
C34 C 0.4137(13) 0.9501(12) 0.2213(8) 0.074(5) Uani 0.609(9) 1 d . . P A 1
H34A H 0.416230 0.948712 0.167018 0.088 Uiso 0.609(9) 1 calc R U P A 1
H34B H 0.445210 1.016705 0.242073 0.088 Uiso 0.609(9) 1 calc R U P A 1
C29 C 0.3165(11) 0.8379(8) 0.5684(6) 0.099(4) Uani 0.609(9) 1 d . . P A 1
H29A H 0.283243 0.769187 0.554830 0.119 Uiso 0.609(9) 1 calc R U P A 1
H29B H 0.315847 0.849453 0.622209 0.119 Uiso 0.609(9) 1 calc R U P A 1
C30 C 0.2566(17) 0.8937(14) 0.5243(8) 0.073(5) Uani 0.609(9) 1 d . . P A 1
H30A H 0.184051 0.881609 0.536784 0.087 Uiso 0.609(9) 1 calc R U P A 1
H30B H 0.292570 0.962557 0.535021 0.087 Uiso 0.609(9) 1 calc R U P A 1
C29A C 0.3363(14) 0.9107(9) 0.5565(11) 0.073(5) Uani 0.391(9) 1 d . . P A 2
H29C H 0.372598 0.979832 0.559837 0.088 Uiso 0.391(9) 1 calc R U P A 2
H29D H 0.312003 0.892989 0.604296 0.088 Uiso 0.391(9) 1 calc R U P A 2
O12A O 0.652(3) 0.8556(16) 0.3866(11) 0.057(4) Uani 0.391(9) 1 d . . P A 2
C37A C 0.7378(12) 0.8376(12) 0.4417(12) 0.058(4) Uani 0.391(9) 1 d . . P A 2
H37C H 0.793217 0.897837 0.458902 0.069 Uiso 0.391(9) 1 calc R U P A 2
H37D H 0.771894 0.792307 0.420721 0.069 Uiso 0.391(9) 1 calc R U P A 2
C36A C 0.7020(18) 0.8938(14) 0.3214(12) 0.091(6) Uani 0.391(9) 1 d . . P A 2
H36C H 0.743169 0.961256 0.332952 0.109 Uiso 0.391(9) 1 calc R U P A 2
H36D H 0.751918 0.856208 0.311045 0.109 Uiso 0.391(9) 1 calc R U P A 2
C38A C 0.686(2) 0.7959(16) 0.505(2) 0.064(6) Uani 0.391(9) 1 d . . P A 2
H38C H 0.642325 0.729783 0.490418 0.077 Uiso 0.391(9) 1 calc R U P A 2
H38D H 0.741338 0.794409 0.549565 0.077 Uiso 0.391(9) 1 calc R U P A 2
C35A C 0.620(2) 0.887(2) 0.2584(14) 0.086(9) Uani 0.391(9) 1 d . . P A 2
H35C H 0.650920 0.921777 0.217225 0.103 Uiso 0.391(9) 1 calc R U P A 2
H35D H 0.589533 0.819332 0.240984 0.103 Uiso 0.391(9) 1 calc R U P A 2
O13A O 0.6214(12) 0.8553(7) 0.5195(9) 0.055(3) Uani 0.391(9) 1 d . . P A 2
O11A O 0.537(2) 0.9259(14) 0.2738(9) 0.099(8) Uani 0.391(9) 1 d . . P A 2
C39A C 0.5795(19) 0.8201(14) 0.5895(14) 0.047(4) Uani 0.391(9) 1 d . . P A 2
H39C H 0.638452 0.827563 0.633465 0.056 Uiso 0.391(9) 1 calc R U P A 2
H39D H 0.537733 0.752373 0.582445 0.056 Uiso 0.391(9) 1 calc R U P A 2
C34A C 0.470(2) 0.935(2) 0.2161(19) 0.128(12) Uani 0.391(9) 1 d . . P A 2
H34C H 0.448259 0.873495 0.186080 0.154 Uiso 0.391(9) 1 calc R U P A 2
H34D H 0.508925 0.983517 0.185677 0.154 Uiso 0.391(9) 1 calc R U P A 2
C40A C 0.5084(14) 0.8867(9) 0.5975(7) 0.061(4) Uani 0.391(9) 1 d . . P A 2
H40C H 0.491583 0.884584 0.648657 0.074 Uiso 0.391(9) 1 calc R U P A 2
H40D H 0.546135 0.953234 0.589527 0.074 Uiso 0.391(9) 1 calc R U P A 2
O8A O 0.4061(16) 0.8547(18) 0.5398(14) 0.041(4) Uani 0.391(9) 1 d . . P A 2
O10A O 0.3177(17) 0.9100(10) 0.2827(13) 0.091(6) Uani 0.391(9) 1 d . . P A 2
C30A C 0.2359(19) 0.8843(17) 0.4857(18) 0.084(12) Uani 0.391(9) 1 d . . P A 2
H30C H 0.205832 0.814153 0.479171 0.101 Uiso 0.391(9) 1 calc R U P A 2
H30D H 0.178538 0.913959 0.494643 0.101 Uiso 0.391(9) 1 calc R U P A 2
C32A C 0.228(2) 0.9372(16) 0.2950(15) 0.112(12) Uani 0.391(9) 1 d . . P A 2
H32C H 0.169806 0.917287 0.250565 0.135 Uiso 0.391(9) 1 calc R U P A 2
H32D H 0.245384 1.007712 0.302067 0.135 Uiso 0.391(9) 1 calc R U P A 2
O9A O 0.2727(7) 0.9178(8) 0.4252(8) 0.075(4) Uani 0.391(9) 1 d . . P A 2
C33 C 0.3011(11) 0.9176(9) 0.2319(7) 0.073(3) Uani 0.609(9) 1 d . . P A 1
H33A H 0.257156 0.955006 0.201268 0.088 Uiso 0.609(9) 1 calc R U P A 1
H33B H 0.271859 0.849342 0.215010 0.088 Uiso 0.609(9) 1 calc R U P A 1
C31 C 0.1861(11) 0.9210(9) 0.3992(7) 0.083(4) Uani 0.609(9) 1 d . . P A 1
H31A H 0.111097 0.903463 0.407369 0.099 Uiso 0.609(9) 1 calc R U P A 1
H31B H 0.215738 0.990629 0.410785 0.099 Uiso 0.609(9) 1 calc R U P A 1
C31A C 0.190(2) 0.892(2) 0.3637(19) 0.109(14) Uani 0.391(9) 1 d . . P A 2
H31C H 0.127480 0.914792 0.372978 0.131 Uiso 0.391(9) 1 calc R U P A 2
H31D H 0.166694 0.821797 0.355520 0.131 Uiso 0.391(9) 1 calc R U P A 2
C33A C 0.369(3) 0.963(3) 0.225(2) 0.117(10) Uani 0.391(9) 1 d . . P A 2
H33C H 0.386381 1.031953 0.238851 0.141 Uiso 0.391(9) 1 calc R U P A 2
H33D H 0.317493 0.950150 0.176883 0.141 Uiso 0.391(9) 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 S4 2.1491(9) . ?
Ni1 S6 2.1558(11) . ?
Ni1 S5 2.1650(11) . ?
Ni1 S7 2.1564(10) . ?
Ni2 S15 2.1582(10) . ?
Ni2 S15 2.1582(10) 2_667 ?
Ni2 S14 2.1595(10) . ?
Ni2 S14 2.1596(10) 2_667 ?
Ni3 S20 2.1540(11) . ?
Ni3 S20 2.1541(11) 2_666 ?
Ni3 S19 2.1534(12) . ?
Ni3 S19 2.1534(12) 2_666 ?
S4 C3 1.706(4) . ?
S6 C5 1.714(4) . ?
S5 C2 1.715(4) . ?
S7 C4 1.714(5) . ?
S15 C9 1.716(4) . ?
S14 C8 1.715(4) . ?
S13 C9 1.742(4) . ?
S13 C7 1.729(5) . ?
S2 C3 1.731(4) . ?
S2 C1 1.738(4) . ?
S9 C4 1.742(4) . ?
S9 C6 1.733(6) . ?
S20 C12 1.715(5) . ?
S19 C11 1.718(4) . ?
S17 C11 1.729(5) . ?
S17 C10 1.732(5) . ?
S12 C7 1.742(5) . ?
S12 C8 1.748(4) . ?
S8 C5 1.742(4) . ?
S8 C6 1.733(5) . ?
S11 C7 1.635(5) . ?
S3 C2 1.740(4) . ?
S3 C1 1.744(4) . ?
S18 C12 1.746(4) . ?
S18 C10 1.726(5) . ?
S10 C6 1.638(5) . ?
S1 C1 1.620(5) . ?
S16 C10 1.629(5) . ?
O7 C26 1.409(5) . ?
O7 C27 1.421(5) . ?
O5 C14 1.427(5) . ?
O5 C15 1.400(5) . ?
O4 C13 1.398(5) . ?
O4 C24 1.426(5) . ?
O6 C16 1.439(6) . ?
O6 C17 1.383(6) . ?
O2 C21 1.410(5) . ?
O2 C20 1.443(6) . ?
O1 C18 1.444(6) . ?
O1 C19 1.423(6) . ?
O3 C22 1.427(5) . ?
O3 C23 1.400(5) . ?
N1 C25 1.482(5) . ?
O12 C37 1.36(3) . ?
O12 C36 1.27(2) . ?
N2 C28 1.484(5) . ?
O8 C40 1.36(2) . ?
O8 C29 1.488(18) . ?
O13 C38 1.40(3) . ?
O13 C39 1.39(2) . ?
C26 C25 1.491(6) . ?
C9 C8 1.357(5) . ?
C5 C4 1.361(6) . ?
C27 C28 1.487(6) . ?
C2 C3 1.364(5) . ?
C13 C14 1.492(7) . ?
C21 C22 1.478(7) . ?
C12 C11 1.359(6) . ?
C16 C15 1.474(7) . ?
C24 C23 1.473(7) . ?
C18 C17 1.484(8) . ?
O10 C32 1.44(2) . ?
O10 C33 1.409(15) . ?
C20 C19 1.464(8) . ?
O11 C35 1.39(3) . ?
O11 C34 1.435(16) . ?
C38 C37 1.49(3) . ?
C39 C40 1.46(2) . ?
C35 C36 1.57(3) . ?
O9 C30 1.412(18) . ?
O9 C31 1.437(15) . ?
C32 C31 1.42(2) . ?
C34 C33 1.48(2) . ?
C29 C30 1.42(2) . ?
C29A O8A 1.43(2) . ?
C29A C30A 1.63(3) . ?
O12A C37A 1.44(4) . ?
O12A C36A 1.49(3) . ?
C37A C38A 1.48(4) . ?
C36A C35A 1.41(4) . ?
C38A O13A 1.41(3) . ?
C35A O11A 1.41(4) . ?
O13A C39A 1.51(3) . ?
O11A C34A 1.27(3) . ?
C39A C40A 1.52(2) . ?
C34A C33A 1.52(4) . ?
C40A O8A 1.51(3) . ?
O10A C32A 1.38(3) . ?
O10A C33A 1.45(4) . ?
C30A O9A 1.32(3) . ?
C32A C31A 1.51(5) . ?
O9A C31A 1.39(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 S6 85.59(4) . . ?
S4 Ni1 S5 93.30(4) . . ?
S4 Ni1 S7 178.71(5) . . ?
S6 Ni1 S5 177.09(4) . . ?
S6 Ni1 S7 93.17(4) . . ?
S7 Ni1 S5 87.93(4) . . ?
S15 Ni2 S15 180.0 2_667 . ?
S15 Ni2 S14 93.35(4) . . ?
S15 Ni2 S14 86.65(4) . 2_667 ?
S15 Ni2 S14 93.34(4) 2_667 2_667 ?
S15 Ni2 S14 86.66(4) 2_667 . ?
S14 Ni2 S14 180.0 . 2_667 ?
S20 Ni3 S20 180.0 . 2_666 ?
S19 Ni3 S20 93.49(4) 2_666 2_666 ?
S19 Ni3 S20 93.49(4) . . ?
S19 Ni3 S20 86.51(4) 2_666 . ?
S19 Ni3 S20 86.51(4) . 2_666 ?
S19 Ni3 S19 180.0 . 2_666 ?
C3 S4 Ni1 102.50(12) . . ?
C5 S6 Ni1 102.03(15) . . ?
C2 S5 Ni1 101.66(13) . . ?
C4 S7 Ni1 102.29(14) . . ?
C9 S15 Ni2 102.11(13) . . ?
C8 S14 Ni2 101.88(14) . . ?
C7 S13 C9 97.7(2) . . ?
C3 S2 C1 97.99(19) . . ?
C6 S9 C4 97.7(2) . . ?
C12 S20 Ni3 101.75(15) . . ?
C11 S19 Ni3 102.32(16) . . ?
C11 S17 C10 97.5(2) . . ?
C7 S12 C8 97.3(2) . . ?
C6 S8 C5 97.3(2) . . ?
C2 S3 C1 97.91(19) . . ?
C10 S18 C12 97.4(2) . . ?
C26 O7 C27 111.4(3) . . ?
C15 O5 C14 112.4(3) . . ?
C13 O4 C24 112.1(3) . . ?
C17 O6 C16 112.8(4) . . ?
C21 O2 C20 113.3(4) . . ?
C19 O1 C18 113.9(4) . . ?
C23 O3 C22 112.1(4) . . ?
C36 O12 C37 127.2(19) . . ?
C40 O8 C29 111.6(16) . . ?
C39 O13 C38 116.1(16) . . ?
O7 C26 C25 109.1(3) . . ?
S15 C9 S13 122.7(2) . . ?
C8 C9 S15 121.1(3) . . ?
C8 C9 S13 116.2(3) . . ?
S6 C5 S8 122.1(2) . . ?
C4 C5 S6 121.4(3) . . ?
C4 C5 S8 116.5(3) . . ?
O7 C27 C28 109.4(4) . . ?
N1 C25 C26 113.1(3) . . ?
N2 C28 C27 112.8(3) . . ?
S7 C4 S9 123.6(3) . . ?
C5 C4 S7 120.8(3) . . ?
C5 C4 S9 115.6(3) . . ?
S5 C2 S3 123.1(2) . . ?
C3 C2 S5 121.3(3) . . ?
C3 C2 S3 115.6(3) . . ?
O4 C13 C14 109.5(4) . . ?
O2 C21 C22 109.0(3) . . ?
O5 C14 C13 109.5(3) . . ?
S13 C7 S12 112.8(3) . . ?
S11 C7 S13 123.5(3) . . ?
S11 C7 S12 123.8(3) . . ?
S20 C12 S18 122.5(3) . . ?
C11 C12 S20 121.9(3) . . ?
C11 C12 S18 115.6(3) . . ?
O6 C16 C15 109.8(4) . . ?
S4 C3 S2 122.5(2) . . ?
C2 C3 S4 121.1(3) . . ?
C2 C3 S2 116.4(3) . . ?
O3 C22 C21 109.9(4) . . ?
S14 C8 S12 122.5(2) . . ?
C9 C8 S14 121.6(3) . . ?
C9 C8 S12 115.9(3) . . ?
S19 C11 S17 123.0(3) . . ?
C12 C11 S19 120.5(3) . . ?
C12 C11 S17 116.5(3) . . ?
O4 C24 C23 109.2(4) . . ?
O3 C23 C24 109.4(4) . . ?
O1 C18 C17 109.5(4) . . ?
S9 C6 S8 112.9(3) . . ?
S10 C6 S9 124.3(3) . . ?
S10 C6 S8 122.7(3) . . ?
O6 C17 C18 110.2(4) . . ?
S2 C1 S3 112.0(2) . . ?
S1 C1 S2 122.9(2) . . ?
S1 C1 S3 125.1(2) . . ?
C33 O10 C32 113.4(12) . . ?
O5 C15 C16 109.1(4) . . ?
S18 C10 S17 113.0(3) . . ?
S16 C10 S17 123.2(3) . . ?
S16 C10 S18 123.7(3) . . ?
O2 C20 C19 109.4(4) . . ?
O1 C19 C20 107.6(4) . . ?
C35 O11 C34 109.1(14) . . ?
O13 C38 C37 110(2) . . ?
O13 C39 C40 112.5(15) . . ?
O12 C37 C38 117.6(15) . . ?
O8 C40 C39 106.6(14) . . ?
O11 C35 C36 105.4(19) . . ?
C30 O9 C31 112.3(11) . . ?
C31 C32 O10 111.1(13) . . ?
O12 C36 C35 114.6(17) . . ?
O11 C34 C33 109.2(9) . . ?
C30 C29 O8 110.3(14) . . ?
O9 C30 C29 109.0(13) . . ?
O8A C29A C30A 103.8(15) . . ?
C37A O12A C36A 106(2) . . ?
O12A C37A C38A 105(2) . . ?
C35A C36A O12A 109(2) . . ?
O13A C38A C37A 106(2) . . ?
O11A C35A C36A 112(2) . . ?
C38A O13A C39A 106.3(17) . . ?
C34A O11A C35A 114(2) . . ?
O13A C39A C40A 101.0(14) . . ?
O11A C34A C33A 120(4) . . ?
O8A C40A C39A 108.7(15) . . ?
C29A O8A C40A 106.4(16) . . ?
C32A O10A C33A 114(2) . . ?
O9A C30A C29A 107.4(17) . . ?
O10A C32A C31A 111(2) . . ?
C30A O9A C31A 108(2) . . ?
O10 C33 C34 110.2(12) . . ?
C32 C31 O9 109.2(12) . . ?
O9A C31A C32A 109(2) . . ?
O10A C33A C34A 112(3) . . ?

_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 7.064
_oxdiff_exptl_absorpt_empirical_full_min 0.494
####################################################################### 
# 
# 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_exp_1088_08_233_00_auto
_database_code_depnum_ccdc_archive 'CCDC 2384659'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2024-09-17 deposited with the CCDC.	2024-11-08 downloaded from the CCDC.
;
_audit_creation_date             2023-09-12
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '4(C3 Ni0.5 S5), C4 H14 N2 O, 2(C12 H24 O6)'
_chemical_formula_sum            'C40 H62 N2 Ni2 O13 S20'
_chemical_formula_weight         1537.53
_chemical_melting_point          ?
_chemical_oxdiff_formula         C24H32N2O6NiS10
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                   13.1552(4)
_cell_length_b                   14.5482(6)
_cell_length_c                   18.0978(7)
_cell_angle_alpha                89.797(3)
_cell_angle_beta                 79.517(3)
_cell_angle_gamma                75.794(3)
_cell_volume                     3298.6(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    17550
_cell_measurement_temperature    232.9(4)
_cell_measurement_theta_max      29.1910
_cell_measurement_theta_min      1.6230
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.258
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84027
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.67a (Rigaku Oxford Diffraction, 2022)
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    1.548
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.717
_exptl_crystal_size_mid          0.557
_exptl_crystal_size_min          0.191
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.0483
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            38461
_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         1.625
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      232.9(4)
_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    -94.00 -69.00   0.50    1.20    --  -20.89 153.00-153.00   50
  2  ω   -112.00 -57.00   0.50    1.20    --  -20.89-153.00 165.00  110
  3  ω    -65.00 -39.00   0.50    1.20    --  -20.89 120.00  48.00   52
  4  ω     42.00 102.00   0.50    1.20    --   21.12-153.00 165.00  120
  5  ω     23.00  76.00   0.50    1.20    --   21.12-120.00 -35.00  106
  6  ω     31.00  56.00   0.50    1.20    --  -20.89  19.00-180.00   50
  7  ω    -22.00  59.00   0.50    1.20    --  -20.89  19.00  30.00  162
  8  ω    -24.00  60.00   0.50    1.20    --  -20.89  19.00 -30.00  168
  9  ω    -17.00  36.00   0.50    1.20    --  -20.89 -99.00 120.00  106
 10  ω    -24.00  10.00   0.50    1.20    --  -20.89  19.00-180.00   68
 11  ω     60.00  86.00   0.50    1.20    --   21.12 178.00-150.00   52
 12  ω    -65.00  28.00   0.50    1.20    --   21.12 -19.00  30.00  186
 13  ω    -74.00  23.00   0.50    1.20    --   21.12 -19.00-180.00  194
;
_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      0.0026988000
_diffrn_orient_matrix_UB_12      0.0015089000
_diffrn_orient_matrix_UB_13      -0.0394726000
_diffrn_orient_matrix_UB_21      0.0209543000
_diffrn_orient_matrix_UB_22      -0.0499176000
_diffrn_orient_matrix_UB_23      -0.0035117000
_diffrn_orient_matrix_UB_31      -0.0525249000
_diffrn_orient_matrix_UB_32      -0.0063304000
_diffrn_orient_matrix_UB_33      0.0046028000
_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                9158
_reflns_number_total             13499
_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 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.071
_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     736
_refine_ls_number_reflns         13499
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0521
_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)+(0.0587P)²+2.7823P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1286
_refine_ls_wR_factor_ref         0.1456
_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
 C38A, O13A, C37A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(H35C)=Sof(H35D)=Sof(H39C)=Sof(H39D)=Sof(C37A)=Sof(H37C)=Sof(H37D)=
 Sof(C36A)=Sof(H36C)=Sof(H36D)=Sof(O13A)=Sof(C38A)=Sof(H38C)=Sof(H38D)=1-FVAR(1)
 Sof(O13)=Sof(H35A)=Sof(H35B)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H39A)=Sof(H39B)=
 Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C36)=Sof(H36A)=Sof(H36B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C17(H17A,
 H17B), C19(H19A,H19B), C15(H15A,H15B), C23(H23A,H23B), C20(H20A,H20B),
 C16(H16A,H16B), C18(H18A,H18B), C24(H24A,H24B), C13(H13A,H13B), C14(H14A,H14B),
  C22(H22A,H22B), C21(H21A,H21B), C35(H35A,H35B), C35(H35C,H35D), C40(H40A,
 H40B), C30(H30A,H30B), C34(H34A,H34B), C29(H29A,H29B), C38(H38A,H38B),
 C31(H31A,H31B), C39(H39A,H39B), C39(H39C,H39D), C33(H33A,H33B), C32(H32A,H32B),
  C37(H37A,H37B), C36(H36A,H36B), C37A(H37C,H37D), C36A(H36C,H36D), C38A(H38C,
 H38D)
4.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(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
Ni2 Ni 0.500000 0.500000 0.500000 0.05181(18) Uani 1 2 d S . P . .
Ni1 Ni 0.70061(3) 1.07805(3) 0.51449(3) 0.05127(14) Uani 1 1 d . . . . .
Ni3 Ni 0.500000 0.500000 1.000000 0.0631(2) Uani 1 2 d S . P . .
S2 S 0.53030(7) 1.09750(7) 0.53919(6) 0.0562(3) Uani 1 1 d . . . . .
S12 S 0.42162(8) 0.47021(8) 0.60980(6) 0.0615(3) Uani 1 1 d . . . . .
S7 S 0.69525(8) 1.00129(8) 0.41389(7) 0.0602(3) Uani 1 1 d . . . . .
S11 S 0.41149(9) 0.64668(8) 0.50844(6) 0.0619(3) Uani 1 1 d . . . . .
S1 S 0.70118(8) 1.16222(8) 0.61296(7) 0.0605(3) Uani 1 1 d . . . . .
S4 S 0.36166(8) 1.21038(8) 0.66312(7) 0.0618(3) Uani 1 1 d . . . . .
S6 S 0.87154(7) 1.05764(8) 0.48669(7) 0.0646(3) Uani 1 1 d . . . . .
S3 S 0.51673(9) 1.27603(9) 0.72871(7) 0.0713(3) Uani 1 1 d . . . . .
S14 S 0.25198(9) 0.59750(9) 0.72739(7) 0.0711(3) Uani 1 1 d . . . . .
S13 S 0.24350(10) 0.75998(8) 0.63440(8) 0.0719(3) Uani 1 1 d . . . . .
S16 S 0.63617(11) 0.42516(9) 0.91904(7) 0.0740(3) Uani 1 1 d . . . . .
S8 S 1.03024(9) 0.97135(10) 0.34525(9) 0.0843(4) Uani 1 1 d . . . . .
S9 S 0.86584(10) 0.92324(9) 0.27815(8) 0.0811(4) Uani 1 1 d . . . . .
S15 S 0.09471(10) 0.77962(11) 0.78073(9) 0.0922(4) Uani 1 1 d . . . . .
S17 S 0.59367(11) 0.50975(11) 1.08427(7) 0.0804(4) Uani 1 1 d . . . . .
S5 S 0.28506(11) 1.34362(12) 0.79546(10) 0.0991(5) Uani 1 1 d . . . . .
S18 S 0.87070(11) 0.36728(10) 0.92737(7) 0.0812(4) Uani 1 1 d . . . . .
S10 S 1.08612(14) 0.88255(11) 0.19051(11) 0.1182(7) Uani 1 1 d . . . . .
S19 S 0.83259(12) 0.44490(13) 1.07884(8) 0.0978(5) Uani 1 1 d . . . . .
O7 O 0.7613(2) 0.67212(18) 0.80856(15) 0.0568(7) Uani 1 1 d . . . . .
N1 N 0.8815(2) 0.5992(2) 0.65694(18) 0.0511(7) Uani 1 1 d . . . . .
H1A H 0.905606 0.619037 0.611437 0.061 Uiso 1 1 calc R U . . .
H1B H 0.809738 0.613599 0.665739 0.061 Uiso 1 1 calc R U . . .
H1C H 0.907018 0.535946 0.658027 0.061 Uiso 1 1 calc R U . . .
S20 S 1.05389(14) 0.35457(18) 1.00393(11) 0.1366(8) Uani 1 1 d . . . . .
O6 O 0.7179(3) 0.7346(2) 0.59772(19) 0.0785(9) Uani 1 1 d . . . . .
N2 N 0.5776(3) 0.8117(2) 0.89748(19) 0.0615(9) Uani 1 1 d . . . . .
H2A H 0.609920 0.829673 0.853595 0.074 Uiso 1 1 calc R U . . .
H2B H 0.603726 0.831451 0.935504 0.074 Uiso 1 1 calc R U . . .
H2C H 0.506867 0.837707 0.904139 0.074 Uiso 1 1 calc R U . . .
O1 O 0.6705(2) 0.5684(3) 0.65729(18) 0.0754(9) Uani 1 1 d . . . . .
O5 O 0.9298(3) 0.7148(2) 0.52885(18) 0.0803(9) Uani 1 1 d . . . . .
O3 O 1.0281(3) 0.4139(2) 0.6425(2) 0.0909(11) Uani 1 1 d . . . . .
O4 O 1.0933(3) 0.5696(3) 0.5691(2) 0.0904(11) Uani 1 1 d . . . . .
O2 O 0.8223(3) 0.4277(2) 0.71266(18) 0.0815(10) Uani 1 1 d . . . . .
C2 C 0.4936(3) 1.1697(2) 0.6179(2) 0.0497(9) Uani 1 1 d . . . . .
C8 C 0.3376(3) 0.5786(3) 0.6400(2) 0.0570(10) Uani 1 1 d . . . . .
C7 C 0.3338(3) 0.6549(3) 0.5964(2) 0.0574(10) Uani 1 1 d . . . . .
C1 C 0.5674(3) 1.1996(3) 0.6504(2) 0.0558(10) Uani 1 1 d . . . . .
C25 C 0.9181(3) 0.6468(3) 0.7154(2) 0.0638(11) Uani 1 1 d . . . . .
H25A H 0.899367 0.715404 0.709026 0.077 Uiso 1 1 calc R U . . .
H25B H 0.996068 0.625535 0.708584 0.077 Uiso 1 1 calc R U . . .
C5 C 0.8258(3) 0.9772(3) 0.3675(3) 0.0627(11) Uani 1 1 d . . . . .
C4 C 0.9019(3) 1.0017(3) 0.3999(3) 0.0626(11) Uani 1 1 d . . . . .
C26 C 0.8705(3) 0.6270(3) 0.7934(2) 0.0648(11) Uani 1 1 d . . . . .
H26A H 0.880538 0.558394 0.798391 0.078 Uiso 1 1 calc R U . . .
H26B H 0.906350 0.650312 0.829637 0.078 Uiso 1 1 calc R U . . .
C9 C 0.1913(3) 0.7163(3) 0.7180(3) 0.0703(12) Uani 1 1 d . . . . .
C3 C 0.3817(3) 1.2807(3) 0.7340(3) 0.0687(12) Uani 1 1 d . . . . .
C27 C 0.7132(4) 0.6587(3) 0.8832(3) 0.0675(11) Uani 1 1 d . . . . .
H27A H 0.747619 0.684793 0.918945 0.081 Uiso 1 1 calc R U . . .
H27B H 0.722496 0.590674 0.891316 0.081 Uiso 1 1 calc R U . . .
C11 C 0.7199(4) 0.4566(3) 1.0381(3) 0.0688(12) Uani 1 1 d . . . . .
C28 C 0.5978(4) 0.7068(3) 0.8962(3) 0.0723(12) Uani 1 1 d . . . . .
H28A H 0.562787 0.687721 0.944206 0.087 Uiso 1 1 calc R U . . .
H28B H 0.565999 0.686053 0.856301 0.087 Uiso 1 1 calc R U . . .
C6 C 0.9994(4) 0.9246(3) 0.2670(3) 0.0854(16) Uani 1 1 d . . . . .
C10 C 0.7391(4) 0.4188(3) 0.9665(2) 0.0642(11) Uani 1 1 d . . . . .
C17 C 0.6201(4) 0.7084(4) 0.5965(4) 0.0953(18) Uani 1 1 d . . . . .
H17A H 0.626938 0.670500 0.550410 0.114 Uiso 1 1 calc R U . . .
H17B H 0.562124 0.765637 0.596970 0.114 Uiso 1 1 calc R U . . .
C19 C 0.6443(4) 0.5085(5) 0.7172(3) 0.0866(16) Uani 1 1 d . . . . .
H19A H 0.572436 0.499996 0.718062 0.104 Uiso 1 1 calc R U . . .
H19B H 0.645083 0.538147 0.765534 0.104 Uiso 1 1 calc R U . . .
C15 C 0.8522(6) 0.8038(4) 0.5372(3) 0.1011(19) Uani 1 1 d . . . . .
H15A H 0.869675 0.843536 0.495344 0.121 Uiso 1 1 calc R U . . .
H15B H 0.852971 0.836886 0.584112 0.121 Uiso 1 1 calc R U . . .
C23 C 1.1376(5) 0.4227(5) 0.6243(4) 0.123(3) Uani 1 1 d . . . . .
H23A H 1.186851 0.359534 0.616024 0.147 Uiso 1 1 calc R U . . .
H23B H 1.154137 0.455222 0.666246 0.147 Uiso 1 1 calc R U . . .
C20 C 0.7225(5) 0.4157(4) 0.7057(3) 0.099(2) Uani 1 1 d . . . . .
H20A H 0.700681 0.372070 0.743203 0.119 Uiso 1 1 calc R U . . .
H20B H 0.726091 0.388337 0.655622 0.119 Uiso 1 1 calc R U . . .
C16 C 0.7449(5) 0.7887(4) 0.5385(3) 0.0968(18) Uani 1 1 d . . . . .
H16A H 0.692319 0.850121 0.543171 0.116 Uiso 1 1 calc R U . . .
H16B H 0.743842 0.756666 0.491208 0.116 Uiso 1 1 calc R U . . .
C18 C 0.5948(4) 0.6535(5) 0.6620(4) 0.0958(17) Uani 1 1 d . . . . .
H18A H 0.593520 0.689449 0.708069 0.115 Uiso 1 1 calc R U . . .
H18B H 0.524133 0.641837 0.664209 0.115 Uiso 1 1 calc R U . . .
C24 C 1.1513(4) 0.4777(6) 0.5552(4) 0.118(3) Uani 1 1 d . . . . .
H24A H 1.226968 0.476043 0.538794 0.142 Uiso 1 1 calc R U . . .
H24B H 1.127633 0.448685 0.514760 0.142 Uiso 1 1 calc R U . . .
C13 C 1.1084(4) 0.6288(6) 0.5051(3) 0.106(2) Uani 1 1 d . . . . .
H13A H 1.095959 0.598930 0.460293 0.128 Uiso 1 1 calc R U . . .
H13B H 1.181972 0.635446 0.495264 0.128 Uiso 1 1 calc R U . . .
C14 C 1.0336(6) 0.7229(5) 0.5212(3) 0.107(2) Uani 1 1 d . . . . .
H14A H 1.043444 0.751227 0.567611 0.129 Uiso 1 1 calc R U . . .
H14B H 1.048206 0.764668 0.480075 0.129 Uiso 1 1 calc R U . . .
C22 C 1.0084(7) 0.3599(4) 0.7056(4) 0.127(3) Uani 1 1 d . . . . .
H22A H 1.007111 0.395394 0.751788 0.153 Uiso 1 1 calc R U . . .
H22B H 1.064298 0.300567 0.701999 0.153 Uiso 1 1 calc R U . . .
C12 C 0.9261(4) 0.3869(4) 1.0042(3) 0.0879(15) Uani 1 1 d . . . . .
C21 C 0.9041(7) 0.3398(4) 0.7061(4) 0.116(2) Uani 1 1 d . . . . .
H21A H 0.906133 0.304719 0.659473 0.139 Uiso 1 1 calc R U . . .
H21B H 0.887699 0.300408 0.748452 0.139 Uiso 1 1 calc R U . . .
O12 O 0.5779(3) 0.8593(2) 1.0524(2) 0.0882(10) Uani 1 1 d . . . . .
O10 O 0.3602(4) 0.8545(3) 0.8684(3) 0.1212(15) Uani 1 1 d . . . . .
O11 O 0.3899(4) 0.8335(4) 1.0112(3) 0.1239(16) Uani 1 1 d . . . . .
O8 O 0.7117(4) 0.9224(3) 0.8067(3) 0.1098(13) Uani 1 1 d . . . . .
O13 O 0.7562(10) 0.8629(7) 0.9486(6) 0.077(3) Uani 0.534(13) 1 d . . P A 1
O9 O 0.5282(5) 0.8953(4) 0.7598(3) 0.1262(16) Uani 1 1 d . . . . .
C35 C 0.4057(6) 0.8382(5) 1.0845(4) 0.113(2) Uani 1 1 d . . . . .
H35A H 0.365326 0.797731 1.113947 0.135 Uiso 0.534(13) 1 calc R U P A 1
H35B H 0.373461 0.903484 1.104240 0.135 Uiso 0.534(13) 1 calc R U P A 1
H35C H 0.431641 0.773345 1.100119 0.135 Uiso 0.466(13) 1 calc R U P A 2
H35D H 0.336639 0.865593 1.116997 0.135 Uiso 0.466(13) 1 calc R U P A 2
C40 C 0.8126(5) 0.8982(5) 0.8260(5) 0.114(2) Uani 1 1 d . . . . .
H40A H 0.844901 0.831262 0.810853 0.137 Uiso 1 1 calc R U . . .
H40B H 0.856471 0.935390 0.795856 0.137 Uiso 1 1 calc R U . . .
C30 C 0.5942(8) 0.9515(5) 0.7210(4) 0.133(3) Uani 1 1 d . . . . .
H30A H 0.595758 0.946202 0.666813 0.159 Uiso 1 1 calc R U . . .
H30B H 0.564560 1.018343 0.737620 0.159 Uiso 1 1 calc R U . . .
C34 C 0.3049(6) 0.8183(6) 0.9940(6) 0.137(3) Uani 1 1 d . . . . .
H34A H 0.244344 0.866726 1.021362 0.164 Uiso 1 1 calc R U . . .
H34B H 0.297759 0.756957 1.013914 0.164 Uiso 1 1 calc R U . . .
C29 C 0.7001(8) 0.9205(6) 0.7355(5) 0.140(3) Uani 1 1 d . . . . .
H29A H 0.729860 0.855260 0.714958 0.168 Uiso 1 1 calc R U . . .
H29B H 0.743238 0.959961 0.707601 0.168 Uiso 1 1 calc R U . . .
C38 C 0.7463(18) 0.8881(15) 1.0263(10) 0.088(6) Uani 0.534(13) 1 d . . P A 1
H38A H 0.817246 0.876136 1.039548 0.106 Uiso 0.534(13) 1 calc R U P A 1
H38B H 0.711566 0.955766 1.035817 0.106 Uiso 0.534(13) 1 calc R U P A 1
C31 C 0.4254(7) 0.9178(7) 0.7536(5) 0.149(3) Uani 1 1 d . . . . .
H31A H 0.422310 0.917213 0.699930 0.179 Uiso 1 1 calc R U . . .
H31B H 0.394146 0.983246 0.773461 0.179 Uiso 1 1 calc R U . . .
C39 C 0.8193(6) 0.9105(6) 0.9002(6) 0.133(3) Uani 1 1 d . . . . .
H39A H 0.796791 0.978418 0.914368 0.160 Uiso 0.534(13) 1 calc R U P A 1
H39B H 0.893832 0.887327 0.905894 0.160 Uiso 0.534(13) 1 calc R U P A 1
H39C H 0.878530 0.861239 0.912609 0.160 Uiso 0.466(13) 1 calc R U P A 2
H39D H 0.833555 0.972397 0.908151 0.160 Uiso 0.466(13) 1 calc R U P A 2
C33 C 0.2928(7) 0.8169(7) 0.9168(7) 0.171(4) Uani 1 1 d . . . . .
H33A H 0.301875 0.750881 0.900163 0.205 Uiso 1 1 calc R U . . .
H33B H 0.219602 0.851259 0.914102 0.205 Uiso 1 1 calc R U . . .
C32 C 0.3593(7) 0.8609(7) 0.7893(6) 0.165(4) Uani 1 1 d . . . . .
H32A H 0.383579 0.796925 0.765455 0.198 Uiso 1 1 calc R U . . .
H32B H 0.286012 0.887590 0.782075 0.198 Uiso 1 1 calc R U . . .
C37 C 0.6864(14) 0.8348(11) 1.0696(7) 0.110(5) Uani 0.534(13) 1 d . . P A 1
H37A H 0.683313 0.848348 1.123058 0.132 Uiso 0.534(13) 1 calc R U P A 1
H37B H 0.719314 0.767046 1.058414 0.132 Uiso 0.534(13) 1 calc R U P A 1
C36 C 0.5132(13) 0.8118(10) 1.0996(7) 0.123(6) Uani 0.534(13) 1 d . . P A 1
H36A H 0.512184 0.828335 1.152229 0.148 Uiso 0.534(13) 1 calc R U P A 1
H36B H 0.542175 0.743129 1.091291 0.148 Uiso 0.534(13) 1 calc R U P A 1
C37A C 0.6544(16) 0.9069(13) 1.0661(11) 0.117(6) Uani 0.466(13) 1 d . . P A 2
H37C H 0.672315 0.891330 1.115651 0.141 Uiso 0.466(13) 1 calc R U P A 2
H37D H 0.624644 0.975642 1.066185 0.141 Uiso 0.466(13) 1 calc R U P A 2
C36A C 0.4770(13) 0.8907(10) 1.0966(6) 0.093(5) Uani 0.466(13) 1 d . . P A 2
H36C H 0.447689 0.957225 1.086323 0.112 Uiso 0.466(13) 1 calc R U P A 2
H36D H 0.483687 0.888125 1.149661 0.112 Uiso 0.466(13) 1 calc R U P A 2
O13A O 0.7364(12) 0.9061(14) 0.9410(14) 0.148(8) Uani 0.466(13) 1 d . . P A 2
C38A C 0.749(4) 0.880(4) 1.009(3) 0.23(2) Uani 0.466(13) 1 d . . P A 2
H38C H 0.804381 0.907029 1.023568 0.270 Uiso 0.466(13) 1 calc R U P A 2
H38D H 0.775791 0.810424 1.007703 0.270 Uiso 0.466(13) 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
Ni2 S12 2.1605(10) . ?
Ni2 S12 2.1605(10) 2_666 ?
Ni2 S11 2.1565(11) . ?
Ni2 S11 2.1566(11) 2_666 ?
Ni1 S2 2.1505(10) . ?
Ni1 S7 2.1603(13) . ?
Ni1 S1 2.1680(13) . ?
Ni1 S6 2.1586(10) . ?
Ni3 S16 2.1541(13) 2_667 ?
Ni3 S16 2.1541(13) . ?
Ni3 S17 2.1531(12) 2_667 ?
Ni3 S17 2.1531(12) . ?
S2 C2 1.696(4) . ?
S12 C8 1.714(4) . ?
S7 C5 1.720(4) . ?
S11 C7 1.715(4) . ?
S1 C1 1.717(4) . ?
S4 C2 1.736(4) . ?
S4 C3 1.740(5) . ?
S6 C4 1.706(5) . ?
S3 C1 1.731(4) . ?
S3 C3 1.746(4) . ?
S14 C8 1.746(4) . ?
S14 C9 1.739(5) . ?
S13 C7 1.743(4) . ?
S13 C9 1.730(5) . ?
S16 C10 1.714(5) . ?
S8 C4 1.747(4) . ?
S8 C6 1.729(6) . ?
S9 C5 1.732(5) . ?
S9 C6 1.736(5) . ?
S15 C9 1.631(5) . ?
S17 C11 1.709(5) . ?
S5 C3 1.616(5) . ?
S18 C10 1.727(5) . ?
S18 C12 1.737(5) . ?
S10 C6 1.637(5) . ?
S19 C11 1.744(5) . ?
S19 C12 1.716(6) . ?
O7 C26 1.402(5) . ?
O7 C27 1.419(5) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N1 H1C 0.9000 . ?
N1 C25 1.478(5) . ?
S20 C12 1.631(6) . ?
O6 C17 1.432(6) . ?
O6 C16 1.373(6) . ?
N2 H2A 0.9000 . ?
N2 H2B 0.9000 . ?
N2 H2C 0.9000 . ?
N2 C28 1.483(5) . ?
O1 C19 1.435(6) . ?
O1 C18 1.377(7) . ?
O5 C15 1.427(6) . ?
O5 C14 1.382(6) . ?
O3 C23 1.456(7) . ?
O3 C22 1.405(8) . ?
O4 C24 1.367(8) . ?
O4 C13 1.454(7) . ?
O2 C20 1.394(6) . ?
O2 C21 1.444(7) . ?
C2 C1 1.376(5) . ?
C8 C7 1.356(6) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 C26 1.494(6) . ?
C5 C4 1.366(6) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 C28 1.483(6) . ?
C11 C10 1.366(6) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 C18 1.460(8) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 C20 1.473(8) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 C16 1.477(8) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 C24 1.488(10) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 C14 1.472(9) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 C21 1.470(9) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
O12 C37 1.474(15) . ?
O12 C36 1.397(14) . ?
O12 C37A 1.411(16) . ?
O12 C36A 1.389(14) . ?
O10 C33 1.344(10) . ?
O10 C32 1.435(10) . ?
O11 C35 1.383(8) . ?
O11 C34 1.283(9) . ?
O8 C40 1.395(7) . ?
O8 C29 1.325(9) . ?
O13 C38 1.43(2) . ?
O13 C39 1.396(13) . ?
O9 C30 1.428(8) . ?
O9 C31 1.337(9) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C35 H35D 0.9800 . ?
C35 C36 1.447(16) . ?
C35 C36A 1.393(15) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 C39 1.376(10) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 C29 1.427(11) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 C33 1.435(12) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 C37 1.38(3) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 C32 1.416(11) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C39 H39D 0.9800 . ?
C39 O13A 1.217(17) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C37A H37C 0.9800 . ?
C37A H37D 0.9800 . ?
C37A C38A 1.44(5) . ?
C36A H36C 0.9800 . ?
C36A H36D 0.9800 . ?
O13A C38A 1.32(6) . ?
C38A H38C 0.9800 . ?
C38A H38D 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
S12 Ni2 S12 180.0 . 2_666 ?
S11 Ni2 S12 86.65(4) . 2_666 ?
S11 Ni2 S12 93.35(4) . . ?
S11 Ni2 S12 86.65(4) 2_666 . ?
S11 Ni2 S12 93.35(4) 2_666 2_666 ?
S11 Ni2 S11 180.0 . 2_666 ?
S2 Ni1 S7 85.43(4) . . ?
S2 Ni1 S1 93.30(4) . . ?
S2 Ni1 S6 178.51(5) . . ?
S7 Ni1 S1 176.81(5) . . ?
S6 Ni1 S7 93.15(5) . . ?
S6 Ni1 S1 88.09(4) . . ?
S16 Ni3 S16 180.0 . 2_667 ?
S17 Ni3 S16 93.54(5) 2_667 2_667 ?
S17 Ni3 S16 86.46(5) 2_667 . ?
S17 Ni3 S16 86.46(5) . 2_667 ?
S17 Ni3 S16 93.54(5) . . ?
S17 Ni3 S17 180.0 2_667 . ?
C2 S2 Ni1 102.47(12) . . ?
C8 S12 Ni2 101.99(15) . . ?
C5 S7 Ni1 102.17(17) . . ?
C7 S11 Ni2 101.95(14) . . ?
C1 S1 Ni1 101.89(14) . . ?
C2 S4 C3 98.4(2) . . ?
C4 S6 Ni1 102.17(14) . . ?
C1 S3 C3 98.2(2) . . ?
C9 S14 C8 97.4(2) . . ?
C9 S13 C7 97.7(2) . . ?
C10 S16 Ni3 102.21(16) . . ?
C6 S8 C4 98.0(2) . . ?
C5 S9 C6 97.0(3) . . ?
C11 S17 Ni3 101.86(16) . . ?
C10 S18 C12 97.5(2) . . ?
C12 S19 C11 97.9(2) . . ?
C26 O7 C27 111.7(3) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C25 N1 H1A 109.5 . . ?
C25 N1 H1B 109.5 . . ?
C25 N1 H1C 109.5 . . ?
C16 O6 C17 112.9(4) . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C28 N2 H2A 109.5 . . ?
C28 N2 H2B 109.5 . . ?
C28 N2 H2C 109.5 . . ?
C18 O1 C19 111.8(4) . . ?
C14 O5 C15 113.8(5) . . ?
C22 O3 C23 113.6(5) . . ?
C24 O4 C13 113.1(5) . . ?
C20 O2 C21 113.5(5) . . ?
S2 C2 S4 122.7(2) . . ?
C1 C2 S2 121.7(3) . . ?
C1 C2 S4 115.6(3) . . ?
S12 C8 S14 122.6(2) . . ?
C7 C8 S12 121.2(3) . . ?
C7 C8 S14 116.2(3) . . ?
S11 C7 S13 122.6(2) . . ?
C8 C7 S11 121.5(3) . . ?
C8 C7 S13 115.9(3) . . ?
S1 C1 S3 123.4(2) . . ?
C2 C1 S1 120.5(3) . . ?
C2 C1 S3 116.0(3) . . ?
N1 C25 H25A 109.0 . . ?
N1 C25 H25B 109.0 . . ?
N1 C25 C26 112.9(3) . . ?
H25A C25 H25B 107.8 . . ?
C26 C25 H25A 109.0 . . ?
C26 C25 H25B 109.0 . . ?
S7 C5 S9 122.0(3) . . ?
C4 C5 S7 120.5(4) . . ?
C4 C5 S9 117.4(3) . . ?
S6 C4 S8 123.8(3) . . ?
C5 C4 S6 121.7(3) . . ?
C5 C4 S8 114.5(4) . . ?
O7 C26 C25 109.6(3) . . ?
O7 C26 H26A 109.8 . . ?
O7 C26 H26B 109.8 . . ?
C25 C26 H26A 109.8 . . ?
C25 C26 H26B 109.8 . . ?
H26A C26 H26B 108.2 . . ?
S13 C9 S14 112.7(3) . . ?
S15 C9 S14 123.7(3) . . ?
S15 C9 S13 123.5(3) . . ?
S4 C3 S3 111.8(3) . . ?
S5 C3 S4 123.1(3) . . ?
S5 C3 S3 125.2(3) . . ?
O7 C27 H27A 109.7 . . ?
O7 C27 H27B 109.7 . . ?
O7 C27 C28 109.6(4) . . ?
H27A C27 H27B 108.2 . . ?
C28 C27 H27A 109.7 . . ?
C28 C27 H27B 109.7 . . ?
S17 C11 S19 123.0(3) . . ?
C10 C11 S17 121.8(4) . . ?
C10 C11 S19 115.2(4) . . ?
N2 C28 H28A 109.1 . . ?
N2 C28 H28B 109.1 . . ?
C27 C28 N2 112.7(4) . . ?
C27 C28 H28A 109.1 . . ?
C27 C28 H28B 109.1 . . ?
H28A C28 H28B 107.8 . . ?
S8 C6 S9 113.0(3) . . ?
S10 C6 S8 124.4(3) . . ?
S10 C6 S9 122.6(4) . . ?
S16 C10 S18 123.0(3) . . ?
C11 C10 S16 120.6(4) . . ?
C11 C10 S18 116.4(4) . . ?
O6 C17 H17A 109.7 . . ?
O6 C17 H17B 109.7 . . ?
O6 C17 C18 109.8(4) . . ?
H17A C17 H17B 108.2 . . ?
C18 C17 H17A 109.7 . . ?
C18 C17 H17B 109.7 . . ?
O1 C19 H19A 109.8 . . ?
O1 C19 H19B 109.8 . . ?
O1 C19 C20 109.4(4) . . ?
H19A C19 H19B 108.2 . . ?
C20 C19 H19A 109.8 . . ?
C20 C19 H19B 109.8 . . ?
O5 C15 H15A 109.6 . . ?
O5 C15 H15B 109.6 . . ?
O5 C15 C16 110.1(4) . . ?
H15A C15 H15B 108.2 . . ?
C16 C15 H15A 109.6 . . ?
C16 C15 H15B 109.6 . . ?
O3 C23 H23A 109.8 . . ?
O3 C23 H23B 109.8 . . ?
O3 C23 C24 109.5(4) . . ?
H23A C23 H23B 108.2 . . ?
C24 C23 H23A 109.8 . . ?
C24 C23 H23B 109.8 . . ?
O2 C20 C19 109.1(4) . . ?
O2 C20 H20A 109.9 . . ?
O2 C20 H20B 109.9 . . ?
C19 C20 H20A 109.9 . . ?
C19 C20 H20B 109.9 . . ?
H20A C20 H20B 108.3 . . ?
O6 C16 C15 110.6(5) . . ?
O6 C16 H16A 109.5 . . ?
O6 C16 H16B 109.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 108.1 . . ?
O1 C18 C17 109.7(5) . . ?
O1 C18 H18A 109.7 . . ?
O1 C18 H18B 109.7 . . ?
C17 C18 H18A 109.7 . . ?
C17 C18 H18B 109.7 . . ?
H18A C18 H18B 108.2 . . ?
O4 C24 C23 110.3(5) . . ?
O4 C24 H24A 109.6 . . ?
O4 C24 H24B 109.6 . . ?
C23 C24 H24A 109.6 . . ?
C23 C24 H24B 109.6 . . ?
H24A C24 H24B 108.1 . . ?
O4 C13 H13A 109.7 . . ?
O4 C13 H13B 109.7 . . ?
O4 C13 C14 109.6(5) . . ?
H13A C13 H13B 108.2 . . ?
C14 C13 H13A 109.7 . . ?
C14 C13 H13B 109.7 . . ?
O5 C14 C13 110.0(5) . . ?
O5 C14 H14A 109.7 . . ?
O5 C14 H14B 109.7 . . ?
C13 C14 H14A 109.7 . . ?
C13 C14 H14B 109.7 . . ?
H14A C14 H14B 108.2 . . ?
O3 C22 H22A 110.4 . . ?
O3 C22 H22B 110.4 . . ?
O3 C22 C21 106.6(5) . . ?
H22A C22 H22B 108.6 . . ?
C21 C22 H22A 110.4 . . ?
C21 C22 H22B 110.4 . . ?
S19 C12 S18 113.0(3) . . ?
S20 C12 S18 123.0(3) . . ?
S20 C12 S19 124.1(3) . . ?
O2 C21 C22 109.8(5) . . ?
O2 C21 H21A 109.7 . . ?
O2 C21 H21B 109.7 . . ?
C22 C21 H21A 109.7 . . ?
C22 C21 H21B 109.7 . . ?
H21A C21 H21B 108.2 . . ?
C36 O12 C37 109.9(9) . . ?
C36A O12 C37A 115.5(11) . . ?
C33 O10 C32 124.1(7) . . ?
C34 O11 C35 123.3(6) . . ?
C29 O8 C40 121.2(6) . . ?
C39 O13 C38 113.6(12) . . ?
C31 O9 C30 117.3(6) . . ?
O11 C35 H35A 107.5 . . ?
O11 C35 H35B 107.5 . . ?
O11 C35 H35C 108.4 . . ?
O11 C35 H35D 108.4 . . ?
O11 C35 C36 119.4(7) . . ?
O11 C35 C36A 115.5(7) . . ?
H35A C35 H35B 107.0 . . ?
H35C C35 H35D 107.5 . . ?
C36 C35 H35A 107.5 . . ?
C36 C35 H35B 107.5 . . ?
C36A C35 H35C 108.4 . . ?
C36A C35 H35D 108.4 . . ?
O8 C40 H40A 107.8 . . ?
O8 C40 H40B 107.8 . . ?
H40A C40 H40B 107.1 . . ?
C39 C40 O8 118.0(6) . . ?
C39 C40 H40A 107.8 . . ?
C39 C40 H40B 107.8 . . ?
O9 C30 H30A 109.6 . . ?
O9 C30 H30B 109.6 . . ?
H30A C30 H30B 108.1 . . ?
C29 C30 O9 110.2(5) . . ?
C29 C30 H30A 109.6 . . ?
C29 C30 H30B 109.6 . . ?
O11 C34 H34A 107.3 . . ?
O11 C34 H34B 107.3 . . ?
O11 C34 C33 120.2(7) . . ?
H34A C34 H34B 106.9 . . ?
C33 C34 H34A 107.3 . . ?
C33 C34 H34B 107.3 . . ?
O8 C29 C30 117.1(7) . . ?
O8 C29 H29A 108.0 . . ?
O8 C29 H29B 108.0 . . ?
C30 C29 H29A 108.0 . . ?
C30 C29 H29B 108.0 . . ?
H29A C29 H29B 107.3 . . ?
O13 C38 H38A 109.8 . . ?
O13 C38 H38B 109.8 . . ?
H38A C38 H38B 108.3 . . ?
C37 C38 O13 109.3(13) . . ?
C37 C38 H38A 109.8 . . ?
C37 C38 H38B 109.8 . . ?
O9 C31 H31A 107.7 . . ?
O9 C31 H31B 107.7 . . ?
O9 C31 C32 118.3(7) . . ?
H31A C31 H31B 107.1 . . ?
C32 C31 H31A 107.7 . . ?
C32 C31 H31B 107.7 . . ?
O13 C39 H39A 109.1 . . ?
O13 C39 H39B 109.1 . . ?
C40 C39 O13 112.5(7) . . ?
C40 C39 H39A 109.1 . . ?
C40 C39 H39B 109.1 . . ?
C40 C39 H39C 109.6 . . ?
C40 C39 H39D 109.6 . . ?
H39A C39 H39B 107.8 . . ?
H39C C39 H39D 108.1 . . ?
O13A C39 C40 110.3(13) . . ?
O13A C39 H39C 109.6 . . ?
O13A C39 H39D 109.6 . . ?
O10 C33 C34 116.0(6) . . ?
O10 C33 H33A 108.3 . . ?
O10 C33 H33B 108.3 . . ?
C34 C33 H33A 108.3 . . ?
C34 C33 H33B 108.3 . . ?
H33A C33 H33B 107.4 . . ?
O10 C32 H32A 109.1 . . ?
O10 C32 H32B 109.1 . . ?
C31 C32 O10 112.6(7) . . ?
C31 C32 H32A 109.1 . . ?
C31 C32 H32B 109.1 . . ?
H32A C32 H32B 107.8 . . ?
O12 C37 H37A 110.0 . . ?
O12 C37 H37B 110.0 . . ?
C38 C37 O12 108.7(11) . . ?
C38 C37 H37A 110.0 . . ?
C38 C37 H37B 110.0 . . ?
H37A C37 H37B 108.3 . . ?
O12 C36 C35 110.0(9) . . ?
O12 C36 H36A 109.7 . . ?
O12 C36 H36B 109.7 . . ?
C35 C36 H36A 109.7 . . ?
C35 C36 H36B 109.7 . . ?
H36A C36 H36B 108.2 . . ?
O12 C37A H37C 109.6 . . ?
O12 C37A H37D 109.6 . . ?
O12 C37A C38A 110(2) . . ?
H37C C37A H37D 108.1 . . ?
C38A C37A H37C 109.6 . . ?
C38A C37A H37D 109.6 . . ?
O12 C36A C35 113.7(9) . . ?
O12 C36A H36C 108.8 . . ?
O12 C36A H36D 108.8 . . ?
C35 C36A H36C 108.8 . . ?
C35 C36A H36D 108.8 . . ?
H36C C36A H36D 107.7 . . ?
C39 O13A C38A 113(3) . . ?
C37A C38A H38C 108.6 . . ?
C37A C38A H38D 108.6 . . ?
O13A C38A C37A 115(4) . . ?
O13A C38A H38C 108.6 . . ?
O13A C38A H38D 108.6 . . ?
H38C C38A H38D 107.6 . . ?

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
Ni2 S12 C8 S14 179.8(2) . . . . ?
Ni2 S12 C8 C7 0.2(3) . . . . ?
Ni2 S11 C7 S13 -179.9(2) . . . . ?
Ni2 S11 C7 C8 -1.4(3) . . . . ?
Ni1 S2 C2 S4 179.3(2) . . . . ?
Ni1 S2 C2 C1 -1.0(3) . . . . ?
Ni1 S7 C5 S9 -175.1(2) . . . . ?
Ni1 S7 C5 C4 3.9(4) . . . . ?
Ni1 S1 C1 S3 -176.5(2) . . . . ?
Ni1 S1 C1 C2 2.9(3) . . . . ?
Ni1 S6 C4 S8 176.7(2) . . . . ?
Ni1 S6 C4 C5 -3.2(4) . . . . ?
Ni3 S16 C10 S18 -178.5(2) . . . . ?
Ni3 S16 C10 C11 0.4(4) . . . . ?
Ni3 S17 C11 S19 179.1(3) . . . . ?
Ni3 S17 C11 C10 -1.9(4) . . . . ?
S2 C2 C1 S1 -1.4(5) . . . . ?
S2 C2 C1 S3 178.0(2) . . . . ?
S12 C8 C7 S11 0.8(5) . . . . ?
S12 C8 C7 S13 179.4(2) . . . . ?
S7 C5 C4 S6 -0.5(5) . . . . ?
S7 C5 C4 S8 179.6(2) . . . . ?
S4 C2 C1 S1 178.3(2) . . . . ?
S4 C2 C1 S3 -2.3(4) . . . . ?
S14 C8 C7 S11 -178.8(2) . . . . ?
S14 C8 C7 S13 -0.2(4) . . . . ?
S9 C5 C4 S6 178.5(2) . . . . ?
S9 C5 C4 S8 -1.4(4) . . . . ?
S17 C11 C10 S16 1.1(6) . . . . ?
S17 C11 C10 S18 -179.9(2) . . . . ?
S19 C11 C10 S16 -179.8(2) . . . . ?
S19 C11 C10 S18 -0.8(5) . . . . ?
O7 C27 C28 N2 -69.0(5) . . . . ?
N1 C25 C26 O7 -69.4(4) . . . . ?
O6 C17 C18 O1 -65.7(6) . . . . ?
O1 C19 C20 O2 65.8(5) . . . . ?
O5 C15 C16 O6 60.4(6) . . . . ?
O3 C23 C24 O4 67.2(6) . . . . ?
O3 C22 C21 O2 -61.0(6) . . . . ?
O4 C13 C14 O5 -64.5(6) . . . . ?
C2 S4 C3 S3 -1.4(3) . . . . ?
C2 S4 C3 S5 177.5(3) . . . . ?
C8 S14 C9 S13 -2.5(3) . . . . ?
C8 S14 C9 S15 176.9(3) . . . . ?
C7 S13 C9 S14 2.4(3) . . . . ?
C7 S13 C9 S15 -177.0(3) . . . . ?
C1 S3 C3 S4 0.4(3) . . . . ?
C1 S3 C3 S5 -178.5(3) . . . . ?
C5 S9 C6 S8 2.2(3) . . . . ?
C5 S9 C6 S10 -179.6(3) . . . . ?
C4 S8 C6 S9 -2.8(3) . . . . ?
C4 S8 C6 S10 179.0(3) . . . . ?
C26 O7 C27 C28 -179.4(3) . . . . ?
C9 S14 C8 S12 -178.0(2) . . . . ?
C9 S14 C8 C7 1.7(3) . . . . ?
C9 S13 C7 S11 177.2(2) . . . . ?
C9 S13 C7 C8 -1.4(3) . . . . ?
C3 S4 C2 S2 -178.1(3) . . . . ?
C3 S4 C2 C1 2.2(3) . . . . ?
C3 S3 C1 S1 -179.4(3) . . . . ?
C3 S3 C1 C2 1.1(3) . . . . ?
C27 O7 C26 C25 -177.6(3) . . . . ?
C11 S19 C12 S18 0.0(4) . . . . ?
C11 S19 C12 S20 179.1(4) . . . . ?
C6 S8 C4 S6 -177.3(3) . . . . ?
C6 S8 C4 C5 2.5(4) . . . . ?
C6 S9 C5 S7 178.5(3) . . . . ?
C6 S9 C5 C4 -0.5(4) . . . . ?
C10 S18 C12 S19 -0.3(4) . . . . ?
C10 S18 C12 S20 -179.4(4) . . . . ?
C17 O6 C16 C15 -173.1(5) . . . . ?
C19 O1 C18 C17 -175.1(4) . . . . ?
C15 O5 C14 C13 -174.2(5) . . . . ?
C23 O3 C22 C21 -167.5(5) . . . . ?
C20 O2 C21 C22 173.7(5) . . . . ?
C16 O6 C17 C18 -178.4(5) . . . . ?
C18 O1 C19 C20 175.1(4) . . . . ?
C24 O4 C13 C14 173.0(4) . . . . ?
C13 O4 C24 C23 176.3(4) . . . . ?
C14 O5 C15 C16 175.2(5) . . . . ?
C22 O3 C23 C24 177.7(5) . . . . ?
C12 S18 C10 S16 179.7(3) . . . . ?
C12 S18 C10 C11 0.7(4) . . . . ?
C12 S19 C11 S17 179.6(3) . . . . ?
C12 S19 C11 C10 0.5(4) . . . . ?
C21 O2 C20 C19 177.1(4) . . . . ?
O12 C37A C38A O13A 66(5) . . . . ?
O11 C35 C36 O12 50.4(14) . . . . ?
O11 C35 C36A O12 -57.2(14) . . . . ?
O11 C34 C33 O10 -15.7(14) . . . . ?
O8 C40 C39 O13 55.5(11) . . . . ?
O8 C40 C39 O13A 26.1(15) . . . . ?
O13 C38 C37 O12 -63.5(18) . . . . ?
O9 C30 C29 O8 -58.6(10) . . . . ?
O9 C31 C32 O10 56.0(12) . . . . ?
C35 O11 C34 C33 178.3(8) . . . . ?
C40 O8 C29 C30 -176.6(6) . . . . ?
C40 C39 O13A C38A 155(3) . . . . ?
C30 O9 C31 C32 177.7(8) . . . . ?
C34 O11 C35 C36 151.5(10) . . . . ?
C34 O11 C35 C36A -155.2(10) . . . . ?
C29 O8 C40 C39 173.8(7) . . . . ?
C38 O13 C39 C40 -169.3(11) . . . . ?
C31 O9 C30 C29 177.9(7) . . . . ?
C39 O13 C38 C37 -177.6(13) . . . . ?
C39 O13A C38A C37A 158(3) . . . . ?
C33 O10 C32 C31 169.7(8) . . . . ?
C32 O10 C33 C34 -179.0(8) . . . . ?
C37 O12 C36 C35 178.1(10) . . . . ?
C36 O12 C37 C38 -175.4(12) . . . . ?
C37A O12 C36A C35 -176.3(11) . . . . ?
C36A O12 C37A C38A -170(3) . . . . ?

_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 2.945
_oxdiff_exptl_absorpt_empirical_full_min 0.551
####################################################################### 
# 
# 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_exp_1088_07_213_00_auto
_database_code_depnum_ccdc_archive 'CCDC 2384658'
loop_
_audit_author_name
_audit_author_address
'Kiyonori Takahashi'
;Hokkaido University
Japan
;
_audit_update_record             
;
2024-09-17 deposited with the CCDC.	2024-11-08 downloaded from the CCDC.
;
_audit_creation_date             2023-09-12
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '4(C3 Ni0.5 S5), C4 H14 N2 O, 2(C12 H24 O6)'
_chemical_formula_sum            'C40 H62 N2 Ni2 O13 S20'
_chemical_formula_weight         1537.53
_chemical_melting_point          ?
_chemical_oxdiff_formula         C24H32N2O6NiS10
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                   13.1444(3)
_cell_length_b                   14.5178(5)
_cell_length_c                   18.1193(5)
_cell_angle_alpha                89.995(2)
_cell_angle_beta                 79.591(2)
_cell_angle_gamma                75.671(2)
_cell_volume                     3291.35(17)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    17936
_cell_measurement_temperature    212.9(3)
_cell_measurement_theta_max      29.3570
_cell_measurement_theta_min      1.4670
_shelx_estimated_absorpt_T_max   0.792
_shelx_estimated_absorpt_T_min   0.403
_exptl_absorpt_coefficient_mu    1.260
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86125
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.67a (Rigaku Oxford Diffraction, 2022)
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    1.551
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.881
_exptl_crystal_size_mid          0.545
_exptl_crystal_size_min          0.194
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            37421
_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         26.373
_diffrn_reflns_theta_min         1.628
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      212.9(3)
_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    -94.00 -69.00   0.50    1.20    --  -20.89 153.00-153.00   50
  2  ω   -112.00 -57.00   0.50    1.20    --  -20.89-153.00 165.00  110
  3  ω    -65.00 -39.00   0.50    1.20    --  -20.89 120.00  48.00   52
  4  ω     42.00 102.00   0.50    1.20    --   21.12-153.00 165.00  120
  5  ω     23.00  76.00   0.50    1.20    --   21.12-120.00 -35.00  106
  6  ω     31.00  56.00   0.50    1.20    --  -20.89  19.00-180.00   50
  7  ω    -22.00  59.00   0.50    1.20    --  -20.89  19.00  30.00  162
  8  ω    -24.00  60.00   0.50    1.20    --  -20.89  19.00 -30.00  168
  9  ω    -17.00  36.00   0.50    1.20    --  -20.89 -99.00 120.00  106
 10  ω    -24.00  10.00   0.50    1.20    --  -20.89  19.00-180.00   68
 11  ω     60.00  86.00   0.50    1.20    --   21.12 178.00-150.00   52
 12  ω    -65.00  28.00   0.50    1.20    --   21.12 -19.00  30.00  186
 13  ω    -74.00  23.00   0.50    1.20    --   21.12 -19.00-180.00  194
;
_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      0.0027892000
_diffrn_orient_matrix_UB_12      0.0016613000
_diffrn_orient_matrix_UB_13      -0.0394219000
_diffrn_orient_matrix_UB_21      0.0210424000
_diffrn_orient_matrix_UB_22      -0.0500655000
_diffrn_orient_matrix_UB_23      -0.0037388000
_diffrn_orient_matrix_UB_31      -0.0525656000
_diffrn_orient_matrix_UB_32      -0.0062519000
_diffrn_orient_matrix_UB_33      0.0044222000
_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                9079
_reflns_number_total             13452
_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 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.762
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     736
_refine_ls_number_reflns         13452
_refine_ls_number_restraints     28
_refine_ls_R_factor_all          0.0871
_refine_ls_R_factor_gt           0.0551
_refine_ls_restrained_S_all      1.040
_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)+(0.0630P)²+3.9293P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1367
_refine_ls_wR_factor_ref         0.1557
_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
 C38A-C37A \\sim C38-C37
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O13A \\sim C38A \\sim C37A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C32 \\sim O10 \\sim C33: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 2A
4. Rigid body (RIGU) restrains
 O13A, C39
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H35C)=Sof(H35D)=Sof(H39C)=Sof(H39D)=Sof(C37A)=Sof(H37C)=Sof(H37D)=
 Sof(C36A)=Sof(H36C)=Sof(H36D)=Sof(O13A)=Sof(C38A)=Sof(H38C)=Sof(H38D)=1-FVAR(1)
 Sof(O13)=Sof(H35A)=Sof(H35B)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H39A)=Sof(H39B)=
 Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C36)=Sof(H36A)=Sof(H36B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C17(H17A,
 H17B), C19(H19A,H19B), C15(H15A,H15B), C23(H23A,H23B), C20(H20A,H20B),
 C16(H16A,H16B), C18(H18A,H18B), C24(H24A,H24B), C13(H13A,H13B), C14(H14A,H14B),
  C22(H22A,H22B), C21(H21A,H21B), C35(H35A,H35B), C35(H35C,H35D), C40(H40A,
 H40B), C30(H30A,H30B), C34(H34A,H34B), C29(H29A,H29B), C38(H38A,H38B),
 C31(H31A,H31B), C39(H39A,H39B), C39(H39C,H39D), C33(H33A,H33B), C32(H32A,H32B),
  C37(H37A,H37B), C36(H36A,H36B), C37A(H37C,H37D), C36A(H36C,H36D), C38A(H38C,
 H38D)
6.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(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
Ni2 Ni 0.500000 0.500000 0.500000 0.0480(2) Uani 1 2 d S . P . .
Ni1 Ni 0.29924(4) 0.92175(4) 0.48522(3) 0.04630(15) Uani 1 1 d . . . . .
Ni3 Ni 0.500000 0.500000 0.000000 0.0575(2) Uani 1 2 d S . P . .
S2 S 0.46981(8) 0.90261(8) 0.46032(7) 0.0509(3) Uani 1 1 d . . . . .
S12 S 0.57787(9) 0.52981(8) 0.39029(7) 0.0566(3) Uani 1 1 d . . . . .
S7 S 0.30421(8) 0.99906(8) 0.58564(7) 0.0545(3) Uani 1 1 d . . . . .
S11 S 0.59010(9) 0.35312(8) 0.49138(7) 0.0569(3) Uani 1 1 d . . . . .
S1 S 0.29898(8) 0.83713(8) 0.38670(7) 0.0542(3) Uani 1 1 d . . . . .
S4 S 0.63904(8) 0.78943(8) 0.33601(7) 0.0564(3) Uani 1 1 d . . . . .
S6 S 0.12817(8) 0.94190(9) 0.51307(8) 0.0577(3) Uani 1 1 d . . . . .
S3 S 0.48402(10) 0.72292(9) 0.27069(8) 0.0651(3) Uani 1 1 d . . . . .
S14 S 0.74843(10) 0.40209(10) 0.27256(8) 0.0658(3) Uani 1 1 d . . . . .
S13 S 0.75917(10) 0.23946(9) 0.36532(8) 0.0663(3) Uani 1 1 d . . . . .
S16 S 0.63692(11) 0.42648(10) -0.08151(7) 0.0673(3) Uani 1 1 d . . . . .
S8 S -0.03120(10) 1.02820(10) 0.65462(9) 0.0754(4) Uani 1 1 d . . . . .
S9 S 0.13294(11) 1.07723(10) 0.72154(9) 0.0732(4) Uani 1 1 d . . . . .
S15 S 0.90769(11) 0.21953(12) 0.21880(10) 0.0857(5) Uani 1 1 d . . . . .
S17 S 0.59351(11) 0.50876(11) 0.08460(7) 0.0725(4) Uani 1 1 d . . . . .
S5 S 0.71610(12) 0.65558(13) 0.20354(10) 0.0933(5) Uani 1 1 d . . . . .
S18 S 0.87235(12) 0.36870(10) -0.07345(8) 0.0736(4) Uani 1 1 d . . . . .
S10 S -0.08750(15) 1.11748(11) 0.80959(12) 0.1064(7) Uani 1 1 d . . . . .
S19 S 0.83310(12) 0.44393(14) 0.07905(8) 0.0876(5) Uani 1 1 d . . . . .
O7 O 0.7603(2) 0.6731(2) 0.80797(17) 0.0528(7) Uani 1 1 d . . . . .
N1 N 0.8810(3) 0.5997(2) 0.65613(19) 0.0472(8) Uani 1 1 d . . . . .
H1A H 0.901633 0.621893 0.610953 0.057 Uiso 1 1 calc R U . . .
H1B H 0.809256 0.611368 0.666469 0.057 Uiso 1 1 calc R U . . .
H1C H 0.909849 0.536632 0.655483 0.057 Uiso 1 1 calc R U . . .
S20 S 1.05536(15) 0.35508(19) 0.00366(12) 0.1233(8) Uani 1 1 d . . . . .
O6 O 0.7148(3) 0.7348(2) 0.5985(2) 0.0690(9) Uani 1 1 d . . . . .
N2 N 0.5752(3) 0.8127(3) 0.8971(2) 0.0559(9) Uani 1 1 d . . . . .
H2A H 0.607178 0.830744 0.853282 0.067 Uiso 1 1 calc R U . . .
H2B H 0.601108 0.832818 0.935079 0.067 Uiso 1 1 calc R U . . .
H2C H 0.504230 0.838280 0.903795 0.067 Uiso 1 1 calc R U . . .
O1 O 0.6701(3) 0.5675(3) 0.6577(2) 0.0679(9) Uani 1 1 d . . . . .
O5 O 0.9271(3) 0.7158(3) 0.5289(2) 0.0718(10) Uani 1 1 d . . . . .
O3 O 1.0306(3) 0.4148(3) 0.6411(2) 0.0812(11) Uani 1 1 d . . . . .
O4 O 1.0927(3) 0.5717(3) 0.5682(2) 0.0799(11) Uani 1 1 d . . . . .
O2 O 0.8247(3) 0.4272(2) 0.7125(2) 0.0740(10) Uani 1 1 d . . . . .
C2 C 0.5072(3) 0.8298(3) 0.3814(3) 0.0468(10) Uani 1 1 d . . . . .
C8 C 0.6634(3) 0.4211(3) 0.3601(3) 0.0528(11) Uani 1 1 d . . . . .
C7 C 0.6678(3) 0.3448(3) 0.4036(3) 0.0528(11) Uani 1 1 d . . . . .
C1 C 0.4331(3) 0.7995(3) 0.3495(3) 0.0497(10) Uani 1 1 d . . . . .
C25 C 0.9175(4) 0.6480(3) 0.7145(3) 0.0596(12) Uani 1 1 d . . . . .
H25A H 0.898095 0.716828 0.708198 0.071 Uiso 1 1 calc R U . . .
H25B H 0.995634 0.627117 0.707442 0.071 Uiso 1 1 calc R U . . .
C5 C 0.1735(4) 1.0231(3) 0.6324(3) 0.0577(12) Uani 1 1 d . . . . .
C4 C 0.0974(3) 0.9984(3) 0.5998(3) 0.0575(12) Uani 1 1 d . . . . .
C26 C 0.8706(4) 0.6283(3) 0.7927(3) 0.0594(12) Uani 1 1 d . . . . .
H26A H 0.881473 0.559487 0.797804 0.071 Uiso 1 1 calc R U . . .
H26B H 0.906206 0.652370 0.828784 0.071 Uiso 1 1 calc R U . . .
C9 C 0.8110(4) 0.2830(4) 0.2817(3) 0.0656(13) Uani 1 1 d . . . . .
C3 C 0.6193(4) 0.7186(3) 0.2651(3) 0.0632(13) Uani 1 1 d . . . . .
C27 C 0.7126(4) 0.6596(3) 0.8828(3) 0.0624(12) Uani 1 1 d . . . . .
H27A H 0.746708 0.686433 0.918401 0.075 Uiso 1 1 calc R U . . .
H27B H 0.722867 0.591394 0.890838 0.075 Uiso 1 1 calc R U . . .
C11 C 0.7205(4) 0.4561(4) 0.0382(3) 0.0621(12) Uani 1 1 d . . . . .
C28 C 0.5966(4) 0.7072(3) 0.8956(3) 0.0681(13) Uani 1 1 d . . . . .
H28A H 0.561814 0.687908 0.943519 0.082 Uiso 1 1 calc R U . . .
H28B H 0.565213 0.685878 0.855694 0.082 Uiso 1 1 calc R U . . .
C6 C -0.0007(4) 1.0755(3) 0.7330(3) 0.0761(16) Uani 1 1 d . . . . .
C10 C 0.7394(4) 0.4202(3) -0.0335(3) 0.0583(11) Uani 1 1 d . . . . .
C17 C 0.6183(4) 0.7075(4) 0.5965(4) 0.0851(18) Uani 1 1 d . . . . .
H17A H 0.626519 0.668861 0.550474 0.102 Uiso 1 1 calc R U . . .
H17B H 0.559745 0.764420 0.596392 0.102 Uiso 1 1 calc R U . . .
C19 C 0.6452(4) 0.5067(5) 0.7174(3) 0.0783(17) Uani 1 1 d . . . . .
H19A H 0.573745 0.497325 0.718318 0.094 Uiso 1 1 calc R U . . .
H19B H 0.645576 0.536776 0.765797 0.094 Uiso 1 1 calc R U . . .
C15 C 0.8488(5) 0.8049(4) 0.5380(4) 0.0875(18) Uani 1 1 d . . . . .
H15A H 0.866282 0.845416 0.496806 0.105 Uiso 1 1 calc R U . . .
H15B H 0.849056 0.837500 0.585335 0.105 Uiso 1 1 calc R U . . .
C23 C 1.1400(5) 0.4245(5) 0.6225(4) 0.105(3) Uani 1 1 d . . . . .
H23A H 1.189967 0.361362 0.614018 0.126 Uiso 1 1 calc R U . . .
H23B H 1.156404 0.457444 0.664362 0.126 Uiso 1 1 calc R U . . .
C20 C 0.7249(5) 0.4141(4) 0.7059(3) 0.0863(19) Uani 1 1 d . . . . .
H20A H 0.704005 0.370312 0.743468 0.104 Uiso 1 1 calc R U . . .
H20B H 0.728641 0.386156 0.655960 0.104 Uiso 1 1 calc R U . . .
C16 C 0.7409(5) 0.7895(4) 0.5384(4) 0.0858(17) Uani 1 1 d . . . . .
H16A H 0.687882 0.851006 0.542958 0.103 Uiso 1 1 calc R U . . .
H16B H 0.740499 0.756972 0.491146 0.103 Uiso 1 1 calc R U . . .
C18 C 0.5929(4) 0.6527(5) 0.6623(4) 0.0843(17) Uani 1 1 d . . . . .
H18A H 0.590804 0.689191 0.708346 0.101 Uiso 1 1 calc R U . . .
H18B H 0.522557 0.640314 0.664201 0.101 Uiso 1 1 calc R U . . .
C24 C 1.1520(5) 0.4795(6) 0.5538(4) 0.100(2) Uani 1 1 d . . . . .
H24A H 1.227462 0.478420 0.536920 0.121 Uiso 1 1 calc R U . . .
H24B H 1.128128 0.450070 0.513568 0.121 Uiso 1 1 calc R U . . .
C13 C 1.1067(5) 0.6308(6) 0.5046(3) 0.092(2) Uani 1 1 d . . . . .
H13A H 1.094359 0.600590 0.459870 0.110 Uiso 1 1 calc R U . . .
H13B H 1.180105 0.638030 0.494603 0.110 Uiso 1 1 calc R U . . .
C14 C 1.0312(5) 0.7246(5) 0.5210(4) 0.092(2) Uani 1 1 d . . . . .
H14A H 1.041022 0.753148 0.567322 0.111 Uiso 1 1 calc R U . . .
H14B H 1.045024 0.766482 0.479991 0.111 Uiso 1 1 calc R U . . .
C22 C 1.0118(6) 0.3609(5) 0.7046(4) 0.110(3) Uani 1 1 d . . . . .
H22A H 1.010318 0.397254 0.750527 0.133 Uiso 1 1 calc R U . . .
H22B H 1.068477 0.301875 0.701138 0.133 Uiso 1 1 calc R U . . .
C12 C 0.9272(5) 0.3871(4) 0.0035(3) 0.0779(15) Uani 1 1 d . . . . .
C21 C 0.9076(7) 0.3392(4) 0.7061(4) 0.102(2) Uani 1 1 d . . . . .
H21A H 0.909646 0.303151 0.659901 0.122 Uiso 1 1 calc R U . . .
H21B H 0.892332 0.300243 0.748824 0.122 Uiso 1 1 calc R U . . .
O12 O 0.5796(4) 0.8591(3) 1.0509(2) 0.0805(11) Uani 1 1 d . . . . .
O10 O 0.3558(4) 0.8533(3) 0.8715(3) 0.1101(15) Uani 1 1 d . U . . .
O11 O 0.3901(4) 0.8323(4) 1.0129(3) 0.1152(17) Uani 1 1 d . . . . .
O8 O 0.7065(4) 0.9237(3) 0.8053(3) 0.1090(16) Uani 1 1 d . . . . .
O13 O 0.7555(9) 0.8656(7) 0.9488(6) 0.067(2) Uani 0.548(13) 1 d . . P A 1
O9 O 0.5229(5) 0.8956(4) 0.7605(3) 0.1261(18) Uani 1 1 d . . . . .
C35 C 0.4085(7) 0.8356(5) 1.0853(4) 0.099(2) Uani 1 1 d . . . . .
H35A H 0.369947 0.793604 1.114262 0.119 Uiso 0.548(13) 1 calc R U P A 1
H35B H 0.374690 0.900470 1.106240 0.119 Uiso 0.548(13) 1 calc R U P A 1
H35C H 0.435747 0.770369 1.099777 0.119 Uiso 0.452(13) 1 calc R U P A 2
H35D H 0.340134 0.862504 1.118991 0.119 Uiso 0.452(13) 1 calc R U P A 2
C40 C 0.8089(5) 0.9005(5) 0.8238(5) 0.117(3) Uani 1 1 d . . . . .
H40A H 0.842319 0.833765 0.807783 0.140 Uiso 1 1 calc R U . . .
H40B H 0.851152 0.938879 0.793635 0.140 Uiso 1 1 calc R U . . .
C30 C 0.5864(9) 0.9524(6) 0.7205(4) 0.147(4) Uani 1 1 d . . . . .
H30A H 0.556144 1.019567 0.736799 0.176 Uiso 1 1 calc R U . . .
H30B H 0.587496 0.945934 0.666551 0.176 Uiso 1 1 calc R U . . .
C34 C 0.3047(7) 0.8159(6) 0.9964(6) 0.125(3) Uani 1 1 d . . . . .
H34A H 0.243805 0.862602 1.025677 0.150 Uiso 1 1 calc R U . . .
H34B H 0.300404 0.753213 1.014839 0.150 Uiso 1 1 calc R U . . .
C29 C 0.6932(9) 0.9213(6) 0.7354(5) 0.138(3) Uani 1 1 d . . . . .
H29A H 0.722799 0.855604 0.715081 0.166 Uiso 1 1 calc R U . . .
H29B H 0.736254 0.960281 0.706878 0.166 Uiso 1 1 calc R U . . .
C38 C 0.745(2) 0.8961(17) 1.0273(11) 0.087(6) Uani 0.548(13) 1 d D . P A 1
H38A H 0.815875 0.887023 1.041001 0.104 Uiso 0.548(13) 1 calc R U P A 1
H38B H 0.706975 0.963351 1.036268 0.104 Uiso 0.548(13) 1 calc R U P A 1
C31 C 0.4191(8) 0.9174(7) 0.7561(5) 0.143(4) Uani 1 1 d . . . . .
H31A H 0.414460 0.915913 0.702723 0.171 Uiso 1 1 calc R U . . .
H31B H 0.388083 0.983282 0.775493 0.171 Uiso 1 1 calc R U . . .
C39 C 0.8176(7) 0.9120(6) 0.8965(6) 0.133(3) Uani 1 1 d . . . . .
H39A H 0.796573 0.980227 0.910420 0.159 Uiso 0.548(13) 1 calc R U P A 1
H39B H 0.892827 0.888221 0.900599 0.159 Uiso 0.548(13) 1 calc R U P A 1
H39C H 0.873898 0.860234 0.909829 0.159 Uiso 0.452(13) 1 calc R U P A 2
H39D H 0.834556 0.972697 0.905110 0.159 Uiso 0.452(13) 1 calc R U P A 2
C33 C 0.2891(7) 0.8168(7) 0.9214(7) 0.153(4) Uani 1 1 d . U . . .
H33A H 0.295368 0.751260 0.904273 0.184 Uiso 1 1 calc R U . . .
H33B H 0.215747 0.853141 0.920621 0.184 Uiso 1 1 calc R U . . .
C32 C 0.3539(8) 0.8617(8) 0.7928(7) 0.156(4) Uani 1 1 d . U . . .
H32A H 0.376587 0.797860 0.768347 0.187 Uiso 1 1 calc R U . . .
H32B H 0.280117 0.889532 0.786645 0.187 Uiso 1 1 calc R U . . .
C37 C 0.6849(13) 0.8352(11) 1.0699(7) 0.105(5) Uani 0.548(13) 1 d D . P A 1
H37A H 0.720221 0.768052 1.056599 0.126 Uiso 0.548(13) 1 calc R U P A 1
H37B H 0.679899 0.846458 1.123907 0.126 Uiso 0.548(13) 1 calc R U P A 1
C36 C 0.5143(13) 0.8115(12) 1.0998(7) 0.114(6) Uani 0.548(13) 1 d . . P A 1
H36A H 0.544026 0.742508 1.092435 0.137 Uiso 0.548(13) 1 calc R U P A 1
H36B H 0.513200 0.829581 1.152068 0.137 Uiso 0.548(13) 1 calc R U P A 1
C37A C 0.6584(14) 0.9071(12) 1.0627(11) 0.099(6) Uani 0.452(13) 1 d D U P A 2
H37C H 0.677233 0.892770 1.112053 0.118 Uiso 0.452(13) 1 calc R U P A 2
H37D H 0.629035 0.976037 1.061892 0.118 Uiso 0.452(13) 1 calc R U P A 2
C36A C 0.4813(14) 0.8894(11) 1.0962(7) 0.085(5) Uani 0.452(13) 1 d . . P A 2
H36C H 0.450762 0.956124 1.086733 0.101 Uiso 0.452(13) 1 calc R U P A 2
H36D H 0.490182 0.886431 1.148715 0.101 Uiso 0.452(13) 1 calc R U P A 2
O13A O 0.7305(10) 0.9108(12) 0.9336(12) 0.112(6) Uani 0.452(13) 1 d . U P A 2
C38A C 0.755(2) 0.877(2) 1.0038(19) 0.120(10) Uani 0.452(13) 1 d D U P A 2
H38C H 0.812048 0.903009 1.016420 0.144 Uiso 0.452(13) 1 calc R U P A 2
H38D H 0.779712 0.807510 1.000469 0.144 Uiso 0.452(13) 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
Ni2 S12 2.1611(12) 2_666 ?
Ni2 S12 2.1611(12) . ?
Ni2 S11 2.1581(12) 2_666 ?
Ni2 S11 2.1580(12) . ?
Ni1 S2 2.1525(11) . ?
Ni1 S7 2.1573(13) . ?
Ni1 S1 2.1682(13) . ?
Ni1 S6 2.1589(11) . ?
Ni3 S16 2.1560(14) 2_665 ?
Ni3 S16 2.1561(14) . ?
Ni3 S17 2.1529(13) . ?
Ni3 S17 2.1530(13) 2_665 ?
S2 C2 1.701(5) . ?
S12 C8 1.719(5) . ?
S7 C5 1.723(5) . ?
S11 C7 1.715(5) . ?
S1 C1 1.719(4) . ?
S4 C2 1.734(4) . ?
S4 C3 1.740(5) . ?
S6 C4 1.707(5) . ?
S3 C1 1.735(5) . ?
S3 C3 1.748(5) . ?
S14 C8 1.745(5) . ?
S14 C9 1.744(5) . ?
S13 C7 1.747(5) . ?
S13 C9 1.732(6) . ?
S16 C10 1.714(5) . ?
S8 C4 1.750(5) . ?
S8 C6 1.730(7) . ?
S9 C5 1.729(5) . ?
S9 C6 1.738(6) . ?
S15 C9 1.631(6) . ?
S17 C11 1.715(5) . ?
S5 C3 1.616(5) . ?
S18 C10 1.742(5) . ?
S18 C12 1.730(6) . ?
S10 C6 1.637(6) . ?
S19 C11 1.742(5) . ?
S19 C12 1.723(6) . ?
O7 C26 1.411(5) . ?
O7 C27 1.422(6) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N1 H1C 0.9000 . ?
N1 C25 1.480(5) . ?
S20 C12 1.634(6) . ?
O6 C17 1.425(6) . ?
O6 C16 1.392(7) . ?
N2 H2A 0.9000 . ?
N2 H2B 0.9000 . ?
N2 H2C 0.9000 . ?
N2 C28 1.487(6) . ?
O1 C19 1.439(6) . ?
O1 C18 1.384(7) . ?
O5 C15 1.428(7) . ?
O5 C14 1.387(7) . ?
O3 C23 1.458(7) . ?
O3 C22 1.411(8) . ?
O4 C24 1.371(8) . ?
O4 C13 1.448(7) . ?
O2 C20 1.397(7) . ?
O2 C21 1.449(7) . ?
C2 C1 1.375(6) . ?
C8 C7 1.355(6) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 C26 1.498(7) . ?
C5 C4 1.366(7) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 C28 1.486(7) . ?
C11 C10 1.357(7) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 C18 1.468(8) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 C20 1.475(9) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 C16 1.488(8) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 C24 1.485(10) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 C14 1.466(9) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 C21 1.474(10) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
O12 C37 1.445(15) . ?
O12 C36 1.421(14) . ?
O12 C37A 1.429(16) . ?
O12 C36A 1.369(16) . ?
O10 C33 1.345(10) . ?
O10 C32 1.435(11) . ?
O11 C35 1.378(8) . ?
O11 C34 1.289(9) . ?
O8 C40 1.405(9) . ?
O8 C29 1.313(10) . ?
O13 C38 1.46(2) . ?
O13 C39 1.418(12) . ?
O9 C30 1.423(10) . ?
O9 C31 1.339(10) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C35 H35D 0.9800 . ?
C35 C36 1.420(16) . ?
C35 C36A 1.416(16) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 C39 1.357(11) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 C29 1.438(12) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 C33 1.411(12) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 C37 1.462(17) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 C32 1.403(12) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C39 H39D 0.9800 . ?
C39 O13A 1.223(15) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C37A H37C 0.9800 . ?
C37A H37D 0.9800 . ?
C37A C38A 1.47(2) . ?
C36A H36C 0.9800 . ?
C36A H36D 0.9800 . ?
O13A C38A 1.43(4) . ?
C38A H38C 0.9800 . ?
C38A H38D 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
S12 Ni2 S12 180.00(4) . 2_666 ?
S11 Ni2 S12 86.71(4) . 2_666 ?
S11 Ni2 S12 93.29(4) . . ?
S11 Ni2 S12 86.71(4) 2_666 . ?
S11 Ni2 S12 93.28(4) 2_666 2_666 ?
S11 Ni2 S11 180.0 . 2_666 ?
S2 Ni1 S7 85.51(4) . . ?
S2 Ni1 S1 93.25(5) . . ?
S2 Ni1 S6 178.58(6) . . ?
S7 Ni1 S1 176.90(5) . . ?
S7 Ni1 S6 93.12(5) . . ?
S6 Ni1 S1 88.09(5) . . ?
S16 Ni3 S16 180.0 2_665 . ?
S17 Ni3 S16 86.48(5) 2_665 . ?
S17 Ni3 S16 86.48(5) . 2_665 ?
S17 Ni3 S16 93.52(5) . . ?
S17 Ni3 S16 93.52(5) 2_665 2_665 ?
S17 Ni3 S17 180.0 . 2_665 ?
C2 S2 Ni1 102.64(14) . . ?
C8 S12 Ni2 102.00(16) . . ?
C5 S7 Ni1 102.36(18) . . ?
C7 S11 Ni2 102.05(16) . . ?
C1 S1 Ni1 101.84(15) . . ?
C2 S4 C3 98.4(2) . . ?
C4 S6 Ni1 102.22(15) . . ?
C1 S3 C3 98.2(2) . . ?
C9 S14 C8 97.5(2) . . ?
C9 S13 C7 98.0(2) . . ?
C10 S16 Ni3 101.93(18) . . ?
C6 S8 C4 98.0(2) . . ?
C5 S9 C6 97.3(3) . . ?
C11 S17 Ni3 101.89(17) . . ?
C12 S18 C10 97.2(3) . . ?
C12 S19 C11 97.7(3) . . ?
C26 O7 C27 111.6(3) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C25 N1 H1A 109.5 . . ?
C25 N1 H1B 109.5 . . ?
C25 N1 H1C 109.5 . . ?
C16 O6 C17 112.1(4) . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C28 N2 H2A 109.5 . . ?
C28 N2 H2B 109.5 . . ?
C28 N2 H2C 109.5 . . ?
C18 O1 C19 112.1(5) . . ?
C14 O5 C15 113.6(5) . . ?
C22 O3 C23 113.6(5) . . ?
C24 O4 C13 112.9(5) . . ?
C20 O2 C21 113.4(5) . . ?
S2 C2 S4 122.9(2) . . ?
C1 C2 S2 121.3(3) . . ?
C1 C2 S4 115.8(3) . . ?
S12 C8 S14 122.6(3) . . ?
C7 C8 S12 121.2(4) . . ?
C7 C8 S14 116.3(4) . . ?
S11 C7 S13 122.7(3) . . ?
C8 C7 S11 121.5(4) . . ?
C8 C7 S13 115.8(4) . . ?
S1 C1 S3 123.3(2) . . ?
C2 C1 S1 120.9(4) . . ?
C2 C1 S3 115.8(3) . . ?
N1 C25 H25A 109.0 . . ?
N1 C25 H25B 109.0 . . ?
N1 C25 C26 113.0(4) . . ?
H25A C25 H25B 107.8 . . ?
C26 C25 H25A 109.0 . . ?
C26 C25 H25B 109.0 . . ?
S7 C5 S9 122.4(3) . . ?
C4 C5 S7 120.3(4) . . ?
C4 C5 S9 117.3(4) . . ?
S6 C4 S8 123.7(3) . . ?
C5 C4 S6 121.7(4) . . ?
C5 C4 S8 114.5(4) . . ?
O7 C26 C25 109.4(4) . . ?
O7 C26 H26A 109.8 . . ?
O7 C26 H26B 109.8 . . ?
C25 C26 H26A 109.8 . . ?
C25 C26 H26B 109.8 . . ?
H26A C26 H26B 108.2 . . ?
S13 C9 S14 112.4(3) . . ?
S15 C9 S14 123.9(3) . . ?
S15 C9 S13 123.7(3) . . ?
S4 C3 S3 111.7(3) . . ?
S5 C3 S4 123.1(3) . . ?
S5 C3 S3 125.2(3) . . ?
O7 C27 H27A 109.8 . . ?
O7 C27 H27B 109.8 . . ?
O7 C27 C28 109.4(4) . . ?
H27A C27 H27B 108.2 . . ?
C28 C27 H27A 109.8 . . ?
C28 C27 H27B 109.8 . . ?
S17 C11 S19 123.0(3) . . ?
C10 C11 S17 121.4(4) . . ?
C10 C11 S19 115.6(4) . . ?
N2 C28 H28A 109.1 . . ?
N2 C28 H28B 109.1 . . ?
C27 C28 N2 112.6(4) . . ?
C27 C28 H28A 109.1 . . ?
C27 C28 H28B 109.1 . . ?
H28A C28 H28B 107.8 . . ?
S8 C6 S9 112.7(3) . . ?
S10 C6 S8 124.5(4) . . ?
S10 C6 S9 122.7(4) . . ?
S16 C10 S18 122.5(3) . . ?
C11 C10 S16 121.2(4) . . ?
C11 C10 S18 116.3(4) . . ?
O6 C17 H17A 109.7 . . ?
O6 C17 H17B 109.7 . . ?
O6 C17 C18 109.7(4) . . ?
H17A C17 H17B 108.2 . . ?
C18 C17 H17A 109.7 . . ?
C18 C17 H17B 109.7 . . ?
O1 C19 H19A 109.7 . . ?
O1 C19 H19B 109.7 . . ?
O1 C19 C20 109.7(5) . . ?
H19A C19 H19B 108.2 . . ?
C20 C19 H19A 109.7 . . ?
C20 C19 H19B 109.7 . . ?
O5 C15 H15A 109.6 . . ?
O5 C15 H15B 109.6 . . ?
O5 C15 C16 110.1(4) . . ?
H15A C15 H15B 108.2 . . ?
C16 C15 H15A 109.6 . . ?
C16 C15 H15B 109.6 . . ?
O3 C23 H23A 109.8 . . ?
O3 C23 H23B 109.8 . . ?
O3 C23 C24 109.3(4) . . ?
H23A C23 H23B 108.3 . . ?
C24 C23 H23A 109.8 . . ?
C24 C23 H23B 109.8 . . ?
O2 C20 C19 109.2(4) . . ?
O2 C20 H20A 109.8 . . ?
O2 C20 H20B 109.8 . . ?
C19 C20 H20A 109.8 . . ?
C19 C20 H20B 109.8 . . ?
H20A C20 H20B 108.3 . . ?
O6 C16 C15 109.5(5) . . ?
O6 C16 H16A 109.8 . . ?
O6 C16 H16B 109.8 . . ?
C15 C16 H16A 109.8 . . ?
C15 C16 H16B 109.8 . . ?
H16A C16 H16B 108.2 . . ?
O1 C18 C17 109.3(5) . . ?
O1 C18 H18A 109.8 . . ?
O1 C18 H18B 109.8 . . ?
C17 C18 H18A 109.8 . . ?
C17 C18 H18B 109.8 . . ?
H18A C18 H18B 108.3 . . ?
O4 C24 C23 110.2(5) . . ?
O4 C24 H24A 109.6 . . ?
O4 C24 H24B 109.6 . . ?
C23 C24 H24A 109.6 . . ?
C23 C24 H24B 109.6 . . ?
H24A C24 H24B 108.1 . . ?
O4 C13 H13A 109.8 . . ?
O4 C13 H13B 109.8 . . ?
O4 C13 C14 109.6(5) . . ?
H13A C13 H13B 108.2 . . ?
C14 C13 H13A 109.8 . . ?
C14 C13 H13B 109.8 . . ?
O5 C14 C13 110.1(5) . . ?
O5 C14 H14A 109.6 . . ?
O5 C14 H14B 109.6 . . ?
C13 C14 H14A 109.6 . . ?
C13 C14 H14B 109.6 . . ?
H14A C14 H14B 108.1 . . ?
O3 C22 H22A 110.3 . . ?
O3 C22 H22B 110.3 . . ?
O3 C22 C21 107.1(5) . . ?
H22A C22 H22B 108.5 . . ?
C21 C22 H22A 110.3 . . ?
C21 C22 H22B 110.3 . . ?
S19 C12 S18 113.1(3) . . ?
S20 C12 S18 123.2(4) . . ?
S20 C12 S19 123.7(3) . . ?
O2 C21 C22 109.5(5) . . ?
O2 C21 H21A 109.8 . . ?
O2 C21 H21B 109.8 . . ?
C22 C21 H21A 109.8 . . ?
C22 C21 H21B 109.8 . . ?
H21A C21 H21B 108.2 . . ?
C36 O12 C37 108.2(9) . . ?
C36A O12 C37A 116.2(10) . . ?
C33 O10 C32 125.9(7) . . ?
C34 O11 C35 123.5(6) . . ?
C29 O8 C40 121.5(7) . . ?
C39 O13 C38 114.4(11) . . ?
C31 O9 C30 117.1(7) . . ?
O11 C35 H35A 107.2 . . ?
O11 C35 H35B 107.2 . . ?
O11 C35 H35C 108.6 . . ?
O11 C35 H35D 108.6 . . ?
O11 C35 C36 120.7(8) . . ?
O11 C35 C36A 114.8(7) . . ?
H35A C35 H35B 106.8 . . ?
H35C C35 H35D 107.5 . . ?
C36 C35 H35A 107.2 . . ?
C36 C35 H35B 107.2 . . ?
C36A C35 H35C 108.6 . . ?
C36A C35 H35D 108.6 . . ?
O8 C40 H40A 107.7 . . ?
O8 C40 H40B 107.7 . . ?
H40A C40 H40B 107.1 . . ?
C39 C40 O8 118.6(7) . . ?
C39 C40 H40A 107.7 . . ?
C39 C40 H40B 107.7 . . ?
O9 C30 H30A 110.0 . . ?
O9 C30 H30B 110.0 . . ?
O9 C30 C29 108.6(6) . . ?
H30A C30 H30B 108.3 . . ?
C29 C30 H30A 110.0 . . ?
C29 C30 H30B 110.0 . . ?
O11 C34 H34A 107.1 . . ?
O11 C34 H34B 107.1 . . ?
O11 C34 C33 120.7(7) . . ?
H34A C34 H34B 106.8 . . ?
C33 C34 H34A 107.1 . . ?
C33 C34 H34B 107.1 . . ?
O8 C29 C30 118.2(8) . . ?
O8 C29 H29A 107.8 . . ?
O8 C29 H29B 107.8 . . ?
C30 C29 H29A 107.8 . . ?
C30 C29 H29B 107.8 . . ?
H29A C29 H29B 107.1 . . ?
O13 C38 H38A 110.9 . . ?
O13 C38 H38B 110.9 . . ?
H38A C38 H38B 108.9 . . ?
C37 C38 O13 104.4(14) . . ?
C37 C38 H38A 110.9 . . ?
C37 C38 H38B 110.9 . . ?
O9 C31 H31A 107.5 . . ?
O9 C31 H31B 107.5 . . ?
O9 C31 C32 119.2(7) . . ?
H31A C31 H31B 107.0 . . ?
C32 C31 H31A 107.5 . . ?
C32 C31 H31B 107.5 . . ?
O13 C39 H39A 108.5 . . ?
O13 C39 H39B 108.5 . . ?
C40 C39 O13 115.1(8) . . ?
C40 C39 H39A 108.5 . . ?
C40 C39 H39B 108.5 . . ?
C40 C39 H39C 110.6 . . ?
C40 C39 H39D 110.6 . . ?
H39A C39 H39B 107.5 . . ?
H39C C39 H39D 108.8 . . ?
O13A C39 C40 105.5(12) . . ?
O13A C39 H39C 110.6 . . ?
O13A C39 H39D 110.6 . . ?
O10 C33 C34 116.6(7) . . ?
O10 C33 H33A 108.1 . . ?
O10 C33 H33B 108.1 . . ?
C34 C33 H33A 108.1 . . ?
C34 C33 H33B 108.1 . . ?
H33A C33 H33B 107.3 . . ?
O10 C32 H32A 108.7 . . ?
O10 C32 H32B 108.7 . . ?
C31 C32 O10 114.3(7) . . ?
C31 C32 H32A 108.7 . . ?
C31 C32 H32B 108.7 . . ?
H32A C32 H32B 107.6 . . ?
O12 C37 C38 107.1(15) . . ?
O12 C37 H37A 110.3 . . ?
O12 C37 H37B 110.3 . . ?
C38 C37 H37A 110.3 . . ?
C38 C37 H37B 110.3 . . ?
H37A C37 H37B 108.6 . . ?
O12 C36 H36A 109.6 . . ?
O12 C36 H36B 109.6 . . ?
C35 C36 O12 110.3(10) . . ?
C35 C36 H36A 109.6 . . ?
C35 C36 H36B 109.6 . . ?
H36A C36 H36B 108.1 . . ?
O12 C37A H37C 109.6 . . ?
O12 C37A H37D 109.6 . . ?
O12 C37A C38A 110.5(15) . . ?
H37C C37A H37D 108.1 . . ?
C38A C37A H37C 109.6 . . ?
C38A C37A H37D 109.6 . . ?
O12 C36A C35 113.8(10) . . ?
O12 C36A H36C 108.8 . . ?
O12 C36A H36D 108.8 . . ?
C35 C36A H36C 108.8 . . ?
C35 C36A H36D 108.8 . . ?
H36C C36A H36D 107.7 . . ?
C39 O13A C38A 103.6(16) . . ?
C37A C38A H38C 109.8 . . ?
C37A C38A H38D 109.8 . . ?
O13A C38A C37A 109(2) . . ?
O13A C38A H38C 109.8 . . ?
O13A C38A H38D 109.8 . . ?
H38C C38A H38D 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
Ni2 S12 C8 S14 179.7(2) . . . . ?
Ni2 S12 C8 C7 0.1(4) . . . . ?
Ni2 S11 C7 S13 179.9(2) . . . . ?
Ni2 S11 C7 C8 1.5(4) . . . . ?
Ni1 S2 C2 S4 -179.5(2) . . . . ?
Ni1 S2 C2 C1 0.8(4) . . . . ?
Ni1 S7 C5 S9 175.0(2) . . . . ?
Ni1 S7 C5 C4 -4.1(4) . . . . ?
Ni1 S1 C1 S3 176.8(2) . . . . ?
Ni1 S1 C1 C2 -3.4(4) . . . . ?
Ni1 S6 C4 S8 -176.3(2) . . . . ?
Ni1 S6 C4 C5 2.9(4) . . . . ?
Ni3 S16 C10 S18 -178.8(2) . . . . ?
Ni3 S16 C10 C11 0.8(4) . . . . ?
Ni3 S17 C11 S19 179.1(3) . . . . ?
Ni3 S17 C11 C10 -1.5(4) . . . . ?
S2 C2 C1 S1 1.9(5) . . . . ?
S2 C2 C1 S3 -178.3(2) . . . . ?
S12 C8 C7 S11 -1.1(5) . . . . ?
S12 C8 C7 S13 -179.7(2) . . . . ?
S7 C5 C4 S6 0.9(5) . . . . ?
S7 C5 C4 S8 -179.8(2) . . . . ?
S4 C2 C1 S1 -177.8(2) . . . . ?
S4 C2 C1 S3 2.0(4) . . . . ?
S14 C8 C7 S11 179.2(2) . . . . ?
S14 C8 C7 S13 0.6(4) . . . . ?
S9 C5 C4 S6 -178.3(2) . . . . ?
S9 C5 C4 S8 1.0(5) . . . . ?
S17 C11 C10 S16 0.5(6) . . . . ?
S17 C11 C10 S18 -179.9(3) . . . . ?
S19 C11 C10 S16 179.9(3) . . . . ?
S19 C11 C10 S18 -0.5(5) . . . . ?
O7 C27 C28 N2 -69.2(5) . . . . ?
N1 C25 C26 O7 -69.2(5) . . . . ?
O6 C17 C18 O1 -66.0(6) . . . . ?
O1 C19 C20 O2 65.5(6) . . . . ?
O5 C15 C16 O6 61.3(6) . . . . ?
O3 C23 C24 O4 67.3(6) . . . . ?
O3 C22 C21 O2 -60.9(7) . . . . ?
O4 C13 C14 O5 -64.5(6) . . . . ?
C2 S4 C3 S3 1.4(3) . . . . ?
C2 S4 C3 S5 -177.4(3) . . . . ?
C8 S14 C9 S13 2.9(3) . . . . ?
C8 S14 C9 S15 -177.0(3) . . . . ?
C7 S13 C9 S14 -2.6(3) . . . . ?
C7 S13 C9 S15 177.2(3) . . . . ?
C1 S3 C3 S4 -0.6(3) . . . . ?
C1 S3 C3 S5 178.3(3) . . . . ?
C5 S9 C6 S8 -2.2(3) . . . . ?
C5 S9 C6 S10 179.5(3) . . . . ?
C4 S8 C6 S9 2.6(3) . . . . ?
C4 S8 C6 S10 -179.1(3) . . . . ?
C26 O7 C27 C28 -179.4(4) . . . . ?
C9 S14 C8 S12 178.1(3) . . . . ?
C9 S14 C8 C7 -2.2(4) . . . . ?
C9 S13 C7 S11 -177.3(3) . . . . ?
C9 S13 C7 C8 1.3(4) . . . . ?
C3 S4 C2 S2 178.2(3) . . . . ?
C3 S4 C2 C1 -2.1(4) . . . . ?
C3 S3 C1 S1 179.0(3) . . . . ?
C3 S3 C1 C2 -0.8(4) . . . . ?
C27 O7 C26 C25 -177.7(3) . . . . ?
C11 S19 C12 S18 0.0(4) . . . . ?
C11 S19 C12 S20 179.1(4) . . . . ?
C6 S8 C4 S6 177.1(3) . . . . ?
C6 S8 C4 C5 -2.2(4) . . . . ?
C6 S9 C5 S7 -178.5(3) . . . . ?
C6 S9 C5 C4 0.7(4) . . . . ?
C10 S18 C12 S19 -0.2(4) . . . . ?
C10 S18 C12 S20 -179.3(4) . . . . ?
C17 O6 C16 C15 -172.7(5) . . . . ?
C19 O1 C18 C17 -175.2(4) . . . . ?
C15 O5 C14 C13 -174.5(5) . . . . ?
C23 O3 C22 C21 -167.5(5) . . . . ?
C20 O2 C21 C22 173.3(5) . . . . ?
C16 O6 C17 C18 -178.2(5) . . . . ?
C18 O1 C19 C20 175.1(4) . . . . ?
C24 O4 C13 C14 172.9(4) . . . . ?
C13 O4 C24 C23 176.1(4) . . . . ?
C14 O5 C15 C16 174.3(5) . . . . ?
C22 O3 C23 C24 178.2(5) . . . . ?
C12 S18 C10 S16 -180.0(3) . . . . ?
C12 S18 C10 C11 0.4(4) . . . . ?
C12 S19 C11 S17 179.7(3) . . . . ?
C12 S19 C11 C10 0.3(4) . . . . ?
C21 O2 C20 C19 176.9(5) . . . . ?
O12 C37A C38A O13A 68(3) . . . . ?
O11 C35 C36 O12 48.2(16) . . . . ?
O11 C35 C36A O12 -57.4(14) . . . . ?
O11 C34 C33 O10 -12.6(15) . . . . ?
O8 C40 C39 O13 53.9(12) . . . . ?
O8 C40 C39 O13A 22.1(14) . . . . ?
O13 C38 C37 O12 -65(2) . . . . ?
O9 C30 C29 O8 -58.6(11) . . . . ?
O9 C31 C32 O10 54.9(14) . . . . ?
C35 O11 C34 C33 177.7(8) . . . . ?
C40 O8 C29 C30 -175.7(7) . . . . ?
C40 C39 O13A C38A 152.9(16) . . . . ?
C30 O9 C31 C32 178.3(9) . . . . ?
C34 O11 C35 C36 151.5(11) . . . . ?
C34 O11 C35 C36A -156.2(11) . . . . ?
C29 O8 C40 C39 174.6(8) . . . . ?
C38 O13 C39 C40 -166.2(16) . . . . ?
C31 O9 C30 C29 177.0(8) . . . . ?
C39 O13 C38 C37 -176.6(13) . . . . ?
C39 O13A C38A C37A 157.6(16) . . . . ?
C33 O10 C32 C31 169.2(9) . . . . ?
C32 O10 C33 C34 -179.6(9) . . . . ?
C37 O12 C36 C35 177.7(10) . . . . ?
C36 O12 C37 C38 -171.3(13) . . . . ?
C37A O12 C36A C35 -176.3(11) . . . . ?
C36A O12 C37A C38A -172.1(19) . . . . ?

