# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_kj-19
_database_code_depnum_ccdc_archive 'CCDC 1912753'
loop_
_audit_author_name
_audit_author_address
'Juan Kang'
;Tianjin University
China
;
_audit_update_record             
;
2019-04-29 deposited with the CCDC.	2019-09-27 downloaded from the CCDC.
;
_audit_creation_date             2019-01-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C40 H44 Cu4 N12 O12 S8, 2(C H4 O)'
_chemical_formula_sum            'C42 H52 Cu4 N12 O14 S8'
_chemical_formula_weight         1459.59
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   32.4476(3)
_cell_length_b                   10.10680(10)
_cell_length_c                   17.29590(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5672.04(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    36041
_cell_measurement_temperature    300.99(10)
_cell_measurement_theta_max      74.5420
_cell_measurement_theta_min      2.7310
_shelx_estimated_absorpt_T_max   0.517
_shelx_estimated_absorpt_T_min   0.431
_exptl_absorpt_coefficient_mu    5.062
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43091
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.45g (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2976
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            49960
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.660
_diffrn_reflns_theta_min         2.724
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      300.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     22.00 118.00   0.50    0.15    --   46.12  79.00  32.00  192
  2  ω   -173.00 -84.00   0.50    0.58    -- -100.00 -55.00  33.00  178
  3  ω   -125.00 -27.00   0.50    0.58    -- -100.00  79.00  32.00  196
  4  ω     29.00 132.00   0.50    0.58    --  101.75 -91.00 167.00  206
  5  ω     32.00 120.00   0.50    0.15    --   46.12  38.00 150.00  176
  6  ω     20.00  95.00   0.50    0.15    --   46.12-125.00-120.00  150
  7  ω   -172.00 -85.00   0.50    0.58    -- -100.00 -45.00 -60.00  174
  8  ω   -115.00 -25.00   0.50    0.58    -- -100.00  30.00-180.00  180
  9  ω   -176.00 -82.00   0.50    0.58    -- -100.00 -15.00 -60.00  188
 10  ω     84.00 178.00   0.50    0.58    --  101.75  15.00 150.00  188
 11  ω     87.00 174.00   0.50    0.58    --  101.75  45.00   0.00  174
 12  ω     30.00 118.00   0.50    0.15    --   46.12  57.00-120.00  176
 13  ω     30.00 118.00   0.50    0.15    --   46.12  57.00-180.00  176
 14  ω     23.00 118.00   0.50    0.15    --   46.12  77.00 -60.00  190
 15  ω     86.00 117.00   0.50    0.58    --  101.75  30.00-150.00   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0073223000
_diffrn_orient_matrix_UB_12      0.1133645000
_diffrn_orient_matrix_UB_13      -0.0579098000
_diffrn_orient_matrix_UB_21      0.0301725000
_diffrn_orient_matrix_UB_22      -0.0653915000
_diffrn_orient_matrix_UB_23      -0.0571667000
_diffrn_orient_matrix_UB_31      -0.0359087000
_diffrn_orient_matrix_UB_32      -0.0781746000
_diffrn_orient_matrix_UB_33      -0.0362390000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.827
_reflns_Friedel_fraction_full    0.920
_reflns_Friedel_fraction_max     0.860
_reflns_number_gt                9979
_reflns_number_total             10667
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details 
;
 Flack x determined using 4245 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.014(8)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         10667
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0289
_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)+(0.0470P)²+1.3875P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0778
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Rotating group:
 N2(H2A,H2B), N4(H4A,H4B), N1(H1A,H1B), N3(H3A,H3B)
2.b Aromatic/amide H refined with riding coordinates:
 C25(H25), C18(H18), C17(H17), C35(H35), C23(H23), C14(H14), C5(H5), C24(H24),
 C34(H34), C28(H28), C19(H19), C31(H31), C8(H8), C29(H29), C12(H12), C9(H9),
 C2(H2), C32(H32), C26(H26), C6(H6), C20(H20), C13(H13), C3(H3), C11(H11)
2.c Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C38(H38A,H38B,H38C), C37(H37A,H37B,H37C), C41(H41A,H41B,
 H41C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C)
2.d Idealised tetrahedral OH refined as rotating group:
 O14(H14A), O13(H13A)
;
_atom_sites_solution_hydrogens   mixed
_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
Cu3 Cu -0.61038(2) -0.50158(6) -0.61567(4) 0.03531(13) Uani 1 1 d . . . . .
Cu2 Cu -0.52784(2) -0.61080(6) -0.57131(3) 0.03606(13) Uani 1 1 d . . . . .
Cu4 Cu -0.64741(2) -0.60522(6) -0.47408(3) 0.03633(13) Uani 1 1 d . . . . .
Cu1 Cu -0.56209(2) -0.67453(6) -0.42061(3) 0.03661(13) Uani 1 1 d . . . . .
S6 S -0.66600(3) -0.55651(11) -0.74737(6) 0.0401(2) Uani 1 1 d . . . . .
S8 S -0.71589(4) -0.41905(11) -0.42912(6) 0.0453(2) Uani 1 1 d . . . . .
S5 S -0.72332(4) -0.77956(12) -0.66562(7) 0.0511(3) Uani 1 1 d . . . . .
S2 S -0.44297(4) -0.49870(12) -0.55280(7) 0.0484(3) Uani 1 1 d . . . . .
S3 S -0.52140(4) -0.92727(12) -0.36770(8) 0.0558(3) Uani 1 1 d . . . . .
S7 S -0.68861(5) -0.16809(11) -0.52928(9) 0.0599(3) Uani 1 1 d . . . . .
S4 S -0.44773(4) -0.44319(14) -0.36949(8) 0.0593(3) Uani 1 1 d . . . . .
S1 S -0.49045(5) -1.03011(13) -0.53309(10) 0.0701(4) Uani 1 1 d . . . . .
O9 O -0.57717(10) -0.6568(3) -0.62687(18) 0.0429(7) Uani 1 1 d . . . . .
O10 O -0.55648(10) -0.4472(3) -0.5821(2) 0.0481(8) Uani 1 1 d . . . . .
O7 O -0.71793(13) -0.5496(4) -0.3953(2) 0.0607(9) Uani 1 1 d . . . . .
O11 O -0.61220(10) -0.7561(3) -0.45421(19) 0.0443(7) Uani 1 1 d . . . . .
O6 O -0.66752(11) -0.6769(3) -0.79168(19) 0.0528(8) Uani 1 1 d . . . . .
O12 O -0.60275(10) -0.5352(3) -0.4149(2) 0.0487(7) Uani 1 1 d . . . . .
N5 N -0.50743(12) -0.7930(4) -0.5715(2) 0.0441(8) Uani 1 1 d . . . . .
O4 O -0.43246(12) -0.3621(4) -0.5390(3) 0.0662(10) Uani 1 1 d . . . . .
N8 N -0.51615(12) -0.5660(4) -0.3828(2) 0.0419(8) Uani 1 1 d . . . . .
N10 N -0.68494(11) -0.7002(3) -0.5450(2) 0.0384(7) Uani 1 1 d . . . . .
O5 O -0.63192(10) -0.4675(4) -0.75979(19) 0.0517(8) Uani 1 1 d . . . . .
O3 O -0.45396(13) -0.5372(5) -0.6300(2) 0.0647(10) Uani 1 1 d . . . . .
O8 O -0.71132(13) -0.3100(4) -0.3764(2) 0.0618(10) Uani 1 1 d . . . . .
N11 N -0.67775(11) -0.4308(3) -0.4887(2) 0.0399(8) Uani 1 1 d . . . . .
N6 N -0.52508(12) -0.8333(4) -0.4427(2) 0.0436(8) Uani 1 1 d . . . . .
N7 N -0.48301(11) -0.5421(4) -0.5026(2) 0.0399(8) Uani 1 1 d . . . . .
N12 N -0.63824(12) -0.3352(4) -0.5870(2) 0.0421(8) Uani 1 1 d . . . . .
N9 N -0.66293(11) -0.5874(3) -0.6554(2) 0.0368(7) Uani 1 1 d . . . . .
O2 O -0.54083(14) -0.8492(4) -0.3082(2) 0.0709(11) Uani 1 1 d . . . . .
C15 C -0.50957(14) -0.8737(4) -0.5119(3) 0.0432(9) Uani 1 1 d . . . . .
C36 C -0.71213(15) -0.4713(5) -0.7647(3) 0.0432(9) Uani 1 1 d . . . . .
C25 C -0.79275(16) -0.3201(5) -0.4503(3) 0.0512(11) Uani 1 1 d . . . . .
H25 H -0.789283 -0.280839 -0.402099 0.061 Uiso 1 1 calc R . . . .
O1 O -0.53794(14) -1.0571(4) -0.3816(3) 0.0785(13) Uani 1 1 d . . . . .
C21 C -0.68683(13) -0.6788(4) -0.6205(2) 0.0362(8) Uani 1 1 d . . . . .
C18 C -0.51068(17) -0.5363(5) -0.3049(3) 0.0519(11) Uani 1 1 d . . . . .
H18 H -0.530009 -0.559073 -0.267525 0.062 Uiso 1 1 calc R . . . .
N2 N -0.30604(17) -0.8236(6) -0.4325(4) 0.0792(15) Uani 1 1 d . . . . .
H2A H -0.301778 -0.895585 -0.458858 0.095 Uiso 1 1 d GR . . . .
H2B H -0.283239 -0.778605 -0.432117 0.095 Uiso 1 1 d GR . . . .
C17 C -0.47636(18) -0.4738(6) -0.2878(3) 0.0606(14) Uani 1 1 d . . . . .
H17 H -0.468590 -0.449357 -0.238028 0.073 Uiso 1 1 calc R . . . .
C22 C -0.66688(14) -0.3257(4) -0.5338(3) 0.0395(9) Uani 1 1 d . . . . .
N4 N -0.87125(17) -0.3451(6) -0.6008(4) 0.0784(15) Uani 1 1 d . . . . .
H4A H -0.868965 -0.379222 -0.646268 0.094 Uiso 1 1 d GR . . . .
H4B H -0.890765 -0.384830 -0.576248 0.094 Uiso 1 1 d GR . . . .
C16 C -0.48474(13) -0.5220(4) -0.4249(3) 0.0390(9) Uani 1 1 d . . . . .
C35 C -0.74543(16) -0.5351(5) -0.7991(3) 0.0494(11) Uani 1 1 d . . . . .
H35 H -0.743539 -0.623888 -0.812736 0.059 Uiso 1 1 calc R . . . .
C23 C -0.65786(18) -0.1187(5) -0.6042(3) 0.0561(12) Uani 1 1 d . . . . .
H23 H -0.658339 -0.034654 -0.626051 0.067 Uiso 1 1 calc R . . . .
C14 C -0.49087(17) -0.8542(6) -0.6363(3) 0.0554(12) Uani 1 1 d . . . . .
H14 H -0.487764 -0.810702 -0.683348 0.066 Uiso 1 1 calc R . . . .
C5 C -0.40077(16) -0.7294(5) -0.5324(3) 0.0564(12) Uani 1 1 d . . . . .
H5 H -0.422435 -0.769718 -0.558612 0.068 Uiso 1 1 calc R . . . .
C24 C -0.63292(16) -0.2170(4) -0.6273(3) 0.0493(11) Uani 1 1 d . . . . .
H24 H -0.613744 -0.207150 -0.666824 0.059 Uiso 1 1 calc R . . . .
C34 C -0.78088(17) -0.4662(5) -0.8127(3) 0.0558(12) Uani 1 1 d . . . . .
H34 H -0.802878 -0.508575 -0.836671 0.067 Uiso 1 1 calc R . . . .
C28 C -0.80185(17) -0.4304(6) -0.5953(3) 0.0553(12) Uani 1 1 d . . . . .
H28 H -0.804731 -0.467485 -0.644223 0.066 Uiso 1 1 calc R . . . .
C33 C -0.78485(17) -0.3338(5) -0.7916(3) 0.0565(12) Uani 1 1 d . . . . .
C19 C -0.73634(16) -0.8469(5) -0.5778(3) 0.0537(11) Uani 1 1 d . . . . .
H19 H -0.756527 -0.911075 -0.570520 0.064 Uiso 1 1 calc R . . . .
C7 C -0.38551(18) -0.9815(6) -0.3175(3) 0.0580(13) Uani 1 1 d . . . . .
C31 C -0.71475(16) -0.3385(5) -0.7445(3) 0.0514(11) Uani 1 1 d . . . . .
H31 H -0.692353 -0.295816 -0.722063 0.062 Uiso 1 1 calc R . . . .
C8 C -0.40309(19) -0.8546(6) -0.3190(3) 0.0597(13) Uani 1 1 d . . . . .
H8 H -0.386507 -0.780974 -0.310365 0.072 Uiso 1 1 calc R . . . .
C10 C -0.46884(17) -0.9463(5) -0.3471(3) 0.0534(12) Uani 1 1 d . . . . .
C29 C -0.76543(16) -0.4450(5) -0.5568(3) 0.0509(11) Uani 1 1 d . . . . .
H29 H -0.743930 -0.491798 -0.579459 0.061 Uiso 1 1 calc R . . . .
C12 C -0.41066(19) -1.0884(5) -0.3346(3) 0.0595(13) Uani 1 1 d . . . . .
H12 H -0.399354 -1.172871 -0.336135 0.071 Uiso 1 1 calc R . . . .
C9 C -0.44400(18) -0.8378(5) -0.3328(3) 0.0560(13) Uani 1 1 d . . . . .
H9 H -0.455301 -0.753197 -0.332581 0.067 Uiso 1 1 calc R . . . .
C30 C -0.76039(14) -0.3902(4) -0.4839(3) 0.0433(9) Uani 1 1 d . . . . .
C2 C -0.33677(17) -0.6107(6) -0.4550(3) 0.0627(14) Uani 1 1 d . . . . .
H2 H -0.314959 -0.569958 -0.429516 0.075 Uiso 1 1 calc R . . . .
C4 C -0.40125(15) -0.5944(5) -0.5206(3) 0.0474(10) Uani 1 1 d . . . . .
C32 C -0.75082(18) -0.2706(5) -0.7582(4) 0.0603(13) Uani 1 1 d . . . . .
H32 H -0.752598 -0.181590 -0.745047 0.072 Uiso 1 1 calc R . . . .
C42 C -0.54078(19) -0.3188(5) -0.5712(5) 0.077(2) Uani 1 1 d . . . . .
H42A H -0.529407 -0.286925 -0.618980 0.116 Uiso 1 1 calc GR . . . .
H42B H -0.519635 -0.320702 -0.532437 0.116 Uiso 1 1 calc GR . . . .
H42C H -0.562598 -0.261037 -0.554875 0.116 Uiso 1 1 calc GR . . . .
C26 C -0.82957(17) -0.3089(5) -0.4881(3) 0.0573(13) Uani 1 1 d . . . . .
H26 H -0.851454 -0.266053 -0.464083 0.069 Uiso 1 1 calc R . . . .
C27 C -0.83491(16) -0.3612(5) -0.5631(3) 0.0545(12) Uani 1 1 d . . . . .
C1 C -0.33630(16) -0.7463(5) -0.4656(3) 0.0569(12) Uani 1 1 d . . . . .
C6 C -0.36886(19) -0.8039(6) -0.5062(4) 0.0651(14) Uani 1 1 d . . . . .
H6 H -0.368715 -0.894547 -0.515313 0.078 Uiso 1 1 calc R . . . .
N1 N -0.34493(17) -0.9995(6) -0.2966(4) 0.0758(15) Uani 1 1 d . . . . .
H1A H -0.336587 -1.076606 -0.311429 0.091 Uiso 1 1 d GR . . . .
H1B H -0.330087 -0.939756 -0.318907 0.091 Uiso 1 1 d GR . . . .
C20 C -0.71332(14) -0.7941(5) -0.5209(3) 0.0464(10) Uani 1 1 d . . . . .
H20 H -0.716229 -0.818642 -0.469371 0.056 Uiso 1 1 calc R . . . .
C38 C -0.61984(17) -0.8911(5) -0.4672(4) 0.0612(14) Uani 1 1 d . . . . .
H38A H -0.621162 -0.936631 -0.418568 0.092 Uiso 1 1 calc GR . . . .
H38B H -0.598006 -0.927746 -0.497948 0.092 Uiso 1 1 calc GR . . . .
H38C H -0.645557 -0.901124 -0.494003 0.092 Uiso 1 1 calc GR . . . .
O14 O -0.61498(18) -0.9797(6) -0.2550(4) 0.0995(17) Uani 1 1 d . . . . .
H14A H -0.590844 -0.957296 -0.260138 0.149 Uiso 1 1 calc GR . . . .
N3 N -0.82105(16) -0.2661(6) -0.8043(4) 0.0805(16) Uani 1 1 d . . . . .
H3A H -0.841707 -0.309836 -0.785906 0.097 Uiso 1 1 d GR . . . .
H3B H -0.819625 -0.190677 -0.780859 0.097 Uiso 1 1 d GR . . . .
C13 C -0.4797(2) -0.9808(6) -0.6261(4) 0.0701(17) Uani 1 1 d . . . . .
H13 H -0.467846 -1.034187 -0.663841 0.084 Uiso 1 1 calc R . . . .
O13 O -0.7000(3) -0.4730(9) -0.2217(4) 0.137(3) Uani 1 1 d . . . . .
H13A H -0.697729 -0.444154 -0.265798 0.205 Uiso 1 1 calc GR . . . .
C37 C -0.58890(19) -0.7809(5) -0.6564(4) 0.0692(17) Uani 1 1 d . . . . .
H37A H -0.605508 -0.826313 -0.618880 0.104 Uiso 1 1 calc GR . . . .
H37B H -0.564719 -0.832321 -0.667330 0.104 Uiso 1 1 calc GR . . . .
H37C H -0.604471 -0.768751 -0.703023 0.104 Uiso 1 1 calc GR . . . .
C3 C -0.36893(17) -0.5356(6) -0.4815(4) 0.0599(13) Uani 1 1 d . . . . .
H3 H -0.369027 -0.444737 -0.473173 0.072 Uiso 1 1 calc R . . . .
C11 C -0.4516(2) -1.0722(5) -0.3492(4) 0.0639(14) Uani 1 1 d . . . . .
H11 H -0.467984 -1.145212 -0.360432 0.077 Uiso 1 1 calc R . . . .
C41 C -0.5973(2) -0.4034(5) -0.3882(4) 0.0719(18) Uani 1 1 d . . . . .
H41A H -0.571441 -0.369757 -0.406507 0.108 Uiso 1 1 calc GR . . . .
H41B H -0.597612 -0.402329 -0.332735 0.108 Uiso 1 1 calc GR . . . .
H41C H -0.619316 -0.348944 -0.407463 0.108 Uiso 1 1 calc GR . . . .
C39 C -0.6176(3) -1.1172(10) -0.2550(7) 0.120(3) Uani 1 1 d . . . . .
H39A H -0.642596 -1.144028 -0.280239 0.181 Uiso 1 1 calc GR . . . .
H39B H -0.617633 -1.148970 -0.202691 0.181 Uiso 1 1 calc GR . . . .
H39C H -0.594382 -1.153493 -0.282099 0.181 Uiso 1 1 calc GR . . . .
C40 C -0.6644(4) -0.4545(18) -0.1835(8) 0.172(6) Uani 1 1 d . . . . .
H40A H -0.641829 -0.483192 -0.215105 0.259 Uiso 1 1 calc GR . . . .
H40B H -0.664810 -0.504800 -0.136383 0.259 Uiso 1 1 calc GR . . . .
H40C H -0.661260 -0.362302 -0.171559 0.259 Uiso 1 1 calc GR . . . .


_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
Cu3 Cu4 2.9220(9) . ?
Cu3 O9 1.913(3) . ?
Cu3 O10 1.923(3) . ?
Cu3 N12 1.973(4) . ?
Cu3 N9 2.033(3) . ?
Cu2 Cu1 2.9057(9) . ?
Cu2 O9 1.924(3) . ?
Cu2 O10 1.906(3) . ?
Cu2 N5 1.957(4) . ?
Cu2 N7 2.003(3) . ?
Cu4 O11 1.936(3) . ?
Cu4 O12 1.910(3) . ?
Cu4 N10 1.977(4) . ?
Cu4 N11 2.035(3) . ?
Cu1 O11 1.913(3) . ?
Cu1 O12 1.932(3) . ?
Cu1 N8 1.963(4) . ?
Cu1 N6 2.040(4) . ?
S6 O6 1.439(3) . ?
S6 O5 1.441(3) . ?
S6 N9 1.624(4) . ?
S6 C36 1.753(5) . ?
S8 O7 1.444(4) . ?
S8 O8 1.439(4) . ?
S8 N11 1.615(4) . ?
S8 C30 1.751(5) . ?
S5 C21 1.746(4) . ?
S5 C19 1.718(6) . ?
S2 O4 1.442(4) . ?
S2 O3 1.437(4) . ?
S2 N7 1.623(4) . ?
S2 C4 1.755(5) . ?
S3 N6 1.611(4) . ?
S3 O2 1.441(5) . ?
S3 O1 1.438(4) . ?
S3 C10 1.753(6) . ?
S7 C22 1.743(4) . ?
S7 C23 1.710(6) . ?
S4 C17 1.719(6) . ?
S4 C16 1.731(4) . ?
S1 C15 1.737(4) . ?
S1 C13 1.720(8) . ?
O9 C37 1.406(6) . ?
O10 C42 1.407(6) . ?
O11 C38 1.405(5) . ?
O12 C41 1.421(5) . ?
N5 C15 1.317(6) . ?
N5 C14 1.388(6) . ?
N8 C18 1.392(6) . ?
N8 C16 1.329(6) . ?
N10 C21 1.326(6) . ?
N10 C20 1.386(6) . ?
N11 C22 1.364(6) . ?
N6 C15 1.362(6) . ?
N7 C16 1.360(6) . ?
N12 C22 1.312(6) . ?
N12 C24 1.393(6) . ?
N9 C21 1.348(5) . ?
C36 C35 1.392(7) . ?
C36 C31 1.390(7) . ?
C25 H25 0.9300 . ?
C25 C30 1.394(6) . ?
C25 C26 1.367(8) . ?
C18 H18 0.9300 . ?
C18 C17 1.314(8) . ?
N2 H2A 0.8702 . ?
N2 H2B 0.8683 . ?
N2 C1 1.380(7) . ?
C17 H17 0.9300 . ?
N4 H4A 0.8621 . ?
N4 H4B 0.8618 . ?
N4 C27 1.357(7) . ?
C35 H35 0.9300 . ?
C35 C34 1.365(7) . ?
C23 H23 0.9300 . ?
C23 C24 1.342(7) . ?
C14 H14 0.9300 . ?
C14 C13 1.342(8) . ?
C5 H5 0.9300 . ?
C5 C4 1.380(7) . ?
C5 C6 1.358(8) . ?
C24 H24 0.9300 . ?
C34 H34 0.9300 . ?
C34 C33 1.393(8) . ?
C28 H28 0.9300 . ?
C28 C29 1.365(8) . ?
C28 C27 1.397(7) . ?
C33 C32 1.400(8) . ?
C33 N3 1.377(7) . ?
C19 H19 0.9300 . ?
C19 C20 1.346(7) . ?
C7 C8 1.405(8) . ?
C7 C12 1.385(8) . ?
C7 N1 1.377(8) . ?
C31 H31 0.9300 . ?
C31 C32 1.377(8) . ?
C8 H8 0.9300 . ?
C8 C9 1.359(8) . ?
C10 C9 1.383(8) . ?
C10 C11 1.391(7) . ?
C29 H29 0.9300 . ?
C29 C30 1.386(7) . ?
C12 H12 0.9300 . ?
C12 C11 1.362(9) . ?
C9 H9 0.9300 . ?
C2 H2 0.9300 . ?
C2 C1 1.382(8) . ?
C2 C3 1.369(8) . ?
C4 C3 1.382(7) . ?
C32 H32 0.9300 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C26 H26 0.9300 . ?
C26 C27 1.410(8) . ?
C1 C6 1.395(9) . ?
C6 H6 0.9300 . ?
N1 H1A 0.8635 . ?
N1 H1B 0.8631 . ?
C20 H20 0.9300 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
O14 H14A 0.8200 . ?
O14 C39 1.393(11) . ?
N3 H3A 0.8636 . ?
N3 H3B 0.8643 . ?
C13 H13 0.9300 . ?
O13 H13A 0.8200 . ?
O13 C40 1.342(14) . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C3 H3 0.9300 . ?
C11 H11 0.9300 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O9 Cu3 Cu4 91.29(10) . . ?
O9 Cu3 O10 75.67(13) . . ?
O9 Cu3 N12 169.32(15) . . ?
O9 Cu3 N9 95.06(13) . . ?
O10 Cu3 Cu4 102.92(11) . . ?
O10 Cu3 N12 95.59(14) . . ?
O10 Cu3 N9 170.71(14) . . ?
N12 Cu3 Cu4 84.63(11) . . ?
N12 Cu3 N9 93.70(15) . . ?
N9 Cu3 Cu4 77.62(10) . . ?
O9 Cu2 Cu1 94.38(10) . . ?
O9 Cu2 N5 93.05(14) . . ?
O9 Cu2 N7 169.90(14) . . ?
O10 Cu2 Cu1 95.39(12) . . ?
O10 Cu2 O9 75.82(13) . . ?
O10 Cu2 N5 168.87(14) . . ?
O10 Cu2 N7 96.41(14) . . ?
N5 Cu2 Cu1 85.56(12) . . ?
N5 Cu2 N7 94.67(16) . . ?
N7 Cu2 Cu1 79.76(11) . . ?
O11 Cu4 Cu3 100.86(10) . . ?
O11 Cu4 N10 95.22(13) . . ?
O11 Cu4 N11 171.83(14) . . ?
O12 Cu4 Cu3 90.26(12) . . ?
O12 Cu4 O11 75.45(13) . . ?
O12 Cu4 N10 168.41(14) . . ?
O12 Cu4 N11 96.49(14) . . ?
N10 Cu4 Cu3 84.70(11) . . ?
N10 Cu4 N11 92.61(15) . . ?
N11 Cu4 Cu3 77.54(11) . . ?
O11 Cu1 Cu2 98.51(10) . . ?
O11 Cu1 O12 75.48(13) . . ?
O11 Cu1 N8 170.86(14) . . ?
O11 Cu1 N6 96.00(14) . . ?
O12 Cu1 Cu2 98.38(12) . . ?
O12 Cu1 N8 95.41(14) . . ?
O12 Cu1 N6 169.96(15) . . ?
N8 Cu1 Cu2 83.37(11) . . ?
N8 Cu1 N6 93.15(16) . . ?
N6 Cu1 Cu2 77.39(11) . . ?
O6 S6 O5 118.4(2) . . ?
O6 S6 N9 111.2(2) . . ?
O6 S6 C36 107.2(2) . . ?
O5 S6 N9 102.65(19) . . ?
O5 S6 C36 108.9(2) . . ?
N9 S6 C36 108.3(2) . . ?
O7 S8 N11 103.1(2) . . ?
O7 S8 C30 109.5(2) . . ?
O8 S8 O7 116.6(2) . . ?
O8 S8 N11 112.5(2) . . ?
O8 S8 C30 107.5(2) . . ?
N11 S8 C30 107.4(2) . . ?
C19 S5 C21 90.2(2) . . ?
O4 S2 N7 111.1(2) . . ?
O4 S2 C4 107.1(2) . . ?
O3 S2 O4 118.1(3) . . ?
O3 S2 N7 103.0(2) . . ?
O3 S2 C4 109.7(3) . . ?
N7 S2 C4 107.4(2) . . ?
N6 S3 C10 107.5(2) . . ?
O2 S3 N6 102.7(2) . . ?
O2 S3 C10 109.9(3) . . ?
O1 S3 N6 112.1(3) . . ?
O1 S3 O2 117.1(3) . . ?
O1 S3 C10 107.3(3) . . ?
C23 S7 C22 89.8(2) . . ?
C17 S4 C16 89.9(2) . . ?
C13 S1 C15 90.4(3) . . ?
Cu3 O9 Cu2 102.70(13) . . ?
C37 O9 Cu3 128.0(3) . . ?
C37 O9 Cu2 128.4(3) . . ?
Cu2 O10 Cu3 103.02(14) . . ?
C42 O10 Cu3 129.3(3) . . ?
C42 O10 Cu2 127.6(3) . . ?
Cu1 O11 Cu4 102.48(13) . . ?
C38 O11 Cu4 129.2(3) . . ?
C38 O11 Cu1 128.1(3) . . ?
Cu4 O12 Cu1 102.75(14) . . ?
C41 O12 Cu4 127.9(3) . . ?
C41 O12 Cu1 128.0(3) . . ?
C15 N5 Cu2 124.3(3) . . ?
C15 N5 C14 112.1(4) . . ?
C14 N5 Cu2 123.5(4) . . ?
C18 N8 Cu1 122.7(3) . . ?
C16 N8 Cu1 125.9(3) . . ?
C16 N8 C18 111.1(4) . . ?
C21 N10 Cu4 124.1(3) . . ?
C21 N10 C20 112.2(4) . . ?
C20 N10 Cu4 123.7(3) . . ?
S8 N11 Cu4 110.81(19) . . ?
C22 N11 Cu4 128.4(3) . . ?
C22 N11 S8 120.3(3) . . ?
S3 N6 Cu1 110.9(2) . . ?
C15 N6 Cu1 128.2(3) . . ?
C15 N6 S3 120.2(3) . . ?
S2 N7 Cu2 111.0(2) . . ?
C16 N7 Cu2 127.5(3) . . ?
C16 N7 S2 121.4(3) . . ?
C22 N12 Cu3 124.3(3) . . ?
C22 N12 C24 112.1(4) . . ?
C24 N12 Cu3 123.2(3) . . ?
S6 N9 Cu3 107.49(18) . . ?
C21 N9 Cu3 128.6(3) . . ?
C21 N9 S6 122.3(3) . . ?
N5 C15 S1 112.3(3) . . ?
N5 C15 N6 121.5(4) . . ?
N6 C15 S1 126.2(4) . . ?
C35 C36 S6 120.6(4) . . ?
C31 C36 S6 118.9(4) . . ?
C31 C36 C35 120.5(5) . . ?
C30 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C26 C25 C30 120.1(5) . . ?
N10 C21 S5 112.1(3) . . ?
N10 C21 N9 121.8(4) . . ?
N9 C21 S5 126.1(3) . . ?
N8 C18 H18 122.3 . . ?
C17 C18 N8 115.5(5) . . ?
C17 C18 H18 122.3 . . ?
H2A N2 H2B 107.8 . . ?
C1 N2 H2A 111.6 . . ?
C1 N2 H2B 108.2 . . ?
S4 C17 H17 124.5 . . ?
C18 C17 S4 111.0(4) . . ?
C18 C17 H17 124.5 . . ?
N11 C22 S7 125.6(3) . . ?
N12 C22 S7 112.6(3) . . ?
N12 C22 N11 121.8(4) . . ?
H4A N4 H4B 109.0 . . ?
C27 N4 H4A 108.4 . . ?
C27 N4 H4B 110.2 . . ?
N8 C16 S4 112.5(3) . . ?
N8 C16 N7 121.5(4) . . ?
N7 C16 S4 126.0(4) . . ?
C36 C35 H35 120.3 . . ?
C34 C35 C36 119.5(5) . . ?
C34 C35 H35 120.3 . . ?
S7 C23 H23 124.4 . . ?
C24 C23 S7 111.2(4) . . ?
C24 C23 H23 124.4 . . ?
N5 C14 H14 122.5 . . ?
C13 C14 N5 115.0(5) . . ?
C13 C14 H14 122.5 . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C6 C5 C4 120.4(5) . . ?
N12 C24 H24 122.9 . . ?
C23 C24 N12 114.3(5) . . ?
C23 C24 H24 122.9 . . ?
C35 C34 H34 119.2 . . ?
C35 C34 C33 121.5(5) . . ?
C33 C34 H34 119.2 . . ?
C29 C28 H28 119.2 . . ?
C29 C28 C27 121.6(5) . . ?
C27 C28 H28 119.2 . . ?
C34 C33 C32 118.2(5) . . ?
N3 C33 C34 120.9(5) . . ?
N3 C33 C32 120.8(5) . . ?
S5 C19 H19 124.7 . . ?
C20 C19 S5 110.6(4) . . ?
C20 C19 H19 124.7 . . ?
C12 C7 C8 118.0(5) . . ?
N1 C7 C8 120.9(6) . . ?
N1 C7 C12 121.1(5) . . ?
C36 C31 H31 120.3 . . ?
C32 C31 C36 119.3(5) . . ?
C32 C31 H31 120.3 . . ?
C7 C8 H8 119.5 . . ?
C9 C8 C7 120.9(5) . . ?
C9 C8 H8 119.5 . . ?
C9 C10 S3 121.1(4) . . ?
C9 C10 C11 119.7(5) . . ?
C11 C10 S3 119.1(5) . . ?
C28 C29 H29 119.9 . . ?
C28 C29 C30 120.2(4) . . ?
C30 C29 H29 119.9 . . ?
C7 C12 H12 119.3 . . ?
C11 C12 C7 121.4(5) . . ?
C11 C12 H12 119.3 . . ?
C8 C9 C10 120.1(5) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
C25 C30 S8 118.7(4) . . ?
C29 C30 S8 121.5(3) . . ?
C29 C30 C25 119.6(5) . . ?
C1 C2 H2 119.6 . . ?
C3 C2 H2 119.6 . . ?
C3 C2 C1 120.9(5) . . ?
C5 C4 S2 120.5(4) . . ?
C5 C4 C3 119.3(5) . . ?
C3 C4 S2 120.2(4) . . ?
C33 C32 H32 119.5 . . ?
C31 C32 C33 121.0(5) . . ?
C31 C32 H32 119.5 . . ?
O10 C42 H42A 109.5 . . ?
O10 C42 H42B 109.5 . . ?
O10 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C25 C26 H26 119.5 . . ?
C25 C26 C27 121.1(5) . . ?
C27 C26 H26 119.5 . . ?
N4 C27 C28 122.3(5) . . ?
N4 C27 C26 120.2(5) . . ?
C28 C27 C26 117.4(5) . . ?
N2 C1 C2 120.9(6) . . ?
N2 C1 C6 120.8(6) . . ?
C2 C1 C6 118.2(5) . . ?
C5 C6 C1 120.9(5) . . ?
C5 C6 H6 119.5 . . ?
C1 C6 H6 119.5 . . ?
C7 N1 H1A 109.9 . . ?
C7 N1 H1B 108.9 . . ?
H1A N1 H1B 108.9 . . ?
N10 C20 H20 122.6 . . ?
C19 C20 N10 114.9(4) . . ?
C19 C20 H20 122.6 . . ?
O11 C38 H38A 109.5 . . ?
O11 C38 H38B 109.5 . . ?
O11 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C39 O14 H14A 109.5 . . ?
C33 N3 H3A 110.4 . . ?
C33 N3 H3B 108.5 . . ?
H3A N3 H3B 108.7 . . ?
S1 C13 H13 124.9 . . ?
C14 C13 S1 110.2(4) . . ?
C14 C13 H13 124.9 . . ?
C40 O13 H13A 109.5 . . ?
O9 C37 H37A 109.5 . . ?
O9 C37 H37B 109.5 . . ?
O9 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C2 C3 C4 120.3(5) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
C10 C11 H11 120.1 . . ?
C12 C11 C10 119.8(6) . . ?
C12 C11 H11 120.1 . . ?
O12 C41 H41A 109.5 . . ?
O12 C41 H41B 109.5 . . ?
O12 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O14 C39 H39A 109.5 . . ?
O14 C39 H39B 109.5 . . ?
O14 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O13 C40 H40A 109.5 . . ?
O13 C40 H40B 109.5 . . ?
O13 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?

_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 2.232
_oxdiff_exptl_absorpt_empirical_full_min 0.631
####################################################################### 
# 
# 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_kj-40-1
_database_code_depnum_ccdc_archive 'CCDC 1938521'
loop_
_audit_author_name
_audit_author_address
'Juan Kang'
;Tianjin University
China
;
_audit_update_record             
;
2019-07-05 deposited with the CCDC.	2019-09-27 downloaded from the CCDC.
;
_audit_creation_date             2019-04-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C36 H38 N12 Ni2 O11 S8'
_chemical_formula_sum            'C36 H38 N12 Ni2 O11 S8'
_chemical_formula_weight         1188.68
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 1 2/n 1'
_space_group_name_Hall           '-P 2yac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z-1/2'

_cell_length_a                   12.0094(4)
_cell_length_b                   12.8836(6)
_cell_length_c                   17.3263(7)
_cell_angle_alpha                90
_cell_angle_beta                 92.444(4)
_cell_angle_gamma                90
_cell_volume                     2678.36(19)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5375
_cell_measurement_temperature    159.99(10)
_cell_measurement_theta_max      76.2030
_cell_measurement_theta_min      3.4550
_shelx_estimated_absorpt_T_max   0.918
_shelx_estimated_absorpt_T_min   0.918
_exptl_absorpt_coefficient_mu    4.328
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47664
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.45g (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1412
_diffrn_reflns_av_unetI/netI     0.0954
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25790
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.175
_diffrn_reflns_theta_min         3.430
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      159.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     19.00 118.00   0.50    0.66    --   46.12  84.00 -73.00  198
  2  ω     73.00 118.00   0.50    0.66    --   46.12 125.00-150.00   90
  3  ω     73.00 118.00   0.50    0.66    --   46.12 125.00-120.00   90
  4  ω     81.00 178.00   0.50    2.64    --  107.31  84.00 -73.00  194
  5  ω     93.00 155.00   0.50    2.64    --  107.31  45.00 -60.00  124
  6  ω     73.00  98.00   0.50    0.66    --   46.12 125.00 120.00   50
  7  ω    -26.00  73.00   0.50    0.66    --   46.12 -84.00 166.00  198
  8  ω     35.00 134.00   0.50    2.64    --  107.31 -84.00 166.00  198
  9  ω     38.00  89.00   0.50    2.64    --  107.31-125.00 150.00  102
 10  ω     36.00 107.00   0.50    2.64    --  107.31 -94.00   0.00  142
 11  ω    -73.00  27.00   0.50    0.66    --  -46.12  84.00 -73.00  200
 12  ω   -118.00 -19.00   0.50    0.66    --  -46.12 -84.00 166.00  198
 13  ω   -118.00 -24.00   0.50    2.64    -- -100.00  15.00-150.00  188
 14  ω   -114.00 -25.00   0.50    2.64    -- -100.00  30.00 -60.00  178
 15  ω   -117.00 -83.00   0.50    2.64    -- -100.00 -15.00   0.00   68
 16  ω   -127.00 -27.00   0.50    2.64    -- -100.00  84.00 -73.00  200
 17  ω   -173.00 -73.00   0.50    2.64    -- -100.00 -84.00 166.00  200
 18  ω   -173.00-144.00   0.50    2.64    -- -100.00 -15.00   0.00   58
 19  ω   -164.00 -87.00   0.50    2.64    -- -100.00 -94.00-120.00  154
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0871412000
_diffrn_orient_matrix_UB_12      -0.0730117000
_diffrn_orient_matrix_UB_13      -0.0389102000
_diffrn_orient_matrix_UB_21      0.0934867000
_diffrn_orient_matrix_UB_22      -0.0757802000
_diffrn_orient_matrix_UB_23      -0.0205774000
_diffrn_orient_matrix_UB_31      -0.0126976000
_diffrn_orient_matrix_UB_32      -0.0567623000
_diffrn_orient_matrix_UB_33      0.0773309000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3275
_reflns_number_total             5352
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.032
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.188
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         5352
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1173
_refine_ls_R_factor_gt           0.0799
_refine_ls_restrained_S_all      0.978
_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)+(0.1453P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1988
_refine_ls_wR_factor_ref         0.2335
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: H5A(0.5) H5B(0.5)
 Fixed X: H5A(0.7876) H5B(0.68944)
 Fixed Y: H5A(0.296529) H5B(0.2958)
 Fixed Z: H5A(0.22561) H5B(0.26008)
3.a Rotating group:
 O6(H6A,H6B), N1(H1A,H1B), N5(H5C,H5D)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14),
 C15(H15), C17(H17), C18(H18)
;
_atom_sites_solution_hydrogens   mixed
_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 0.81115(7) 0.41380(7) 0.34167(5) 0.0411(3) Uani 1 1 d . . . . .
S1 S 0.64910(14) 0.18442(15) 0.50233(10) 0.0635(5) Uani 1 1 d . . . . .
S2 S 0.52811(11) 0.15746(12) 0.32975(9) 0.0503(4) Uani 1 1 d . . . . .
S3 S 0.49868(11) 0.62150(13) 0.33847(9) 0.0512(4) Uani 1 1 d . . . . .
S4 S 0.55121(10) 0.59056(11) 0.15931(8) 0.0409(3) Uani 1 1 d . . . . .
O1 O 0.5908(3) 0.5380(3) 0.0903(2) 0.0466(9) Uani 1 1 d . . . . .
O2 O 0.4315(3) 0.5913(3) 0.1681(2) 0.0486(10) Uani 1 1 d . . . . .
O3 O 0.5332(3) 0.0606(3) 0.3716(3) 0.0629(12) Uani 1 1 d . . . . .
O4 O 0.5163(3) 0.1502(4) 0.2467(2) 0.0558(11) Uani 1 1 d . . . . .
O5 O 0.750000 0.3285(4) 0.250000 0.0462(13) Uani 1 2 d S T P . .
H5A H 0.787600 0.296529 0.225610 0.069 Uiso 0.5 1 d R . . . .
H5B H 0.689440 0.295800 0.260080 0.069 Uiso 0.5 1 d R . . . .
O6 O 0.9593(3) 0.3314(3) 0.3401(3) 0.0564(11) Uani 1 1 d . . . . .
H6A H 1.014748 0.373178 0.345158 0.085 Uiso 1 1 d GR . . . .
H6B H 0.966047 0.304666 0.295199 0.085 Uiso 1 1 d GR . . . .
N1 N 0.7021(5) 1.0251(5) 0.1585(5) 0.0789(18) Uani 1 1 d . . . . .
H1A H 0.704151 1.044826 0.111136 0.095 Uiso 1 1 d GR . . . .
H1B H 0.655699 1.063156 0.182185 0.095 Uiso 1 1 d GR . . . .
N2 N 0.6194(3) 0.5278(4) 0.2254(2) 0.0403(10) Uani 1 1 d . . . . .
N3 N 0.6664(3) 0.4972(4) 0.3553(3) 0.0414(10) Uani 1 1 d . . . . .
N4 N 0.7631(4) 0.3153(4) 0.4260(3) 0.0498(12) Uani 1 1 d . . . . .
N5 N 0.1405(4) 0.4005(5) 0.4289(3) 0.0603(14) Uani 1 1 d . . . . .
H5C H 0.142349 0.380561 0.476278 0.072 Uiso 1 1 d GR . . . .
H5D H 0.178901 0.456483 0.424960 0.072 Uiso 1 1 d GR . . . .
N6 N 0.6341(4) 0.2263(4) 0.3451(3) 0.0497(12) Uani 1 1 d . . . . .
C1 C 0.2354(4) 0.3429(5) 0.4083(4) 0.0519(15) Uani 1 1 d . . . . .
C2 C 0.2575(5) 0.2455(6) 0.4397(4) 0.0592(17) Uani 1 1 d . . . . .
H2 H 0.210958 0.218638 0.476314 0.071 Uiso 1 1 calc R . . . .
C3 C 0.3472(5) 0.1884(6) 0.4175(4) 0.0589(16) Uani 1 1 d . . . . .
H3 H 0.362422 0.123772 0.439387 0.071 Uiso 1 1 calc R . . . .
C4 C 0.4141(5) 0.2287(5) 0.3623(4) 0.0542(15) Uani 1 1 d . . . . .
C5 C 0.3930(5) 0.3261(5) 0.3294(4) 0.0591(16) Uani 1 1 d . . . . .
H5 H 0.438309 0.351432 0.291506 0.071 Uiso 1 1 calc R . . . .
C6 C 0.3049(5) 0.3842(5) 0.3533(4) 0.0568(15) Uani 1 1 d . . . . .
H6 H 0.291679 0.450218 0.333172 0.068 Uiso 1 1 calc R . . . .
C7 C 0.6817(4) 0.2464(5) 0.4174(3) 0.0474(13) Uani 1 1 d . . . . .
C8 C 0.7494(6) 0.2578(6) 0.5509(4) 0.0680(19) Uani 1 1 d . . . . .
H8 H 0.764908 0.254376 0.603896 0.082 Uiso 1 1 calc R . . . .
C9 C 0.8019(5) 0.3198(6) 0.5031(4) 0.0575(16) Uani 1 1 d . . . . .
H9 H 0.860062 0.362976 0.519796 0.069 Uiso 1 1 calc R . . . .
C10 C 0.6324(4) 0.5241(5) 0.4278(3) 0.0468(13) Uani 1 1 d . . . . .
H10 H 0.667017 0.497145 0.472499 0.056 Uiso 1 1 calc R . . . .
C11 C 0.5470(5) 0.5908(5) 0.4306(4) 0.0537(15) Uani 1 1 d . . . . .
H11 H 0.518134 0.616729 0.475734 0.064 Uiso 1 1 calc R . . . .
C12 C 0.6020(4) 0.5435(4) 0.3007(3) 0.0396(12) Uani 1 1 d . . . . .
C13 C 0.5951(4) 0.7182(4) 0.1595(3) 0.0420(12) Uani 1 1 d . . . . .
C14 C 0.7031(4) 0.7444(5) 0.1396(3) 0.0475(13) Uani 1 1 d . . . . .
H14 H 0.751817 0.692587 0.125146 0.057 Uiso 1 1 calc R . . . .
C15 C 0.7379(4) 0.8455(5) 0.1413(4) 0.0509(14) Uani 1 1 d . . . . .
H15 H 0.810776 0.860950 0.129272 0.061 Uiso 1 1 calc R . . . .
C16 C 0.6674(5) 0.9247(5) 0.1604(4) 0.0538(15) Uani 1 1 d . . . . .
C17 C 0.5600(5) 0.8983(5) 0.1842(4) 0.0592(17) Uani 1 1 d . . . . .
H17 H 0.512959 0.949971 0.201242 0.071 Uiso 1 1 calc R . . . .
C18 C 0.5245(4) 0.7974(5) 0.1824(4) 0.0520(14) Uani 1 1 d . . . . .
H18 H 0.452626 0.781512 0.196559 0.062 Uiso 1 1 calc R . . . .


_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 O1 2.284(4) 2_655 ?
Ni1 O5 2.042(3) . ?
Ni1 O6 2.073(4) . ?
Ni1 N2 2.070(5) 2_655 ?
Ni1 N3 2.065(4) . ?
Ni1 N4 2.038(5) . ?
S1 C7 1.734(6) . ?
S1 C8 1.722(8) . ?
S2 O3 1.443(5) . ?
S2 O4 1.443(5) . ?
S2 N6 1.565(5) . ?
S2 C4 1.761(6) . ?
S3 C11 1.722(6) . ?
S3 C12 1.747(6) . ?
S4 O1 1.470(4) . ?
S4 O2 1.452(4) . ?
S4 N2 1.598(4) . ?
S4 C13 1.726(6) . ?
O5 H5A 0.754(3) . ?
O5 H5A 0.754(3) 2_655 ?
O5 H5B 0.864(3) 2_655 ?
O5 H5B 0.864(3) . ?
O6 H6A 0.8577 . ?
O6 H6B 0.8576 . ?
N1 H1A 0.8601 . ?
N1 H1B 0.8597 . ?
N1 C16 1.360(8) . ?
N2 C12 1.345(7) . ?
N3 C10 1.383(7) . ?
N3 C12 1.336(6) . ?
N4 C7 1.324(7) . ?
N4 C9 1.397(8) . ?
N5 H5C 0.8599 . ?
N5 H5D 0.8601 . ?
N5 C1 1.418(8) . ?
N6 C7 1.378(7) . ?
C1 C2 1.389(9) . ?
C1 C6 1.398(9) . ?
C2 H2 0.9300 . ?
C2 C3 1.372(9) . ?
C3 H3 0.9300 . ?
C3 C4 1.377(9) . ?
C4 C5 1.397(9) . ?
C5 H5 0.9300 . ?
C5 C6 1.375(9) . ?
C6 H6 0.9300 . ?
C8 H8 0.9300 . ?
C8 C9 1.328(10) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C10 C11 1.341(8) . ?
C11 H11 0.9300 . ?
C13 C14 1.397(8) . ?
C13 C18 1.396(8) . ?
C14 H14 0.9300 . ?
C14 C15 1.367(8) . ?
C15 H15 0.9300 . ?
C15 C16 1.375(9) . ?
C16 C17 1.413(9) . ?
C17 H17 0.9300 . ?
C17 C18 1.367(9) . ?
C18 H18 0.9300 . ?

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
O5 Ni1 O1 159.83(14) . 2_655 ?
O5 Ni1 O6 89.68(15) . . ?
O5 Ni1 N2 94.92(16) . 2_655 ?
O5 Ni1 N3 95.29(15) . . ?
O6 Ni1 O1 86.64(15) . 2_655 ?
N2 Ni1 O1 65.25(15) 2_655 2_655 ?
N2 Ni1 O6 89.40(18) 2_655 . ?
N3 Ni1 O1 89.70(16) . 2_655 ?
N3 Ni1 O6 174.16(17) . . ?
N3 Ni1 N2 93.20(18) . 2_655 ?
N4 Ni1 O1 102.82(17) . 2_655 ?
N4 Ni1 O5 96.83(18) . . ?
N4 Ni1 O6 87.69(19) . . ?
N4 Ni1 N2 167.88(18) . 2_655 ?
N4 Ni1 N3 88.69(19) . . ?
C8 S1 C7 89.1(3) . . ?
O3 S2 N6 112.8(3) . . ?
O3 S2 C4 107.9(3) . . ?
O4 S2 O3 116.4(3) . . ?
O4 S2 N6 104.6(3) . . ?
O4 S2 C4 107.9(3) . . ?
N6 S2 C4 106.8(3) . . ?
C11 S3 C12 89.9(3) . . ?
O1 S4 N2 100.1(2) . . ?
O1 S4 C13 109.3(3) . . ?
O2 S4 O1 116.4(2) . . ?
O2 S4 N2 114.0(2) . . ?
O2 S4 C13 107.3(2) . . ?
N2 S4 C13 109.5(2) . . ?
S4 O1 Ni1 94.65(18) . 2_655 ?
Ni1 O5 Ni1 114.9(3) 2_655 . ?
Ni1 O5 H5A 121.72(8) 2_655 2_655 ?
Ni1 O5 H5A 121.72(8) . . ?
Ni1 O5 H5A 93.55(14) . 2_655 ?
Ni1 O5 H5A 93.55(14) 2_655 . ?
Ni1 O5 H5B 112.50(10) 2_655 2_655 ?
Ni1 O5 H5B 98.13(12) 2_655 . ?
Ni1 O5 H5B 112.49(10) . . ?
Ni1 O5 H5B 98.13(12) . 2_655 ?
H5A O5 H5A 113.8(7) . 2_655 ?
H5A O5 H5B 112.2(6) . . ?
H5A O5 H5B 24.73(9) . 2_655 ?
H5A O5 H5B 112.2(6) 2_655 2_655 ?
H5B O5 H5A 24.73(9) . 2_655 ?
H5B O5 H5B 121.8(7) . 2_655 ?
Ni1 O6 H6A 109.9 . . ?
Ni1 O6 H6B 109.4 . . ?
H6A O6 H6B 104.0 . . ?
H1A N1 H1B 109.4 . . ?
C16 N1 H1A 108.9 . . ?
C16 N1 H1B 109.0 . . ?
S4 N2 Ni1 99.4(2) . 2_655 ?
C12 N2 Ni1 137.2(4) . 2_655 ?
C12 N2 S4 121.5(4) . . ?
C10 N3 Ni1 121.1(3) . . ?
C12 N3 Ni1 128.0(4) . . ?
C12 N3 C10 110.3(5) . . ?
C7 N4 Ni1 124.5(4) . . ?
C7 N4 C9 110.5(5) . . ?
C9 N4 Ni1 124.6(4) . . ?
H5C N5 H5D 109.5 . . ?
C1 N5 H5C 95.5 . . ?
C1 N5 H5D 88.8 . . ?
C7 N6 S2 124.3(4) . . ?
C2 C1 N5 121.1(6) . . ?
C2 C1 C6 120.1(6) . . ?
C6 C1 N5 118.8(6) . . ?
C1 C2 H2 119.6 . . ?
C3 C2 C1 120.9(6) . . ?
C3 C2 H2 119.6 . . ?
C2 C3 H3 120.6 . . ?
C2 C3 C4 118.8(7) . . ?
C4 C3 H3 120.6 . . ?
C3 C4 S2 120.8(5) . . ?
C3 C4 C5 121.4(6) . . ?
C5 C4 S2 117.9(5) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 C4 119.7(6) . . ?
C6 C5 H5 120.1 . . ?
C1 C6 H6 120.4 . . ?
C5 C6 C1 119.1(6) . . ?
C5 C6 H6 120.4 . . ?
N4 C7 S1 113.9(4) . . ?
N4 C7 N6 120.3(5) . . ?
N6 C7 S1 125.7(4) . . ?
S1 C8 H8 124.3 . . ?
C9 C8 S1 111.5(5) . . ?
C9 C8 H8 124.3 . . ?
N4 C9 H9 122.5 . . ?
C8 C9 N4 115.1(6) . . ?
C8 C9 H9 122.5 . . ?
N3 C10 H10 121.6 . . ?
C11 C10 N3 116.7(5) . . ?
C11 C10 H10 121.6 . . ?
S3 C11 H11 125.0 . . ?
C10 C11 S3 110.0(4) . . ?
C10 C11 H11 125.0 . . ?
N2 C12 S3 126.3(4) . . ?
N3 C12 S3 113.0(4) . . ?
N3 C12 N2 120.7(5) . . ?
C14 C13 S4 121.1(4) . . ?
C18 C13 S4 120.6(4) . . ?
C18 C13 C14 118.3(6) . . ?
C13 C14 H14 119.6 . . ?
C15 C14 C13 120.8(6) . . ?
C15 C14 H14 119.6 . . ?
C14 C15 H15 119.3 . . ?
C14 C15 C16 121.4(5) . . ?
C16 C15 H15 119.3 . . ?
N1 C16 C15 120.5(6) . . ?
N1 C16 C17 121.4(6) . . ?
C15 C16 C17 118.0(6) . . ?
C16 C17 H17 119.6 . . ?
C18 C17 C16 120.7(6) . . ?
C18 C17 H17 119.6 . . ?
C13 C18 H18 119.7 . . ?
C17 C18 C13 120.6(5) . . ?
C17 C18 H18 119.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 N2 C12 S3 -154.5(3) 2_655 . . . ?
Ni1 N2 C12 N3 25.2(8) 2_655 . . . ?
Ni1 N3 C10 C11 170.4(4) . . . . ?
Ni1 N3 C12 S3 -171.2(3) . . . . ?
Ni1 N3 C12 N2 9.0(8) . . . . ?
Ni1 N4 C7 S1 -172.7(3) . . . . ?
Ni1 N4 C7 N6 10.0(8) . . . . ?
Ni1 N4 C9 C8 171.3(5) . . . . ?
S1 C8 C9 N4 2.1(8) . . . . ?
S2 N6 C7 S1 11.1(7) . . . . ?
S2 N6 C7 N4 -171.9(4) . . . . ?
S2 C4 C5 C6 -179.9(5) . . . . ?
S4 N2 C12 S3 6.2(7) . . . . ?
S4 N2 C12 N3 -174.1(4) . . . . ?
S4 C13 C14 C15 -178.8(5) . . . . ?
S4 C13 C18 C17 178.5(5) . . . . ?
O1 S4 N2 Ni1 -7.1(2) . . . 2_655 ?
O1 S4 N2 C12 -174.0(4) . . . . ?
O1 S4 C13 C14 -42.6(5) . . . . ?
O1 S4 C13 C18 139.9(5) . . . . ?
O2 S4 O1 Ni1 -117.0(2) . . . 2_655 ?
O2 S4 N2 Ni1 117.9(2) . . . 2_655 ?
O2 S4 N2 C12 -48.9(5) . . . . ?
O2 S4 C13 C14 -169.6(4) . . . . ?
O2 S4 C13 C18 12.8(5) . . . . ?
O3 S2 N6 C7 -47.0(6) . . . . ?
O3 S2 C4 C3 -1.0(6) . . . . ?
O3 S2 C4 C5 -180.0(5) . . . . ?
O4 S2 N6 C7 -174.5(5) . . . . ?
O4 S2 C4 C3 125.6(5) . . . . ?
O4 S2 C4 C5 -53.4(6) . . . . ?
N1 C16 C17 C18 177.0(7) . . . . ?
N2 S4 O1 Ni1 6.4(2) . . . 2_655 ?
N2 S4 C13 C14 66.2(5) . . . . ?
N2 S4 C13 C18 -111.4(5) . . . . ?
N3 C10 C11 S3 2.4(7) . . . . ?
N5 C1 C2 C3 177.6(6) . . . . ?
N5 C1 C6 C5 -175.9(6) . . . . ?
N6 S2 C4 C3 -122.5(5) . . . . ?
N6 S2 C4 C5 58.5(6) . . . . ?
C1 C2 C3 C4 -1.1(10) . . . . ?
C2 C1 C6 C5 1.8(9) . . . . ?
C2 C3 C4 S2 -178.3(5) . . . . ?
C2 C3 C4 C5 0.6(10) . . . . ?
C3 C4 C5 C6 1.2(10) . . . . ?
C4 S2 N6 C7 71.3(5) . . . . ?
C4 C5 C6 C1 -2.4(10) . . . . ?
C6 C1 C2 C3 -0.1(10) . . . . ?
C7 S1 C8 C9 -1.7(6) . . . . ?
C7 N4 C9 C8 -1.3(8) . . . . ?
C8 S1 C7 N4 1.0(5) . . . . ?
C8 S1 C7 N6 178.1(5) . . . . ?
C9 N4 C7 S1 -0.1(6) . . . . ?
C9 N4 C7 N6 -177.4(5) . . . . ?
C10 N3 C12 S3 0.3(6) . . . . ?
C10 N3 C12 N2 -179.5(5) . . . . ?
C11 S3 C12 N2 -179.4(5) . . . . ?
C11 S3 C12 N3 0.8(4) . . . . ?
C12 S3 C11 C10 -1.7(5) . . . . ?
C12 N3 C10 C11 -1.8(7) . . . . ?
C13 S4 O1 Ni1 121.3(2) . . . 2_655 ?
C13 S4 N2 Ni1 -121.9(2) . . . 2_655 ?
C13 S4 N2 C12 71.2(5) . . . . ?
C13 C14 C15 C16 -1.8(9) . . . . ?
C14 C13 C18 C17 0.9(9) . . . . ?
C14 C15 C16 N1 -177.2(6) . . . . ?
C14 C15 C16 C17 4.8(10) . . . . ?
C15 C16 C17 C18 -5.0(10) . . . . ?
C16 C17 C18 C13 2.2(10) . . . . ?
C18 C13 C14 C15 -1.2(8) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.314 0.000 0.814 490.1 51.6 ?

_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 3.770
_oxdiff_exptl_absorpt_empirical_full_min 0.352
####################################################################### 
# 
# 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_kj-15-2_twin1_hklf5_sq
_database_code_depnum_ccdc_archive 'CCDC 1912755'
loop_
_audit_author_name
_audit_author_address
'Juan Kang'
;Tianjin University
China
;
_audit_update_record             
;
2019-04-29 deposited with the CCDC.	2019-09-27 downloaded from the CCDC.
;
_audit_creation_date             2019-04-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C36 H48 Co N12 Na2 O16 S8, 2(H2 O)'
_chemical_formula_sum            'C36 H52 Co N12 Na2 O18 S8'
_chemical_formula_weight         1302.28
_chemical_melting_point          ?
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'
Co Co 0.3494 0.9721 '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'
Na Na 0.0362 0.0249 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.4803(5)
_cell_length_b                   7.7683(4)
_cell_length_c                   27.2802(15)
_cell_angle_alpha                90
_cell_angle_beta                 90.800(4)
_cell_angle_gamma                90
_cell_volume                     2644.6(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5179
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.6530
_cell_measurement_theta_min      1.8450
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.738
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90381
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.43d (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1346
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0674
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.805
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            9243
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.805
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.080
_diffrn_reflns_theta_min         2.726
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.805
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -97.00  32.00   0.50    2.00    --  -13.65 -25.00 -31.00  258
  2  ω    -89.00   6.00   0.50    2.00    --  -13.65 -57.00-120.00  190
  3  ω     39.00  67.00   0.50    2.00    --   12.17 178.00-120.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0237480000
_diffrn_orient_matrix_UB_12      -0.0184928000
_diffrn_orient_matrix_UB_13      0.0231059000
_diffrn_orient_matrix_UB_21      0.0482823000
_diffrn_orient_matrix_UB_22      -0.0231039000
_diffrn_orient_matrix_UB_23      -0.0116770000
_diffrn_orient_matrix_UB_31      0.0180229000
_diffrn_orient_matrix_UB_32      0.0862173000
_diffrn_orient_matrix_UB_33      0.0018311000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7191
_reflns_number_total             9243
_reflns_odcompleteness_completeness 98.48
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.43d (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43d (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43d (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.169
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.112
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         9243
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0535
_refine_ls_restrained_S_all      1.048
_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)+(0.0716P)²+1.6206P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1272
_refine_ls_wR_factor_ref         0.1464
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.6115
 0.3885
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 O4-H4A
 0.9 with sigma of 0.02
 O4-H4B
 0.9 with sigma of 0.02
 O4_$1-H4B_$1
 0.9 with sigma of 0.02
 O4_$1-H4A_$1
 0.9 with sigma of 0.02
 H6A-N6
 0.92 with sigma of 0.02
 H6B-N6
 0.92 with sigma of 0.02
 H2A-O2
 0.9 with sigma of 0.01
 H2B-O2
 0.9 with sigma of 0.01
 H4A-H4B
 1.6 with sigma of 0.04
 H2B-H2A
 1.5 with sigma of 0.01
 Na1-O3A \\sim Na1-O3
 with sigma of 0.01
4. Others
 Sof(O3)=Sof(H3A)=Sof(H3B)=1-FVAR(1)
 Sof(O3A)=Sof(H3AA)=Sof(H3AB)=FVAR(1)
5.a Free rotating group:
 O1(H1A,H1B), O3A(H3AA,H3AB), O3(H3A,H3B)
5.b Rotating group:
 N1(H1C,H1D)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C14(H14),
 C15(H15), C17(H17), C18(H18)
;
_atom_sites_solution_hydrogens   mixed
_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
Co1 Co 0.000000 0.500000 0.500000 0.01277(18) Uani 1 2 d S T P . .
S1 S 0.20744(8) 0.77466(13) 0.38045(4) 0.0195(2) Uani 1 1 d . . . . .
S2 S 0.28393(7) 0.27203(12) 0.61181(4) 0.0140(2) Uani 1 1 d . . . . .
S3 S 0.22615(8) 0.67296(13) 0.63071(4) 0.0209(2) Uani 1 1 d . . . . .
S4 S 0.26706(7) 0.37815(13) 0.36978(4) 0.0150(2) Uani 1 1 d . . . . .
Na1 Na 0.48836(12) 0.5236(2) 0.43298(7) 0.0257(4) Uani 1 1 d D . . . .
O1 O 0.4776(3) 0.8204(5) 0.4481(2) 0.0556(13) Uani 1 1 d . . . . .
H1A H 0.427366 0.878168 0.460878 0.083 Uiso 1 1 d G . . . .
H1B H 0.517394 0.895440 0.434858 0.083 Uiso 1 1 d G . . . .
O2 O 0.3727(2) 0.5389(5) 0.50479(14) 0.0307(8) Uani 1 1 d D . . . .
H2A H 0.350(4) 0.648(2) 0.508(3) 0.07(2) Uiso 1 1 d D . . . .
H2B H 0.321(3) 0.462(5) 0.512(3) 0.08(2) Uiso 1 1 d D . . . .
O4 O -0.1079(2) 0.7121(4) 0.50869(12) 0.0166(6) Uani 1 1 d D . . . .
H4A H -0.144(4) 0.702(7) 0.4800(10) 0.049(17) Uiso 1 1 d D . . . .
H4B H -0.143(3) 0.675(6) 0.5354(10) 0.025(13) Uiso 1 1 d D . . . .
O5 O 0.37673(19) 0.3731(4) 0.62838(12) 0.0177(6) Uani 1 1 d . . . . .
O6 O 0.31272(19) 0.1123(4) 0.58823(11) 0.0181(6) Uani 1 1 d . . . . .
O7 O 0.2898(2) 0.1979(4) 0.37943(11) 0.0188(6) Uani 1 1 d . . . . .
O8 O 0.36041(19) 0.4889(4) 0.36658(12) 0.0184(6) Uani 1 1 d . . . . .
N1 N 0.0415(3) 0.0979(6) 0.79024(16) 0.0300(10) Uani 1 1 d . . . . .
H1C H -0.027717 0.129879 0.787900 0.036 Uiso 1 1 d GR . . . .
H1D H 0.040305 -0.015713 0.796245 0.036 Uiso 1 1 d GR . . . .
N2 N 0.2098(2) 0.3737(4) 0.57499(13) 0.0149(7) Uani 1 1 d . . . . .
N3 N 0.0976(2) 0.6085(4) 0.55870(13) 0.0150(7) Uani 1 1 d . . . . .
N4 N 0.0831(2) 0.6532(4) 0.44660(13) 0.0152(7) Uani 1 1 d . . . . .
N5 N 0.1868(2) 0.4358(4) 0.41134(13) 0.0156(7) Uani 1 1 d . . . . .
N6 N 0.0431(3) 0.3942(6) 0.17694(16) 0.0261(9) Uani 1 1 d D . . . .
H6A H 0.076(4) 0.435(7) 0.1499(15) 0.048(17) Uiso 1 1 d D . . . .
H6B H 0.001(3) 0.301(4) 0.1692(19) 0.024(12) Uiso 1 1 d D . . . .
C1 C 0.0945(3) 0.3921(6) 0.22212(17) 0.0194(9) Uani 1 1 d . . . . .
C2 C 0.1896(3) 0.4843(5) 0.22981(18) 0.0204(9) Uani 1 1 d . . . . .
H2 H 0.218428 0.546941 0.204116 0.024 Uiso 1 1 calc R . . . .
C3 C 0.2409(3) 0.4839(5) 0.27453(17) 0.0176(9) Uani 1 1 d . . . . .
H3 H 0.304337 0.545171 0.278903 0.021 Uiso 1 1 calc R . . . .
C4 C 0.1986(3) 0.3928(5) 0.31300(16) 0.0147(8) Uani 1 1 d . . . . .
C5 C 0.1010(3) 0.3053(6) 0.30672(17) 0.0199(9) Uani 1 1 d . . . . .
H5 H 0.070654 0.247648 0.332982 0.024 Uiso 1 1 calc R . . . .
C6 C 0.0504(3) 0.3049(6) 0.26157(19) 0.0222(10) Uani 1 1 d . . . . .
H6 H -0.013928 0.245911 0.257395 0.027 Uiso 1 1 calc R . . . .
C7 C 0.0759(3) 0.7726(5) 0.57511(18) 0.0179(9) Uani 1 1 d . . . . .
H7 H 0.023798 0.841313 0.560246 0.021 Uiso 1 1 calc R . . . .
C8 C 0.1341(3) 0.8275(6) 0.61363(18) 0.0212(10) Uani 1 1 d . . . . .
H8 H 0.125960 0.933593 0.628926 0.025 Uiso 1 1 calc R . . . .
C9 C 0.1753(3) 0.5378(5) 0.58487(16) 0.0156(8) Uani 1 1 d . . . . .
C10 C 0.2092(3) 0.2226(5) 0.66398(16) 0.0144(8) Uani 1 1 d . . . . .
C11 C 0.1038(3) 0.2771(5) 0.66916(17) 0.0174(9) Uani 1 1 d . . . . .
H11 H 0.070835 0.340995 0.644391 0.021 Uiso 1 1 calc R . . . .
C12 C 0.0481(3) 0.2366(5) 0.71091(18) 0.0201(9) Uani 1 1 d . . . . .
H12 H -0.022075 0.274969 0.714139 0.024 Uiso 1 1 calc R . . . .
C13 C 0.0950(3) 0.1391(6) 0.74837(17) 0.0192(9) Uani 1 1 d . . . . .
C14 C 0.2009(3) 0.0773(5) 0.74173(17) 0.0193(9) Uani 1 1 d . . . . .
H14 H 0.232643 0.006645 0.765297 0.023 Uiso 1 1 calc R . . . .
C15 C 0.2564(3) 0.1219(5) 0.70047(17) 0.0172(9) Uani 1 1 d . . . . .
H15 H 0.326535 0.084123 0.696901 0.021 Uiso 1 1 calc R . . . .
C16 C 0.1567(3) 0.6043(5) 0.41479(16) 0.0158(8) Uani 1 1 d . . . . .
C17 C 0.1241(3) 0.9144(5) 0.41068(18) 0.0198(9) Uani 1 1 d . . . . .
H17 H 0.119807 1.032189 0.404957 0.024 Uiso 1 1 calc R . . . .
C18 C 0.0663(3) 0.8282(5) 0.44369(18) 0.0189(9) Uani 1 1 d . . . . .
H18 H 0.017281 0.883821 0.463614 0.023 Uiso 1 1 calc R . . . .
O3A O 0.4700(6) 0.2204(9) 0.4432(4) 0.033(2) Uani 0.524(13) 1 d D . . A 1
H3AA H 0.457703 0.248370 0.472746 0.050 Uiso 0.524(13) 1 d G . . A 1
H3AB H 0.411870 0.190381 0.429098 0.050 Uiso 0.524(13) 1 d G . . A 1
O3 O 0.5130(6) 0.2126(8) 0.4135(4) 0.034(3) Uani 0.476(13) 1 d D . . A 2
H3A H 0.451682 0.183611 0.402393 0.051 Uiso 0.476(13) 1 d G . . A 2
H3B H 0.560905 0.181438 0.393506 0.051 Uiso 0.476(13) 1 d G . . A 2
O9 O 0.2983(3) 0.8910(5) 0.50460(15) 0.0345(9) Uani 1 1 d . . . . .
H9A H 0.232(5) 0.916(9) 0.494(3) 0.08(2) Uiso 1 1 d . . . . .
H9B H 0.295(4) 0.964(7) 0.528(2) 0.037(16) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O4 2.143(3) 3_566 ?
Co1 O4 2.143(3) . ?
Co1 N3 2.169(3) 3_566 ?
Co1 N3 2.169(3) . ?
Co1 N4 2.158(3) 3_566 ?
Co1 N4 2.158(3) . ?
S1 C16 1.746(4) . ?
S1 C17 1.722(4) . ?
S2 O5 1.466(3) . ?
S2 O6 1.445(3) . ?
S2 N2 1.569(3) . ?
S2 C10 1.755(4) . ?
S3 C8 1.722(4) . ?
S3 C9 1.746(4) . ?
S4 O7 1.452(3) . ?
S4 O8 1.452(3) . ?
S4 N5 1.588(3) . ?
S4 C4 1.762(4) . ?
Na1 O1 2.346(4) . ?
Na1 O2 2.458(4) 3_666 ?
Na1 O2 2.453(4) . ?
Na1 O5 2.522(3) 3_666 ?
Na1 O8 2.413(3) . ?
Na1 O3A 2.383(7) . ?
Na1 H3AA 2.4303 . ?
Na1 O3 2.494(7) . ?
O1 H1A 0.8497 . ?
O1 H1B 0.8495 . ?
O2 H2A 0.899(12) . ?
O2 H2B 0.904(12) . ?
O4 H4A 0.901(17) . ?
O4 H4B 0.906(17) . ?
N1 H1C 0.8998 . ?
N1 H1D 0.8978 . ?
N1 C13 1.369(6) . ?
N2 C9 1.374(5) . ?
N3 C7 1.380(5) . ?
N3 C9 1.316(5) . ?
N4 C16 1.328(5) . ?
N4 C18 1.378(5) . ?
N5 C16 1.365(5) . ?
N6 H6A 0.91(2) . ?
N6 H6B 0.92(2) . ?
N6 C1 1.382(6) . ?
C1 C2 1.399(6) . ?
C1 C6 1.392(6) . ?
C2 H2 0.9300 . ?
C2 C3 1.370(6) . ?
C3 H3 0.9300 . ?
C3 C4 1.377(6) . ?
C4 C5 1.403(5) . ?
C5 H5 0.9300 . ?
C5 C6 1.376(6) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C7 C8 1.338(6) . ?
C8 H8 0.9300 . ?
C10 C11 1.390(5) . ?
C10 C15 1.391(6) . ?
C11 H11 0.9300 . ?
C11 C12 1.379(6) . ?
C12 H12 0.9300 . ?
C12 C13 1.395(6) . ?
C13 C14 1.419(6) . ?
C14 H14 0.9300 . ?
C14 C15 1.374(6) . ?
C15 H15 0.9300 . ?
C17 H17 0.9300 . ?
C17 C18 1.341(6) . ?
C18 H18 0.9300 . ?
O3A H3AA 0.8516 . ?
O3A H3AB 0.8492 . ?
O3 H3A 0.8490 . ?
O3 H3B 0.8501 . ?
O9 H9A 0.89(7) . ?
O9 H9B 0.86(6) . ?

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
O4 Co1 O4 180.00(17) 3_566 . ?
O4 Co1 N3 88.11(12) . . ?
O4 Co1 N3 91.89(12) . 3_566 ?
O4 Co1 N3 88.11(12) 3_566 3_566 ?
O4 Co1 N3 91.89(12) 3_566 . ?
O4 Co1 N4 87.65(12) 3_566 3_566 ?
O4 Co1 N4 92.35(12) 3_566 . ?
O4 Co1 N4 92.35(12) . 3_566 ?
O4 Co1 N4 87.65(12) . . ?
N3 Co1 N3 180.0 . 3_566 ?
N4 Co1 N3 90.80(13) . . ?
N4 Co1 N3 89.20(13) 3_566 . ?
N4 Co1 N3 90.80(13) 3_566 3_566 ?
N4 Co1 N3 89.20(13) . 3_566 ?
N4 Co1 N4 180.0 3_566 . ?
C17 S1 C16 89.7(2) . . ?
O5 S2 N2 112.57(18) . . ?
O5 S2 C10 107.09(19) . . ?
O6 S2 O5 113.39(16) . . ?
O6 S2 N2 107.18(18) . . ?
O6 S2 C10 108.14(18) . . ?
N2 S2 C10 108.30(18) . . ?
C8 S3 C9 89.5(2) . . ?
O7 S4 N5 105.44(18) . . ?
O7 S4 C4 108.22(18) . . ?
O8 S4 O7 115.31(16) . . ?
O8 S4 N5 112.98(18) . . ?
O8 S4 C4 106.78(19) . . ?
N5 S4 C4 107.84(18) . . ?
O1 Na1 O2 77.07(14) . . ?
O1 Na1 O2 96.57(17) . 3_666 ?
O1 Na1 O5 81.05(13) . 3_666 ?
O1 Na1 O8 101.70(16) . . ?
O1 Na1 O3A 160.9(3) . . ?
O1 Na1 H3AA 140.9 . . ?
O1 Na1 O3 175.6(3) . . ?
O2 Na1 O2 82.85(12) . 3_666 ?
O2 Na1 O5 157.03(13) . 3_666 ?
O2 Na1 O5 92.87(11) 3_666 3_666 ?
O2 Na1 H3AA 68.4 3_666 . ?
O2 Na1 H3AA 65.7 . . ?
O2 Na1 O3 107.0(3) . . ?
O2 Na1 O3 82.4(2) 3_666 . ?
O5 Na1 H3AA 133.4 3_666 . ?
O8 Na1 O2 102.37(12) . . ?
O8 Na1 O2 161.69(14) . 3_666 ?
O8 Na1 O5 88.76(11) . 3_666 ?
O8 Na1 H3AA 97.5 . . ?
O8 Na1 O3 79.3(2) . . ?
O3A Na1 O2 78.0(2) . 3_666 ?
O3A Na1 O2 84.0(3) . . ?
O3A Na1 O5 117.3(3) . 3_666 ?
O3A Na1 O8 85.0(2) . . ?
O3A Na1 H3AA 20.3 . . ?
Na1 O1 H1A 129.4 . . ?
Na1 O1 H1B 124.4 . . ?
H1A O1 H1B 104.6 . . ?
Na1 O2 Na1 97.15(12) . 3_666 ?
Na1 O2 H2A 108(4) . . ?
Na1 O2 H2A 110(5) 3_666 . ?
Na1 O2 H2B 124(4) . . ?
Na1 O2 H2B 103(4) 3_666 . ?
H2A O2 H2B 112(2) . . ?
Co1 O4 H4A 98(4) . . ?
Co1 O4 H4B 99(3) . . ?
H4A O4 H4B 115(4) . . ?
S2 O5 Na1 119.85(18) . 3_666 ?
S4 O8 Na1 122.98(18) . . ?
H1C N1 H1D 105.4 . . ?
C13 N1 H1C 110.8 . . ?
C13 N1 H1D 113.0 . . ?
C9 N2 S2 121.7(3) . . ?
C7 N3 Co1 119.2(3) . . ?
C9 N3 Co1 129.8(3) . . ?
C9 N3 C7 110.8(4) . . ?
C16 N4 Co1 128.8(3) . . ?
C16 N4 C18 110.5(3) . . ?
C18 N4 Co1 120.6(3) . . ?
C16 N5 S4 119.8(3) . . ?
H6A N6 H6B 111(5) . . ?
C1 N6 H6A 122(4) . . ?
C1 N6 H6B 117(3) . . ?
N6 C1 C2 120.7(4) . . ?
N6 C1 C6 120.8(4) . . ?
C6 C1 C2 118.5(4) . . ?
C1 C2 H2 119.4 . . ?
C3 C2 C1 121.2(4) . . ?
C3 C2 H2 119.4 . . ?
C2 C3 H3 120.0 . . ?
C2 C3 C4 120.0(4) . . ?
C4 C3 H3 120.0 . . ?
C3 C4 S4 121.1(3) . . ?
C3 C4 C5 119.8(4) . . ?
C5 C4 S4 119.0(3) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 C4 119.8(4) . . ?
C6 C5 H5 120.1 . . ?
C1 C6 H6 119.7 . . ?
C5 C6 C1 120.6(4) . . ?
C5 C6 H6 119.7 . . ?
N3 C7 H7 121.9 . . ?
C8 C7 N3 116.3(4) . . ?
C8 C7 H7 121.9 . . ?
S3 C8 H8 125.0 . . ?
C7 C8 S3 110.1(3) . . ?
C7 C8 H8 125.0 . . ?
N2 C9 S3 125.9(3) . . ?
N3 C9 S3 113.3(3) . . ?
N3 C9 N2 120.8(4) . . ?
C11 C10 S2 122.0(3) . . ?
C11 C10 C15 119.4(4) . . ?
C15 C10 S2 118.6(3) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 C10 120.2(4) . . ?
C12 C11 H11 119.9 . . ?
C11 C12 H12 119.4 . . ?
C11 C12 C13 121.1(4) . . ?
C13 C12 H12 119.4 . . ?
N1 C13 C12 122.2(4) . . ?
N1 C13 C14 119.6(4) . . ?
C12 C13 C14 118.2(4) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 C13 120.0(4) . . ?
C15 C14 H14 120.0 . . ?
C10 C15 H15 119.5 . . ?
C14 C15 C10 121.0(4) . . ?
C14 C15 H15 119.5 . . ?
N4 C16 S1 113.1(3) . . ?
N4 C16 N5 120.9(4) . . ?
N5 C16 S1 126.0(3) . . ?
S1 C17 H17 125.0 . . ?
C18 C17 S1 110.0(3) . . ?
C18 C17 H17 125.0 . . ?
N4 C18 H18 121.7 . . ?
C17 C18 N4 116.6(4) . . ?
C17 C18 H18 121.7 . . ?
Na1 O3A H3AA 82.9 . . ?
Na1 O3A H3AB 107.5 . . ?
H3AA O3A H3AB 109.5 . . ?
Na1 O3 H3A 102.7 . . ?
Na1 O3 H3B 120.2 . . ?
H3A O3 H3B 109.5 . . ?
H9A O9 H9B 92(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Co1 N3 C7 C8 175.5(3) . . . . ?
Co1 N3 C9 S3 -176.72(19) . . . . ?
Co1 N3 C9 N2 3.7(6) . . . . ?
Co1 N4 C16 S1 -176.94(19) . . . . ?
Co1 N4 C16 N5 2.6(6) . . . . ?
Co1 N4 C18 C17 177.6(3) . . . . ?
S1 C17 C18 N4 -0.6(5) . . . . ?
S2 N2 C9 S3 13.8(5) . . . . ?
S2 N2 C9 N3 -166.8(3) . . . . ?
S2 C10 C11 C12 -179.5(3) . . . . ?
S2 C10 C15 C14 -179.0(3) . . . . ?
S4 N5 C16 S1 -6.1(5) . . . . ?
S4 N5 C16 N4 174.5(3) . . . . ?
S4 C4 C5 C6 -175.3(3) . . . . ?
O5 S2 N2 C9 -49.5(4) . . . . ?
O5 S2 C10 C11 119.1(3) . . . . ?
O5 S2 C10 C15 -62.7(4) . . . . ?
O6 S2 O5 Na1 60.5(2) . . . 3_666 ?
O6 S2 N2 C9 -174.8(3) . . . . ?
O6 S2 C10 C11 -118.4(3) . . . . ?
O6 S2 C10 C15 59.8(4) . . . . ?
O7 S4 O8 Na1 -59.4(2) . . . . ?
O7 S4 N5 C16 174.7(3) . . . . ?
O7 S4 C4 C3 -119.2(3) . . . . ?
O7 S4 C4 C5 58.8(4) . . . . ?
O8 S4 N5 C16 47.9(4) . . . . ?
O8 S4 C4 C3 5.5(4) . . . . ?
O8 S4 C4 C5 -176.5(3) . . . . ?
N1 C13 C14 C15 -178.2(4) . . . . ?
N2 S2 O5 Na1 -61.4(2) . . . 3_666 ?
N2 S2 C10 C11 -2.5(4) . . . . ?
N2 S2 C10 C15 175.7(3) . . . . ?
N3 C7 C8 S3 2.2(5) . . . . ?
N5 S4 O8 Na1 62.0(2) . . . . ?
N5 S4 C4 C3 127.2(3) . . . . ?
N5 S4 C4 C5 -54.8(4) . . . . ?
N6 C1 C2 C3 179.6(4) . . . . ?
N6 C1 C6 C5 -179.0(4) . . . . ?
C1 C2 C3 C4 -0.5(6) . . . . ?
C2 C1 C6 C5 -2.0(6) . . . . ?
C2 C3 C4 S4 175.8(3) . . . . ?
C2 C3 C4 C5 -2.1(6) . . . . ?
C3 C4 C5 C6 2.7(6) . . . . ?
C4 S4 O8 Na1 -179.62(18) . . . . ?
C4 S4 N5 C16 -69.9(3) . . . . ?
C4 C5 C6 C1 -0.6(6) . . . . ?
C6 C1 C2 C3 2.6(6) . . . . ?
C7 N3 C9 S3 -0.7(4) . . . . ?
C7 N3 C9 N2 179.8(3) . . . . ?
C8 S3 C9 N2 -178.9(4) . . . . ?
C8 S3 C9 N3 1.6(3) . . . . ?
C9 S3 C8 C7 -2.1(3) . . . . ?
C9 N3 C7 C8 -1.0(5) . . . . ?
C10 S2 O5 Na1 179.67(17) . . . 3_666 ?
C10 S2 N2 C9 68.7(3) . . . . ?
C10 C11 C12 C13 -0.8(7) . . . . ?
C11 C10 C15 C14 -0.8(6) . . . . ?
C11 C12 C13 N1 179.7(4) . . . . ?
C11 C12 C13 C14 -2.1(7) . . . . ?
C12 C13 C14 C15 3.6(6) . . . . ?
C13 C14 C15 C10 -2.2(6) . . . . ?
C15 C10 C11 C12 2.3(6) . . . . ?
C16 S1 C17 C18 0.5(4) . . . . ?
C16 N4 C18 C17 0.3(5) . . . . ?
C17 S1 C16 N4 -0.4(3) . . . . ?
C17 S1 C16 N5 -179.9(4) . . . . ?
C18 N4 C16 S1 0.2(4) . . . . ?
C18 N4 C16 N5 179.7(4) . . . . ?

_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.143
_oxdiff_exptl_absorpt_empirical_full_min 0.919
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.6115
2 0.3885

