# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_C20
_database_code_depnum_ccdc_archive 'CCDC 1589052'
_audit_update_record             
;
2018-08-24 deposited with the CCDC.
2018-10-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C48 H48 Co20 N72 O24 S24, O8 S2, C H4 O, 6(C3 H7 N O), 3(H2 O)'
_chemical_formula_sum            'C67 H100 Co20 N78 O42 S26'
_chemical_formula_weight         4682.40

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_H-M_alt        'P a -3'
_space_group_name_Hall           '-P 2ac 2ab 3'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'z, x, y'
'y, z, x'
'-y+1/2, -z, x+1/2'
'z+1/2, -x+1/2, -y'
'-y, z+1/2, -x+1/2'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'-z, -x, -y'
'-y, -z, -x'
'y-1/2, z, -x-1/2'
'-z-1/2, x-1/2, y'
'y, -z-1/2, x-1/2'
'z-1/2, x, -y-1/2'
'z, -x-1/2, y-1/2'
'-y-1/2, z-1/2, x'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   26.34708(15)
_cell_length_b                   26.34708(15)
_cell_length_c                   26.34708(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     18289.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    25985
_cell_measurement_theta_min      3.5340
_cell_measurement_theta_max      24.0570

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_F_000             9360
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    2.138
_shelx_estimated_absorpt_T_min   0.557
_shelx_estimated_absorpt_T_max   0.783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.560
_exptl_absorpt_correction_T_max  0.774
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            194272
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_av_R_equivalents  0.0851
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         3.370
_diffrn_reflns_theta_max         25.003
_diffrn_reflns_theta_full        25.003
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             5325
_reflns_number_gt                3979
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  'SHELXTL (Bruker, 1998)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0997P)²+107.3862P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5325
_refine_ls_number_parameters     405
_refine_ls_number_restraints     104
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0607
_refine_ls_wR_factor_ref         0.2070
_refine_ls_wR_factor_gt          0.1563
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.61361(4) 0.71762(4) -0.17274(4) 0.0425(3) Uani 1 1 d . . . . .
Co2 Co 0.44858(3) 0.69052(4) -0.11096(4) 0.0403(3) Uani 1 1 d . . . . .
Co3 Co 0.40095(4) 0.77836(4) 0.03705(4) 0.0478(3) Uani 1 1 d . . . . .
Co4 Co 0.37078(4) 0.62922(4) 0.12922(4) 0.0457(4) Uani 1 3 d S T P . .
S1 S 0.69109(7) 0.71337(8) -0.20130(7) 0.0492(5) Uani 1 1 d . . . . .
S2 S 0.56823(8) 0.75712(9) -0.23022(8) 0.0586(6) Uani 1 1 d . . . . .
S3 S 0.43363(8) 0.83962(7) -0.00818(9) 0.0565(5) Uani 1 1 d . U . . .
S4 S 0.39019(9) 0.80785(8) 0.11377(9) 0.0615(6) Uani 1 1 d . . . . .
O1 O 0.61630(18) 0.64147(18) -0.04328(17) 0.0414(11) Uani 1 1 d . . . . .
O2 O 0.51463(17) 0.67556(19) -0.06800(17) 0.0432(11) Uani 1 1 d . . . . .
O3 O 0.40689(19) 0.65771(19) -0.05153(18) 0.0457(11) Uani 1 1 d . . . . .
O4 O 0.3757(2) 0.63118(18) 0.04909(19) 0.0467(12) Uani 1 1 d . . . . .
N1 N 0.7654(2) 0.6654(3) -0.1510(3) 0.0557(17) Uani 1 1 d . . . . .
H1A H 0.7686 0.6332 -0.1470 0.067 Uiso 1 1 d R U . . .
H1B H 0.7784 0.6740 -0.1795 0.067 Uiso 1 1 d R U . . .
N2 N 0.6879(2) 0.6635(2) -0.1123(2) 0.0432(13) Uani 1 1 d . . . . .
N3 N 0.6380(2) 0.6808(2) -0.1179(2) 0.0425(13) Uani 1 1 d . . . . .
N4 N 0.5527(2) 0.7086(2) -0.1392(2) 0.0426(13) Uani 1 1 d . . . . .
N5 N 0.5052(2) 0.7243(2) -0.1574(2) 0.0441(14) Uani 1 1 d . . . . .
N6 N 0.4673(3) 0.7655(3) -0.2235(3) 0.0640(19) Uani 1 1 d . . . . .
H6A H 0.4683 0.7577 -0.2556 0.077 Uiso 1 1 d R U . . .
H6B H 0.4398 0.7520 -0.2109 0.077 Uiso 1 1 d R U . . .
N7 N 0.4631(3) 0.8263(3) -0.1033(3) 0.078(2) Uani 1 1 d . . . . .
H7A H 0.4679 0.8086 -0.1312 0.094 Uiso 1 1 d R U . . .
H7B H 0.4722 0.8584 -0.1020 0.094 Uiso 1 1 d R U . . .
N8 N 0.4289(2) 0.7562(2) -0.0672(2) 0.0475(14) Uani 1 1 d . . . . .
N9 N 0.4083(2) 0.7394(2) -0.0209(2) 0.0452(14) Uani 1 1 d . . . . .
N10 N 0.3805(2) 0.7173(2) 0.0644(2) 0.0479(14) Uani 1 1 d . . . . .
N11 N 0.3701(2) 0.7087(2) 0.1162(2) 0.0482(14) Uani 1 1 d . . . . .
N12 N 0.3650(3) 0.7481(3) 0.1926(3) 0.073(2) Uani 1 1 d . . . . .
H12A H 0.3820 0.7237 0.2065 0.087 Uiso 1 1 d R U . . .
H12B H 0.3742 0.7763 0.2066 0.087 Uiso 1 1 d R U . . .
C1 C 0.7155(3) 0.6775(3) -0.1507(3) 0.0425(16) Uani 1 1 d . . . . .
C2 C 0.6059(3) 0.6673(3) -0.0819(3) 0.0386(15) Uani 1 1 d . . . . .
C3 C 0.5529(3) 0.6847(3) -0.0953(2) 0.0395(15) Uani 1 1 d . . . . .
C4 C 0.5094(3) 0.7477(3) -0.2003(3) 0.0493(18) Uani 1 1 d . . . . .
C5 C 0.4419(3) 0.8044(3) -0.0631(3) 0.0529(19) Uani 1 1 d . U . . .
C6 C 0.4000(2) 0.6902(3) -0.0177(3) 0.0390(15) Uani 1 1 d . . . . .
C7 C 0.3834(3) 0.6761(3) 0.0356(3) 0.0428(16) Uani 1 1 d . . . . .
C8 C 0.3746(3) 0.7505(3) 0.1418(3) 0.0509(18) Uani 1 1 d . . . . .
S51 S 0.4247(5) 0.4418(6) 0.2108(6) 0.070(10) Uani 0.1667 1 d D . P A 1
O51 O 0.4397(8) 0.4424(8) 0.1568(6) 0.029(3) Uani 0.1667 1 d D . P A 1
O61 O 0.3698(5) 0.4334(8) 0.2155(8) 0.029(3) Uani 0.1667 1 d D U P A 1
O71 O 0.4388(8) 0.4909(6) 0.2339(7) 0.029(3) Uani 0.1667 1 d D U P A 1
O81 O 0.4520(7) 0.4006(6) 0.2368(7) 0.029(3) Uani 0.1667 1 d D U P A 1
S52 S 0.4238(6) 0.4496(7) 0.2136(6) 0.074(10) Uani 0.1667 1 d D . P B 2
O52 O 0.4449(10) 0.4702(11) 0.1659(8) 0.054(4) Uani 0.1667 1 d D . P B 2
O62 O 0.4143(10) 0.3953(7) 0.2054(10) 0.054(4) Uani 0.1667 1 d D U P B 2
O72 O 0.3758(8) 0.4749(10) 0.2261(10) 0.054(4) Uani 0.1667 1 d D U P B 2
O82 O 0.4606(9) 0.4564(10) 0.2549(8) 0.054(4) Uani 0.1667 1 d D U P B 2
C12 C 0.5000 0.5000 0.0000 0.078(7) Uani 1 6 d DS T P . .
O91 O 0.4654(2) 0.5346(2) 0.0346(2) 0.07(3) Uani 0.12(3) 3 d DS T P C 1
H91 H 0.4401 0.5384 0.0581 0.110 Uiso 0.041(11) 1 d R U P C 1
O92 O 0.5477(8) 0.5255(15) -0.0114(17) 0.055(13) Uani 0.125(11) 1 d D . P C 2
H92 H 0.5415 0.5543 -0.0277 0.083 Uiso 0.125(11) 1 d R U P C 2
O10 O 0.3355(5) 0.3355(5) 0.3355(5) 0.190(10) Uani 1 3 d S T P . .
H101 H 0.3296 0.3241 0.3048 0.285 Uiso 0.3333 1 d R U P . .
H102 H 0.3693 0.3395 0.3458 0.285 Uiso 0.3333 1 d R U P . .
O11 O 0.5000 0.5000 0.5000 0.50(7) Uani 1 6 d S T P . .
H11 H 0.5015 0.5124 0.4699 0.756 Uiso 0.3333 1 d R U P . .
O12 O 0.4628(8) 0.3504(10) 0.3742(9) 0.299(11) Uani 1 1 d D U . . .
C9 C 0.4949(10) 0.3885(10) 0.3728(9) 0.39(3) Uani 1 1 d D U . . .
H9 H 0.4950 0.4159 0.3962 0.463 Uiso 1 1 calc R U . . .
N13 N 0.5290(6) 0.3833(7) 0.3325(7) 0.179(7) Uani 1 1 d D U . . .
C10 C 0.5725(9) 0.4153(9) 0.3210(9) 0.227(13) Uani 1 1 d D . . . .
H10A H 0.5638 0.4384 0.2932 0.340 Uiso 1 1 calc R U . . .
H10B H 0.6012 0.3939 0.3109 0.340 Uiso 1 1 calc R U . . .
H10C H 0.5817 0.4350 0.3511 0.340 Uiso 1 1 calc R U . . .
C11 C 0.5271(13) 0.3403(11) 0.2958(12) 0.33(2) Uani 1 1 d D U . . .
H11A H 0.5558 0.3175 0.3019 0.495 Uiso 1 1 calc R U . . .
H11B H 0.5290 0.3536 0.2611 0.495 Uiso 1 1 calc R U . . .
H11C H 0.4952 0.3217 0.3002 0.495 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 N4 1.847(6) . ?
Co1 N3 1.856(6) . ?
Co1 S1 2.179(2) . ?
Co1 S2 2.192(2) . ?
Co2 O3 2.099(5) . ?
Co2 O2 2.113(5) . ?
Co2 N2 2.119(6) 19_656 ?
Co2 N5 2.125(6) . ?
Co2 O1 2.125(5) 19_656 ?
Co2 N8 2.142(7) . ?
Co3 N10 1.844(6) . ?
Co3 N9 1.850(6) . ?
Co3 S3 2.183(2) . ?
Co3 S4 2.184(2) . ?
Co4 O4 2.116(5) 7_564 ?
Co4 O4 2.116(5) 6_655 ?
Co4 O4 2.116(5) . ?
Co4 N11 2.122(6) 7_564 ?
Co4 N11 2.122(6) . ?
Co4 N11 2.122(6) 6_655 ?
S1 C1 1.756(7) . ?
S2 C4 1.756(8) . ?
S3 C5 1.733(9) . ?
S4 C8 1.731(8) . ?
O1 C2 1.255(8) . ?
O1 Co2 2.125(5) 18_565 ?
O2 C3 1.261(8) . ?
O3 C6 1.250(8) . ?
O4 C7 1.252(9) . ?
N1 C1 1.355(9) . ?
N1 H1A 0.8580 . ?
N1 H1B 0.8577 . ?
N2 C1 1.300(9) . ?
N2 N3 1.399(8) . ?
N2 Co2 2.119(6) 18_565 ?
N3 C2 1.320(9) . ?
N4 C3 1.319(9) . ?
N4 N5 1.402(8) . ?
N5 C4 1.292(9) . ?
N6 C4 1.350(10) . ?
N6 H6A 0.8697 . ?
N6 H6B 0.8722 . ?
N7 C5 1.328(11) . ?
N7 H7A 0.8800 . ?
N7 H7B 0.8801 . ?
N8 C5 1.320(10) . ?
N8 N9 1.407(8) . ?
N9 C6 1.317(9) . ?
N10 C7 1.326(9) . ?
N10 N11 1.411(9) . ?
N11 C8 1.297(10) . ?
N12 C8 1.364(11) . ?
N12 H12A 0.8654 . ?
N12 H12B 0.8645 . ?
C2 C3 1.511(9) . ?
C6 C7 1.517(10) . ?
S51 O61 1.468(9) . ?
S51 O81 1.471(9) . ?
S51 O71 1.475(9) . ?
S51 O51 1.478(9) . ?
S52 O72 1.468(9) . ?
S52 O62 1.468(10) . ?
S52 O82 1.469(9) . ?
S52 O52 1.476(9) . ?
C12 O92 1.456(10) . ?
C12 O92 1.456(10) 18_565 ?
C12 O92 1.456(10) 6_655 ?
C12 O92 1.456(10) 13_665 ?
C12 O92 1.456(10) 19_656 ?
C12 O92 1.456(10) 7_564 ?
C12 O91 1.578(10) 13_665 ?
C12 O91 1.578(10) . ?
O91 H91 0.9152 . ?
O92 O92 1.70(4) 19_656 ?
O92 O92 1.70(4) 18_565 ?
O92 H92 0.8883 . ?
O10 H101 0.8776 . ?
O10 H102 0.9373 . ?
O11 H11 0.8584 . ?
O12 C9 1.313(10) . ?
C9 N13 1.398(9) . ?
C9 H9 0.9500 . ?
N13 C10 1.454(9) . ?
N13 C11 1.490(9) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 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
N4 Co1 N3 82.0(2) . . ?
N4 Co1 S1 166.58(19) . . ?
N3 Co1 S1 85.28(19) . . ?
N4 Co1 S2 85.26(18) . . ?
N3 Co1 S2 167.18(19) . . ?
S1 Co1 S2 107.27(8) . . ?
O3 Co2 O2 87.40(19) . . ?
O3 Co2 N2 94.5(2) . 19_656 ?
O2 Co2 N2 165.2(2) . 19_656 ?
O3 Co2 N5 165.8(2) . . ?
O2 Co2 N5 78.9(2) . . ?
N2 Co2 N5 99.7(2) 19_656 . ?
O3 Co2 O1 87.49(19) . 19_656 ?
O2 Co2 O1 87.02(19) . 19_656 ?
N2 Co2 O1 78.41(19) 19_656 19_656 ?
N5 Co2 O1 95.6(2) . 19_656 ?
O3 Co2 N8 78.7(2) . . ?
O2 Co2 N8 93.5(2) . . ?
N2 Co2 N8 101.2(2) 19_656 . ?
N5 Co2 N8 98.1(2) . . ?
O1 Co2 N8 166.2(2) 19_656 . ?
N10 Co3 N9 82.5(3) . . ?
N10 Co3 S3 166.9(2) . . ?
N9 Co3 S3 85.31(19) . . ?
N10 Co3 S4 84.9(2) . . ?
N9 Co3 S4 167.1(2) . . ?
S3 Co3 S4 107.05(9) . . ?
O4 Co4 O4 88.0(2) 7_564 6_655 ?
O4 Co4 O4 88.0(2) 7_564 . ?
O4 Co4 O4 88.0(2) 6_655 . ?
O4 Co4 N11 79.4(2) 7_564 7_564 ?
O4 Co4 N11 94.2(2) 6_655 7_564 ?
O4 Co4 N11 167.1(2) . 7_564 ?
O4 Co4 N11 94.2(2) 7_564 . ?
O4 Co4 N11 167.1(2) 6_655 . ?
O4 Co4 N11 79.4(2) . . ?
N11 Co4 N11 98.8(2) 7_564 . ?
O4 Co4 N11 167.1(2) 7_564 6_655 ?
O4 Co4 N11 79.4(2) 6_655 6_655 ?
O4 Co4 N11 94.2(2) . 6_655 ?
N11 Co4 N11 98.8(2) 7_564 6_655 ?
N11 Co4 N11 98.8(2) . 6_655 ?
C1 S1 Co1 96.2(2) . . ?
C4 S2 Co1 96.0(2) . . ?
C5 S3 Co3 96.3(3) . . ?
C8 S4 Co3 96.6(3) . . ?
C2 O1 Co2 109.0(4) . 18_565 ?
C3 O2 Co2 108.5(4) . . ?
C6 O3 Co2 109.1(4) . . ?
C7 O4 Co4 108.4(4) . . ?
C1 N1 H1A 109.0 . . ?
C1 N1 H1B 109.2 . . ?
H1A N1 H1B 109.3 . . ?
C1 N2 N3 110.5(6) . . ?
C1 N2 Co2 139.1(5) . 18_565 ?
N3 N2 Co2 108.9(4) . 18_565 ?
C2 N3 N2 116.0(6) . . ?
C2 N3 Co1 118.6(5) . . ?
N2 N3 Co1 125.3(4) . . ?
C3 N4 N5 116.3(6) . . ?
C3 N4 Co1 118.6(5) . . ?
N5 N4 Co1 125.1(4) . . ?
C4 N5 N4 111.3(6) . . ?
C4 N5 Co2 139.8(5) . . ?
N4 N5 Co2 107.9(4) . . ?
C4 N6 H6A 109.5 . . ?
C4 N6 H6B 111.6 . . ?
H6A N6 H6B 107.4 . . ?
C5 N7 H7A 119.8 . . ?
C5 N7 H7B 120.2 . . ?
H7A N7 H7B 120.0 . . ?
C5 N8 N9 109.3(6) . . ?
C5 N8 Co2 139.3(5) . . ?
N9 N8 Co2 107.9(4) . . ?
C6 N9 N8 115.4(6) . . ?
C6 N9 Co3 118.4(5) . . ?
N8 N9 Co3 125.6(5) . . ?
C7 N10 N11 115.7(6) . . ?
C7 N10 Co3 118.3(5) . . ?
N11 N10 Co3 125.1(5) . . ?
C8 N11 N10 110.5(6) . . ?
C8 N11 Co4 138.9(5) . . ?
N10 N11 Co4 108.2(4) . . ?
C8 N12 H12A 110.7 . . ?
C8 N12 H12B 109.1 . . ?
H12A N12 H12B 108.2 . . ?
N2 C1 N1 118.7(7) . . ?
N2 C1 S1 122.7(5) . . ?
N1 C1 S1 118.6(5) . . ?
O1 C2 N3 126.0(6) . . ?
O1 C2 C3 123.8(6) . . ?
N3 C2 C3 110.1(6) . . ?
O2 C3 N4 126.1(6) . . ?
O2 C3 C2 123.2(6) . . ?
N4 C3 C2 110.7(6) . . ?
N5 C4 N6 119.5(7) . . ?
N5 C4 S2 122.4(6) . . ?
N6 C4 S2 118.2(5) . . ?
N8 C5 N7 117.5(8) . . ?
N8 C5 S3 123.5(6) . . ?
N7 C5 S3 119.0(6) . . ?
O3 C6 N9 127.1(6) . . ?
O3 C6 C7 122.3(6) . . ?
N9 C6 C7 110.4(6) . . ?
O4 C7 N10 127.0(7) . . ?
O4 C7 C6 122.7(6) . . ?
N10 C7 C6 110.2(6) . . ?
N11 C8 N12 117.0(7) . . ?
N11 C8 S4 122.8(6) . . ?
N12 C8 S4 120.2(6) . . ?
O61 S51 O81 109.4(11) . . ?
O61 S51 O71 110.2(11) . . ?
O81 S51 O71 109.4(11) . . ?
O61 S51 O51 110.2(11) . . ?
O81 S51 O51 109.0(12) . . ?
O71 S51 O51 108.6(11) . . ?
O72 S52 O62 109.3(12) . . ?
O72 S52 O82 110.3(12) . . ?
O62 S52 O82 109.8(12) . . ?
O72 S52 O52 110.4(12) . . ?
O62 S52 O52 107.4(12) . . ?
O82 S52 O52 109.6(12) . . ?
O92 C12 O92 71.7(19) . 18_565 ?
O92 C12 O92 108.3(19) . 6_655 ?
O92 C12 O92 180(4) 18_565 6_655 ?
O92 C12 O92 180.0 . 13_665 ?
O92 C12 O92 108.3(19) 18_565 13_665 ?
O92 C12 O92 71.7(19) 6_655 13_665 ?
O92 C12 O92 71.7(19) . 19_656 ?
O92 C12 O92 108.3(19) 18_565 19_656 ?
O92 C12 O92 71.7(19) 6_655 19_656 ?
O92 C12 O92 108.3(19) 13_665 19_656 ?
O92 C12 O92 108.3(19) . 7_564 ?
O92 C12 O92 71.7(19) 18_565 7_564 ?
O92 C12 O92 108.3(19) 6_655 7_564 ?
O92 C12 O92 71.7(19) 13_665 7_564 ?
O92 C12 O92 180(2) 19_656 7_564 ?
O91 C12 O91 180.0(11) 13_665 . ?
C12 O91 H91 150.9 . . ?
C12 O92 O92 54.2(10) . 19_656 ?
C12 O92 O92 54.2(9) . 18_565 ?
O92 O92 O92 88(4) 19_656 18_565 ?
C12 O92 H92 109.6 . . ?
O92 O92 H92 55.4 19_656 . ?
O92 O92 H92 124.3 18_565 . ?
H101 O10 H102 118.3 . . ?
O12 C9 N13 111.2(15) . . ?
O12 C9 H9 124.4 . . ?
N13 C9 H9 124.4 . . ?
C9 N13 C10 127.4(13) . . ?
C9 N13 C11 123.1(13) . . ?
C10 N13 C11 109.4(12) . . ?
N13 C10 H10A 109.5 . . ?
N13 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N13 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N13 C11 H11A 109.5 . . ?
N13 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N13 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N2 N3 C2 177.7(6) . . . . ?
Co2 N2 N3 C2 8.9(7) 18_565 . . . ?
C1 N2 N3 Co1 0.9(8) . . . . ?
Co2 N2 N3 Co1 -168.0(3) 18_565 . . . ?
N4 Co1 N3 C2 -2.4(5) . . . . ?
S1 Co1 N3 C2 -178.1(5) . . . . ?
S2 Co1 N3 C2 -9.5(14) . . . . ?
N4 Co1 N3 N2 174.3(6) . . . . ?
S1 Co1 N3 N2 -1.3(5) . . . . ?
S2 Co1 N3 N2 167.3(6) . . . . ?
N3 Co1 N4 C3 2.4(5) . . . . ?
S1 Co1 N4 C3 21.4(13) . . . . ?
S2 Co1 N4 C3 -179.2(5) . . . . ?
N3 Co1 N4 N5 -176.0(6) . . . . ?
S1 Co1 N4 N5 -157.0(6) . . . . ?
S2 Co1 N4 N5 2.4(5) . . . . ?
C3 N4 N5 C4 179.4(7) . . . . ?
Co1 N4 N5 C4 -2.2(9) . . . . ?
C3 N4 N5 Co2 -10.1(7) . . . . ?
Co1 N4 N5 Co2 168.3(3) . . . . ?
C5 N8 N9 C6 -171.3(6) . . . . ?
Co2 N8 N9 C6 -8.1(7) . . . . ?
C5 N8 N9 Co3 -0.5(8) . . . . ?
Co2 N8 N9 Co3 162.7(3) . . . . ?
N10 Co3 N9 C6 -3.8(5) . . . . ?
S3 Co3 N9 C6 171.4(5) . . . . ?
S4 Co3 N9 C6 7.1(13) . . . . ?
N10 Co3 N9 N8 -174.4(6) . . . . ?
S3 Co3 N9 N8 0.8(5) . . . . ?
S4 Co3 N9 N8 -163.5(6) . . . . ?
N9 Co3 N10 C7 4.7(6) . . . . ?
S3 Co3 N10 C7 -17.1(14) . . . . ?
S4 Co3 N10 C7 -172.9(6) . . . . ?
N9 Co3 N10 N11 173.3(6) . . . . ?
S3 Co3 N10 N11 151.5(7) . . . . ?
S4 Co3 N10 N11 -4.3(5) . . . . ?
C7 N10 N11 C8 171.8(7) . . . . ?
Co3 N10 N11 C8 3.0(9) . . . . ?
C7 N10 N11 Co4 6.0(7) . . . . ?
Co3 N10 N11 Co4 -162.8(4) . . . . ?
N3 N2 C1 N1 178.0(6) . . . . ?
Co2 N2 C1 N1 -18.2(12) 18_565 . . . ?
N3 N2 C1 S1 0.4(9) . . . . ?
Co2 N2 C1 S1 164.2(4) 18_565 . . . ?
Co1 S1 C1 N2 -1.1(6) . . . . ?
Co1 S1 C1 N1 -178.7(6) . . . . ?
Co2 O1 C2 N3 -10.4(8) 18_565 . . . ?
Co2 O1 C2 C3 165.3(5) 18_565 . . . ?
N2 N3 C2 O1 1.1(10) . . . . ?
Co1 N3 C2 O1 178.2(5) . . . . ?
N2 N3 C2 C3 -175.0(6) . . . . ?
Co1 N3 C2 C3 2.0(8) . . . . ?
Co2 O2 C3 N4 12.1(9) . . . . ?
Co2 O2 C3 C2 -165.7(5) . . . . ?
N5 N4 C3 O2 -1.4(11) . . . . ?
Co1 N4 C3 O2 -179.9(5) . . . . ?
N5 N4 C3 C2 176.7(6) . . . . ?
Co1 N4 C3 C2 -1.8(8) . . . . ?
O1 C2 C3 O2 1.8(11) . . . . ?
N3 C2 C3 O2 178.0(6) . . . . ?
O1 C2 C3 N4 -176.4(6) . . . . ?
N3 C2 C3 N4 -0.1(8) . . . . ?
N4 N5 C4 N6 179.9(7) . . . . ?
Co2 N5 C4 N6 14.0(14) . . . . ?
N4 N5 C4 S2 0.3(9) . . . . ?
Co2 N5 C4 S2 -165.6(5) . . . . ?
Co1 S2 C4 N5 1.1(7) . . . . ?
Co1 S2 C4 N6 -178.5(7) . . . . ?
N9 N8 C5 N7 178.7(7) . . . . ?
Co2 N8 C5 N7 23.7(13) . . . . ?
N9 N8 C5 S3 -0.3(9) . . . . ?
Co2 N8 C5 S3 -155.3(5) . . . . ?
Co3 S3 C5 N8 0.7(7) . . . . ?
Co3 S3 C5 N7 -178.3(7) . . . . ?
Co2 O3 C6 N9 11.8(9) . . . . ?
Co2 O3 C6 C7 -164.0(5) . . . . ?
N8 N9 C6 O3 -2.5(10) . . . . ?
Co3 N9 C6 O3 -174.0(6) . . . . ?
N8 N9 C6 C7 173.8(5) . . . . ?
Co3 N9 C6 C7 2.2(7) . . . . ?
Co4 O4 C7 N10 -10.6(9) . . . . ?
Co4 O4 C7 C6 166.6(5) . . . . ?
N11 N10 C7 O4 3.3(11) . . . . ?
Co3 N10 C7 O4 172.9(6) . . . . ?
N11 N10 C7 C6 -174.2(6) . . . . ?
Co3 N10 C7 C6 -4.6(8) . . . . ?
O3 C6 C7 O4 0.3(11) . . . . ?
N9 C6 C7 O4 -176.2(6) . . . . ?
O3 C6 C7 N10 177.9(6) . . . . ?
N9 C6 C7 N10 1.4(8) . . . . ?
N10 N11 C8 N12 179.2(7) . . . . ?
Co4 N11 C8 N12 -21.6(13) . . . . ?
N10 N11 C8 S4 1.1(9) . . . . ?
Co4 N11 C8 S4 160.3(5) . . . . ?
Co3 S4 C8 N11 -3.5(7) . . . . ?
Co3 S4 C8 N12 178.5(7) . . . . ?
O92 C12 O92 O92 -117(4) 18_565 . . 19_656 ?
O92 C12 O92 O92 63(4) 6_655 . . 19_656 ?
O92 C12 O92 O92 180.000(0) 7_564 . . 19_656 ?
O92 C12 O92 O92 180.000(3) 6_655 . . 18_565 ?
O92 C12 O92 O92 117(4) 19_656 . . 18_565 ?
O92 C12 O92 O92 -63(4) 7_564 . . 18_565 ?
O12 C9 N13 C10 -175(2) . . . . ?
O12 C9 N13 C11 1(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A N8 0.86 2.67 3.342(9) 136.2 18_565
N1 H1B S1 0.86 2.91 3.742(7) 165.1 2_654
N6 H6B N1 0.87 2.70 3.473(10) 148.4 19_656
N6 H6B N2 0.87 2.51 3.329(9) 156.6 19_656
N7 H7A N5 0.88 2.53 3.238(11) 138.6 .
N7 H7A N6 0.88 2.69 3.553(12) 168.7 .
N7 H7B S3 0.88 2.68 3.416(7) 141.8 17_664
N12 H12A N11 0.87 2.47 3.183(10) 139.7 7_564
N12 H12B S1 0.86 3.02 3.428(8) 110.9 5_566
O91 H91 O4 0.92 2.58 3.494(10) 180.0 6_655
O10 H101 S1 0.88 2.95 3.828(18) 179.4 13_665
O10 H102 O12 0.94 2.59 3.53(3) 180.0 .
C11 H11A S4 0.98 2.65 3.34(4) 127.7 12_645
C11 H11B O81 0.98 2.46 2.97(4) 112.3 .

_refine_diff_density_max         1.111
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.122

####################################################################### 
# 
# 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_20161128-jym-wh-ni_sq
_database_code_depnum_ccdc_archive 'CCDC 1589053'
_audit_update_record             
;
2018-08-24 deposited with the CCDC.
2018-10-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C48 H48 Co20 N72 O24 S24, O8 S2, C H4 O, 6(C3 H7 N O), 3(H2 O)'
_chemical_formula_sum            'C67 H100 N78 Ni20 O42 S26'
_chemical_formula_weight         4678.00

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

_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_H-M_alt        'P a -3'
_space_group_name_Hall           '-P 2ac 2ab 3'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
'-z, -x, -y'
'-z-1/2, x-1/2, y'
'z-1/2, x, -y-1/2'
'z, -x-1/2, y-1/2'
'-y, -z, -x'
'y, -z-1/2, x-1/2'
'-y-1/2, z-1/2, x'
'y-1/2, z, -x-1/2'

_cell_length_a                   26.09030(10)
_cell_length_b                   26.09030(10)
_cell_length_c                   26.09030(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     17759.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    39595
_cell_measurement_theta_min      3.4900
_cell_measurement_theta_max      36.7600

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.750
_exptl_crystal_F_000             9440
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.170
_exptl_absorpt_coefficient_mu    2.454
_shelx_estimated_absorpt_T_min   0.526
_shelx_estimated_absorpt_T_max   0.680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.513
_exptl_absorpt_correction_T_max  0.659
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            191320
_diffrn_reflns_av_unetI/netI     0.0122
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         3.219
_diffrn_reflns_theta_max         25.018
_diffrn_reflns_theta_full        25.018
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5215
_reflns_number_gt                4293
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 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.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  'SHELXTL (Bruker, 1998)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0594P)²+94.0735P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5215
_refine_ls_number_parameters     333
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0491
_refine_ls_wR_factor_ref         0.1516
_refine_ls_wR_factor_gt          0.1215
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.073
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.61128(3) 0.71333(3) -0.17381(3) 0.0450(2) Uani 1 1 d . . . . .
Ni2 Ni 0.44774(3) 0.68998(3) -0.10998(3) 0.0425(2) Uani 1 1 d . . . . .
Ni3 Ni 0.40135(3) 0.77723(3) 0.03717(3) 0.0495(2) Uani 1 1 d . . . . .
Ni4 Ni 0.36971(3) 0.63029(3) 0.13029(3) 0.0463(3) Uani 1 3 d S T P . .
S1 S 0.68875(6) 0.71183(6) -0.20289(6) 0.0509(4) Uani 1 1 d . . . . .
S2 S 0.56682(6) 0.75410(8) -0.23114(7) 0.0628(5) Uani 1 1 d . . . . .
S3 S 0.43455(7) 0.83892(6) -0.00740(7) 0.0590(4) Uani 1 1 d . . . . .
S4 S 0.39102(8) 0.80867(7) 0.11346(7) 0.0654(5) Uani 1 1 d . . . . .
O1 O 0.61631(14) 0.64023(15) -0.04167(14) 0.0423(9) Uani 1 1 d . . . . .
O2 O 0.51298(14) 0.67557(15) -0.06568(14) 0.0435(9) Uani 1 1 d . . . . .
O3 O 0.40511(15) 0.65597(15) -0.05232(15) 0.0452(9) Uani 1 1 d . . . . .
O4 O 0.37193(15) 0.62985(15) 0.05040(15) 0.0466(9) Uani 1 1 d . . . . .
N1 N 0.76534(19) 0.6649(2) -0.1525(2) 0.0573(13) Uani 1 1 d . . . . .
H1A H 0.7693 0.6349 -0.1400 0.069 Uiso 1 1 d R U . . .
H1B H 0.7768 0.6651 -0.1831 0.069 Uiso 1 1 d R U . . .
N2 N 0.68700(17) 0.66084(18) -0.11353(17) 0.0431(11) Uani 1 1 d . . . . .
N3 N 0.63648(17) 0.67759(18) -0.11841(18) 0.0428(11) Uani 1 1 d . . . . .
N4 N 0.55063(17) 0.70554(19) -0.13940(17) 0.0437(11) Uani 1 1 d . . . . .
N5 N 0.50287(18) 0.72179(19) -0.15745(18) 0.0459(11) Uani 1 1 d . . . . .
N6 N 0.4651(2) 0.7640(2) -0.2244(2) 0.0651(16) Uani 1 1 d . . . . .
H6A H 0.4626 0.7508 -0.2547 0.078 Uiso 1 1 d R U . . .
H6B H 0.4374 0.7558 -0.2079 0.078 Uiso 1 1 d R U . . .
N7 N 0.4668(3) 0.8250(2) -0.1033(3) 0.082(2) Uani 1 1 d . . . . .
H7A H 0.4718 0.8075 -0.1316 0.099 Uiso 1 1 calc R U . . .
H7B H 0.4768 0.8572 -0.1013 0.099 Uiso 1 1 calc R U . . .
N8 N 0.42942(18) 0.75502(18) -0.06717(19) 0.0470(11) Uani 1 1 d . . . . .
N9 N 0.40761(18) 0.73830(18) -0.02117(19) 0.0457(11) Uani 1 1 d . . . . .
N10 N 0.37884(19) 0.71659(19) 0.06480(19) 0.0489(12) Uani 1 1 d . . . . .
N11 N 0.36881(19) 0.70851(19) 0.11696(19) 0.0480(11) Uani 1 1 d . . . . .
N12 N 0.3658(3) 0.7503(2) 0.1940(2) 0.0692(16) Uani 1 1 d . . . . .
H12A H 0.3748 0.7213 0.2068 0.083 Uiso 1 1 d R U . . .
H12B H 0.3829 0.7738 0.2094 0.083 Uiso 1 1 d R U . . .
C1 C 0.7144(2) 0.6756(2) -0.1525(2) 0.0452(13) Uani 1 1 d . . . . .
C2 C 0.6048(2) 0.6652(2) -0.0814(2) 0.0385(12) Uani 1 1 d . . . . .
C3 C 0.5512(2) 0.6830(2) -0.0944(2) 0.0408(12) Uani 1 1 d . . . . .
C4 C 0.5076(2) 0.7451(3) -0.2010(2) 0.0519(15) Uani 1 1 d . . . . .
C5 C 0.4437(3) 0.8027(2) -0.0628(3) 0.0551(15) Uani 1 1 d . . . . .
C6 C 0.3984(2) 0.6888(2) -0.0181(2) 0.0415(12) Uani 1 1 d . . . . .
C7 C 0.3809(2) 0.6750(2) 0.0360(2) 0.0430(12) Uani 1 1 d . . . . .
C8 C 0.3747(3) 0.7507(2) 0.1426(2) 0.0526(15) Uani 1 1 d . . . . .
S5 S 0.4226(4) 0.4424(3) 0.2210(5) 0.154(5) Uani 0.3333 1 d D . P . .
O5 O 0.4405(6) 0.4540(12) 0.1691(8) 0.186(17) Uani 0.3333 1 d D . P . .
O6 O 0.3686(5) 0.4373(10) 0.2212(7) 0.148(12) Uani 0.3333 1 d D . P . .
O7 O 0.4429(7) 0.4898(6) 0.2383(10) 0.142(10) Uani 0.3333 1 d D . P . .
O8 O 0.4520(10) 0.3996(7) 0.2406(9) 0.164(13) Uani 0.3333 1 d D . P . .


_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 N4 1.831(5) . ?
Ni1 N3 1.841(5) . ?
Ni1 S1 2.1593(17) . ?
Ni1 S2 2.1714(17) . ?
Ni2 O3 2.071(4) . ?
Ni2 N5 2.072(5) . ?
Ni2 N2 2.079(5) 19_656 ?
Ni2 N8 2.087(5) . ?
Ni2 O2 2.092(4) . ?
Ni2 O1 2.096(4) 19_656 ?
Ni3 N10 1.835(5) . ?
Ni3 N9 1.837(5) . ?
Ni3 S3 2.1664(18) . ?
Ni3 S4 2.170(2) . ?
Ni4 N11 2.070(5) . ?
Ni4 N11 2.070(5) 10_655 ?
Ni4 N11 2.070(5) 7_564 ?
Ni4 O4 2.085(4) 10_655 ?
Ni4 O4 2.085(4) 7_564 ?
Ni4 O4 2.085(4) . ?
S1 C1 1.752(6) . ?
S2 C4 1.751(6) . ?
S3 C5 1.744(7) . ?
S4 C8 1.746(7) . ?
O1 C2 1.261(6) . ?
O1 Ni2 2.096(4) 22_565 ?
O2 C3 1.262(6) . ?
O3 C6 1.249(7) . ?
O4 C7 1.258(7) . ?
N1 C1 1.358(8) . ?
N1 H1A 0.8531 . ?
N1 H1B 0.8541 . ?
N2 C1 1.301(7) . ?
N2 N3 1.394(6) . ?
N2 Ni2 2.079(5) 22_565 ?
N3 C2 1.310(7) . ?
N4 C3 1.314(7) . ?
N4 N5 1.398(6) . ?
N5 C4 1.294(7) . ?
N6 C4 1.359(8) . ?
N6 H6A 0.8637 . ?
N6 H6B 0.8669 . ?
N7 C5 1.348(9) . ?
N7 H7A 0.8800 . ?
N7 H7B 0.8800 . ?
N8 C5 1.303(8) . ?
N8 N9 1.398(7) . ?
N9 C6 1.317(7) . ?
N10 C7 1.321(7) . ?
N10 N11 1.402(7) . ?
N11 C8 1.297(8) . ?
N12 C8 1.360(8) . ?
N12 H12A 0.8595 . ?
N12 H12B 0.8595 . ?
C2 C3 1.512(7) . ?
C6 C7 1.526(8) . ?
S5 O6 1.416(9) . ?
S5 O7 1.420(9) . ?
S5 O8 1.447(9) . ?
S5 O5 1.465(9) . ?

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
N4 Ni1 N3 82.4(2) . . ?
N4 Ni1 S1 168.35(15) . . ?
N3 Ni1 S1 86.12(15) . . ?
N4 Ni1 S2 86.01(15) . . ?
N3 Ni1 S2 168.39(15) . . ?
S1 Ni1 S2 105.48(7) . . ?
O3 Ni2 N5 168.22(17) . . ?
O3 Ni2 N2 91.99(17) . 19_656 ?
N5 Ni2 N2 99.63(18) . 19_656 ?
O3 Ni2 N8 80.59(17) . . ?
N5 Ni2 N8 98.81(19) . . ?
N2 Ni2 N8 101.30(19) 19_656 . ?
O3 Ni2 O2 87.63(15) . . ?
N5 Ni2 O2 80.63(16) . . ?
N2 Ni2 O2 166.36(17) 19_656 . ?
N8 Ni2 O2 92.10(17) . . ?
O3 Ni2 O1 87.22(15) . 19_656 ?
N5 Ni2 O1 92.91(18) . 19_656 ?
N2 Ni2 O1 80.03(16) 19_656 19_656 ?
N8 Ni2 O1 167.77(17) . 19_656 ?
O2 Ni2 O1 86.33(15) . 19_656 ?
N10 Ni3 N9 83.0(2) . . ?
N10 Ni3 S3 168.35(17) . . ?
N9 Ni3 S3 86.02(15) . . ?
N10 Ni3 S4 85.74(17) . . ?
N9 Ni3 S4 168.57(16) . . ?
S3 Ni3 S4 105.14(7) . . ?
N11 Ni4 N11 98.99(18) . 10_655 ?
N11 Ni4 N11 98.99(18) . 7_564 ?
N11 Ni4 N11 98.99(18) 10_655 7_564 ?
N11 Ni4 O4 168.73(18) . 10_655 ?
N11 Ni4 O4 80.66(17) 10_655 10_655 ?
N11 Ni4 O4 92.17(18) 7_564 10_655 ?
N11 Ni4 O4 92.17(18) . 7_564 ?
N11 Ni4 O4 168.73(18) 10_655 7_564 ?
N11 Ni4 O4 80.66(17) 7_564 7_564 ?
O4 Ni4 O4 88.08(17) 10_655 7_564 ?
N11 Ni4 O4 80.66(17) . . ?
N11 Ni4 O4 92.17(18) 10_655 . ?
N11 Ni4 O4 168.73(18) 7_564 . ?
O4 Ni4 O4 88.08(16) 10_655 . ?
O4 Ni4 O4 88.08(17) 7_564 . ?
C1 S1 Ni1 96.0(2) . . ?
C4 S2 Ni1 95.5(2) . . ?
C5 S3 Ni3 95.6(2) . . ?
C8 S4 Ni3 95.9(2) . . ?
C2 O1 Ni2 107.7(3) . 22_565 ?
C3 O2 Ni2 106.8(3) . . ?
C6 O3 Ni2 107.5(3) . . ?
C7 O4 Ni4 107.4(4) . . ?
C1 N1 H1A 108.0 . . ?
C1 N1 H1B 109.9 . . ?
H1A N1 H1B 108.6 . . ?
C1 N2 N3 110.8(5) . . ?
C1 N2 Ni2 140.3(4) . 22_565 ?
N3 N2 Ni2 107.8(3) . 22_565 ?
C2 N3 N2 116.8(4) . . ?
C2 N3 Ni1 118.5(4) . . ?
N2 N3 Ni1 124.6(3) . . ?
C3 N4 N5 116.6(5) . . ?
C3 N4 Ni1 118.6(4) . . ?
N5 N4 Ni1 124.9(3) . . ?
C4 N5 N4 110.7(5) . . ?
C4 N5 Ni2 141.1(4) . . ?
N4 N5 Ni2 107.2(3) . . ?
C4 N6 H6A 109.1 . . ?
C4 N6 H6B 111.4 . . ?
H6A N6 H6B 107.2 . . ?
C5 N7 H7A 120.0 . . ?
C5 N7 H7B 120.0 . . ?
H7A N7 H7B 120.0 . . ?
C5 N8 N9 109.8(5) . . ?
C5 N8 Ni2 139.2(5) . . ?
N9 N8 Ni2 107.4(3) . . ?
C6 N9 N8 115.6(5) . . ?
C6 N9 Ni3 118.4(4) . . ?
N8 N9 Ni3 125.1(4) . . ?
C7 N10 N11 115.9(5) . . ?
C7 N10 Ni3 118.1(4) . . ?
N11 N10 Ni3 124.8(4) . . ?
C8 N11 N10 110.5(5) . . ?
C8 N11 Ni4 138.4(4) . . ?
N10 N11 Ni4 108.0(3) . . ?
C8 N12 H12A 110.1 . . ?
C8 N12 H12B 111.6 . . ?
H12A N12 H12B 107.6 . . ?
N2 C1 N1 118.4(5) . . ?
N2 C1 S1 122.4(5) . . ?
N1 C1 S1 119.0(4) . . ?
O1 C2 N3 125.7(5) . . ?
O1 C2 C3 124.2(5) . . ?
N3 C2 C3 110.1(5) . . ?
O2 C3 N4 126.1(5) . . ?
O2 C3 C2 123.5(5) . . ?
N4 C3 C2 110.3(5) . . ?
N5 C4 N6 119.2(6) . . ?
N5 C4 S2 122.8(5) . . ?
N6 C4 S2 118.0(4) . . ?
N8 C5 N7 118.2(6) . . ?
N8 C5 S3 123.4(5) . . ?
N7 C5 S3 118.4(5) . . ?
O3 C6 N9 127.1(5) . . ?
O3 C6 C7 122.8(5) . . ?
N9 C6 C7 110.0(5) . . ?
O4 C7 N10 126.3(5) . . ?
O4 C7 C6 123.5(5) . . ?
N10 C7 C6 110.2(5) . . ?
N11 C8 N12 118.8(6) . . ?
N11 C8 S4 122.7(5) . . ?
N12 C8 S4 118.5(5) . . ?
O6 S5 O7 116.8(13) . . ?
O6 S5 O8 117.0(16) . . ?
O7 S5 O8 111.3(12) . . ?
O6 S5 O5 109.9(10) . . ?
O7 S5 O5 89.7(18) . . ?
O8 S5 O5 108.6(11) . . ?

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
C1 N2 N3 C2 -179.9(5) . . . . ?
Ni2 N2 N3 C2 9.7(6) 22_565 . . . ?
C1 N2 N3 Ni1 2.4(7) . . . . ?
Ni2 N2 N3 Ni1 -168.0(3) 22_565 . . . ?
N4 Ni1 N3 C2 -2.6(4) . . . . ?
S1 Ni1 N3 C2 179.2(4) . . . . ?
S2 Ni1 N3 C2 -1.7(11) . . . . ?
N4 Ni1 N3 N2 175.0(5) . . . . ?
S1 Ni1 N3 N2 -3.2(4) . . . . ?
S2 Ni1 N3 N2 175.9(6) . . . . ?
N3 Ni1 N4 C3 3.1(4) . . . . ?
S1 Ni1 N4 C3 12.4(12) . . . . ?
S2 Ni1 N4 C3 -176.8(4) . . . . ?
N3 Ni1 N4 N5 -176.8(5) . . . . ?
S1 Ni1 N4 N5 -167.5(6) . . . . ?
S2 Ni1 N4 N5 3.4(4) . . . . ?
C3 N4 N5 C4 177.5(5) . . . . ?
Ni1 N4 N5 C4 -2.6(7) . . . . ?
C3 N4 N5 Ni2 -11.1(6) . . . . ?
Ni1 N4 N5 Ni2 168.7(3) . . . . ?
C5 N8 N9 C6 -170.5(5) . . . . ?
Ni2 N8 N9 C6 -7.5(5) . . . . ?
C5 N8 N9 Ni3 -1.3(7) . . . . ?
Ni2 N8 N9 Ni3 161.7(3) . . . . ?
N10 Ni3 N9 C6 -4.7(4) . . . . ?
S3 Ni3 N9 C6 171.5(4) . . . . ?
S4 Ni3 N9 C6 4.0(11) . . . . ?
N10 Ni3 N9 N8 -173.7(5) . . . . ?
S3 Ni3 N9 N8 2.6(4) . . . . ?
S4 Ni3 N9 N8 -164.9(6) . . . . ?
N9 Ni3 N10 C7 5.4(4) . . . . ?
S3 Ni3 N10 C7 -13.6(12) . . . . ?
S4 Ni3 N10 C7 -172.8(4) . . . . ?
N9 Ni3 N10 N11 172.5(5) . . . . ?
S3 Ni3 N10 N11 153.4(6) . . . . ?
S4 Ni3 N10 N11 -5.8(4) . . . . ?
C7 N10 N11 C8 171.0(5) . . . . ?
Ni3 N10 N11 C8 3.7(7) . . . . ?
C7 N10 N11 Ni4 6.9(6) . . . . ?
Ni3 N10 N11 Ni4 -160.4(3) . . . . ?
N3 N2 C1 N1 176.4(5) . . . . ?
Ni2 N2 C1 N1 -18.0(10) 22_565 . . . ?
N3 N2 C1 S1 0.3(7) . . . . ?
Ni2 N2 C1 S1 165.9(3) 22_565 . . . ?
Ni1 S1 C1 N2 -2.1(5) . . . . ?
Ni1 S1 C1 N1 -178.2(5) . . . . ?
Ni2 O1 C2 N3 -11.0(6) 22_565 . . . ?
Ni2 O1 C2 C3 165.7(4) 22_565 . . . ?
N2 N3 C2 O1 1.0(8) . . . . ?
Ni1 N3 C2 O1 178.8(4) . . . . ?
N2 N3 C2 C3 -176.0(4) . . . . ?
Ni1 N3 C2 C3 1.8(6) . . . . ?
Ni2 O2 C3 N4 12.9(7) . . . . ?
Ni2 O2 C3 C2 -165.4(4) . . . . ?
N5 N4 C3 O2 -1.4(9) . . . . ?
Ni1 N4 C3 O2 178.7(4) . . . . ?
N5 N4 C3 C2 177.1(4) . . . . ?
Ni1 N4 C3 C2 -2.8(6) . . . . ?
O1 C2 C3 O2 2.1(9) . . . . ?
N3 C2 C3 O2 179.2(5) . . . . ?
O1 C2 C3 N4 -176.5(5) . . . . ?
N3 C2 C3 N4 0.6(7) . . . . ?
N4 N5 C4 N6 -179.5(6) . . . . ?
Ni2 N5 C4 N6 13.7(11) . . . . ?
N4 N5 C4 S2 -0.3(8) . . . . ?
Ni2 N5 C4 S2 -167.1(4) . . . . ?
Ni1 S2 C4 N5 2.2(6) . . . . ?
Ni1 S2 C4 N6 -178.5(5) . . . . ?
N9 N8 C5 N7 178.5(6) . . . . ?
Ni2 N8 C5 N7 23.8(10) . . . . ?
N9 N8 C5 S3 -1.5(7) . . . . ?
Ni2 N8 C5 S3 -156.2(4) . . . . ?
Ni3 S3 C5 N8 2.8(6) . . . . ?
Ni3 S3 C5 N7 -177.2(6) . . . . ?
Ni2 O3 C6 N9 11.9(7) . . . . ?
Ni2 O3 C6 C7 -164.0(4) . . . . ?
N8 N9 C6 O3 -3.2(8) . . . . ?
Ni3 N9 C6 O3 -173.2(4) . . . . ?
N8 N9 C6 C7 173.1(4) . . . . ?
Ni3 N9 C6 C7 3.2(6) . . . . ?
Ni4 O4 C7 N10 -12.7(7) . . . . ?
Ni4 O4 C7 C6 164.4(4) . . . . ?
N11 N10 C7 O4 4.3(8) . . . . ?
Ni3 N10 C7 O4 172.5(4) . . . . ?
N11 N10 C7 C6 -173.1(4) . . . . ?
Ni3 N10 C7 C6 -4.9(6) . . . . ?
O3 C6 C7 O4 0.1(8) . . . . ?
N9 C6 C7 O4 -176.4(5) . . . . ?
O3 C6 C7 N10 177.6(5) . . . . ?
N9 C6 C7 N10 1.1(6) . . . . ?
N10 N11 C8 N12 179.0(6) . . . . ?
Ni4 N11 C8 N12 -24.1(10) . . . . ?
N10 N11 C8 S4 1.9(8) . . . . ?
Ni4 N11 C8 S4 158.9(4) . . . . ?
Ni3 S4 C8 N11 -5.1(6) . . . . ?
Ni3 S4 C8 N12 177.8(5) . . . . ?

_refine_diff_density_max         0.832
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.101



