# 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_Na3[1]
_database_code_depnum_ccdc_archive 'CCDC 1581365'
_audit_update_record             
;
2018-01-11 deposited with the CCDC.
2018-01-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H84 Co2 Cu3 N6 Na3 O23 S6'
_chemical_formula_weight         1514.88

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'
Cu Cu 0.3201 1.2651 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 2'
_space_group_name_Hall           'C 2y'

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

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

_cell_length_a                   11.7354(7)
_cell_length_b                   20.308(3)
_cell_length_c                   13.771(3)
_cell_angle_alpha                90
_cell_angle_beta                 107.289(11)
_cell_angle_gamma                90
_cell_volume                     3133.7(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    12525
_cell_measurement_theta_min      3.099
_cell_measurement_theta_max      27.482

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_F_000             1568
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    1.813
_shelx_estimated_absorpt_T_min   0.839
_shelx_estimated_absorpt_T_max   0.965
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_correction_T_min  0.7904
_exptl_absorpt_correction_T_max  1.0000

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_measurement_device_type  'Rigaku R-AXIS VII'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12525
_diffrn_reflns_av_unetI/netI     0.0889
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.099
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_point_group_measured_fraction_full 0.979
_reflns_number_total             6916
_reflns_number_gt                5761
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.869
_reflns_Friedel_fraction_max     0.918
_reflns_Friedel_fraction_full    0.961

_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       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    Mercury
_computing_publication_material  WinGX

_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)+(0.0280P)²] 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_abs_structure_details 
;
 Flack x determined using 2089 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.053(9)
_chemical_absolute_configuration rmad
_refine_ls_number_reflns         6916
_refine_ls_number_parameters     369
_refine_ls_number_restraints     53
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0507
_refine_ls_wR_factor_ref         0.0795
_refine_ls_wR_factor_gt          0.0756
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.042
_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
Cu1 Cu 0.61068(6) 0.28044(4) -0.01197(5) 0.02120(19) Uani 1 1 d . . . . .
Cu2 Cu 0.5000 0.39557(5) 0.0000 0.0218(3) Uani 1 2 d S T P . .
Co1 Co 0.61349(7) 0.32039(4) 0.24522(6) 0.01406(19) Uani 1 1 d . . . . .
S1 S 0.48077(13) 0.24314(8) 0.16287(11) 0.0188(4) Uani 1 1 d . . . . .
C1 C 0.3684(5) 0.2453(3) 0.2363(4) 0.0215(15) Uani 1 1 d . . . . .
C2 C 0.4435(5) 0.2639(3) 0.3452(4) 0.0167(14) Uani 1 1 d . . . . .
H2 H 0.4979 0.2263 0.3739 0.020 Uiso 1 1 calc R U . . .
C3 C 0.3657(5) 0.2766(4) 0.4155(4) 0.0199(14) Uani 1 1 d . . . . .
C4 C 0.2688(5) 0.2947(3) 0.1916(5) 0.0300(17) Uani 1 1 d . . . . .
H4A H 0.3027 0.3391 0.1952 0.045 Uiso 1 1 calc R U . . .
H4B H 0.2285 0.2834 0.1205 0.045 Uiso 1 1 calc R U . . .
H4C H 0.2111 0.2934 0.2305 0.045 Uiso 1 1 calc R U . . .
C5 C 0.3170(6) 0.1759(3) 0.2313(5) 0.0325(18) Uani 1 1 d . . . . .
H5A H 0.3817 0.1445 0.2602 0.049 Uiso 1 1 calc R U . . .
H5B H 0.2594 0.1743 0.2703 0.049 Uiso 1 1 calc R U . . .
H5C H 0.2769 0.1643 0.1603 0.049 Uiso 1 1 calc R U . . .
N1 N 0.5182(4) 0.3223(3) 0.3420(3) 0.0173(11) Uani 1 1 d . . . . .
H1A H 0.5692 0.3285 0.4055 0.021 Uiso 1 1 calc R U . . .
H1B H 0.4695 0.3581 0.3272 0.021 Uiso 1 1 calc R U . . .
O1 O 0.3522(4) 0.3359(2) 0.4374(3) 0.0255(11) Uani 1 1 d . . . . .
O2 O 0.3249(4) 0.2281(2) 0.4484(3) 0.0313(12) Uani 1 1 d . . . . .
S2 S 0.72222(12) 0.31296(8) 0.13585(11) 0.0172(3) Uani 1 1 d . . . . .
C6 C 0.8266(5) 0.2448(3) 0.1928(5) 0.0216(15) Uani 1 1 d . . . . .
C7 C 0.8468(5) 0.2520(3) 0.3075(4) 0.0168(14) Uani 1 1 d . . . . .
H7 H 0.8858 0.2957 0.3279 0.020 Uiso 1 1 calc R U . . .
C8 C 0.9338(6) 0.1987(3) 0.3693(5) 0.0209(14) Uani 1 1 d . . . . .
C9 C 0.7729(6) 0.1776(3) 0.1529(5) 0.0289(16) Uani 1 1 d . . . . .
H9A H 0.6990 0.1709 0.1709 0.043 Uiso 1 1 calc R U . . .
H9B H 0.7555 0.1764 0.0788 0.043 Uiso 1 1 calc R U . . .
H9C H 0.8300 0.1428 0.1835 0.043 Uiso 1 1 calc R U . . .
C10 C 0.9420(5) 0.2563(4) 0.1656(5) 0.0363(19) Uani 1 1 d . . . . .
H10A H 0.9265 0.2514 0.0921 0.054 Uiso 1 1 calc R U . . .
H10B H 0.9715 0.3008 0.1862 0.054 Uiso 1 1 calc R U . . .
H10C H 1.0020 0.2240 0.2012 0.054 Uiso 1 1 calc R U . . .
N2 N 0.7290(4) 0.2541(2) 0.3284(4) 0.0182(12) Uani 1 1 d . . . . .
H2A H 0.7417 0.2634 0.3955 0.022 Uiso 1 1 calc R U . . .
H2B H 0.6951 0.2135 0.3165 0.022 Uiso 1 1 calc R U . . .
O3 O 1.0432(4) 0.2138(2) 0.3912(3) 0.0298(11) Uani 1 1 d . . . . .
O4 O 0.8906(3) 0.1472(2) 0.3912(3) 0.0239(11) Uani 1 1 d . . . . .
S3 S 0.49950(13) 0.40266(8) 0.15545(11) 0.0182(4) Uani 1 1 d . . . . .
C11 C 0.5904(5) 0.4759(3) 0.2119(5) 0.0222(15) Uani 1 1 d . . . . .
C12 C 0.6486(5) 0.4544(3) 0.3231(5) 0.0173(14) Uani 1 1 d . . . . .
H12 H 0.5835 0.4444 0.3541 0.021 Uiso 1 1 calc R U . . .
C13 C 0.7280(6) 0.5100(3) 0.3868(5) 0.0217(15) Uani 1 1 d . . . . .
C14 C 0.5024(6) 0.5331(3) 0.2040(6) 0.0357(19) Uani 1 1 d . . . . .
H14A H 0.4438 0.5211 0.2389 0.054 Uiso 1 1 calc R U . . .
H14B H 0.5461 0.5724 0.2358 0.054 Uiso 1 1 calc R U . . .
H14C H 0.4612 0.5421 0.1322 0.054 Uiso 1 1 calc R U . . .
C15 C 0.6820(6) 0.4933(3) 0.1583(5) 0.0279(16) Uani 1 1 d . . . . .
H15A H 0.7374 0.4563 0.1640 0.042 Uiso 1 1 calc R U . . .
H15B H 0.6415 0.5022 0.0864 0.042 Uiso 1 1 calc R U . . .
H15C H 0.7264 0.5325 0.1899 0.042 Uiso 1 1 calc R U . . .
N3 N 0.7168(4) 0.3928(2) 0.3224(4) 0.0170(12) Uani 1 1 d . . . . .
H3A H 0.7514 0.3794 0.3876 0.020 Uiso 1 1 calc R U . . .
H3B H 0.7761 0.4011 0.2940 0.020 Uiso 1 1 calc R U . . .
O5 O 0.8365(4) 0.5074(2) 0.3987(4) 0.0381(13) Uani 1 1 d . . . . .
O6 O 0.6714(4) 0.5518(2) 0.4195(3) 0.0309(12) Uani 1 1 d . . . . .
Na1 Na 0.5000 0.55261(17) 0.5000 0.0287(9) Uani 1 2 d S T P . .
Na2 Na 0.20796(19) 0.15189(11) 0.48415(18) 0.0227(6) Uani 1 1 d . . . . .
O1W O 1.1229(4) 0.6256(2) 0.3705(3) 0.0356(12) Uani 1 1 d . . . . .
H1WA H 1.1441 0.5959 0.3325 0.053 Uiso 1 1 d R U . . .
H1WB H 1.1038 0.6603 0.3306 0.053 Uiso 1 1 d R U . . .
O2W O 0.3839(4) 0.4678(2) 0.3922(4) 0.0375(13) Uani 1 1 d . . . . .
H2WA H 0.3115 0.4831 0.3569 0.056 Uiso 1 1 d R U . . .
H2WB H 0.3666 0.4351 0.4297 0.056 Uiso 1 1 d R U . . .
O3W O 1.1323(4) 0.33382(19) 0.4700(3) 0.0328(12) Uani 1 1 d G . . . .
H3WA H 1.1950 0.3355 0.4488 0.049 Uiso 1 1 d G U . . .
H3WB H 1.0965 0.2975 0.4442 0.049 Uiso 1 1 d G U . . .
O4W O 1.0000(19) 0.5933(3) 0.5000(8) 0.0336(18) Uani 1 2 d G T P . .
H4WA H 0.9316 0.5779 0.4613 0.050 Uiso 0.5 1 d G U P . .
H4WB H 1.0435 0.6001 0.4645 0.050 Uiso 0.5 1 d G U P . .
O5W O 0.9893(4) 0.4267(2) 0.3387(3) 0.0413(13) Uani 1 1 d G . . . .
H5WA H 0.9458 0.4440 0.3733 0.062 Uiso 1 1 d G U . . .
H5WB H 1.0369 0.3998 0.3811 0.062 Uiso 1 1 d G U . . .
O7A O 1.1462(4) 0.5020(3) 0.2771(4) 0.0495(14) Uani 0.46(2) 1 d D U P A 1
H7A H 1.0999 0.4818 0.3030 0.074 Uiso 0.46(2) 1 calc R U P A 1
O7B O 1.1462(4) 0.5020(3) 0.2771(4) 0.0495(14) Uani 0.54(2) 1 d D U P A 2
H7B H 1.0982 0.4767 0.2934 0.074 Uiso 0.54(2) 1 calc R U P A 2
C16A C 1.110(3) 0.4905(19) 0.1685(12) 0.092(14) Uani 0.46(2) 1 d D U P A 1
H16A H 1.0785 0.4453 0.1523 0.111 Uiso 0.46(2) 1 calc R U P A 1
H16B H 1.1778 0.4970 0.1406 0.111 Uiso 0.46(2) 1 calc R U P A 1
C17A C 1.013(3) 0.5415(14) 0.126(2) 0.137(14) Uani 0.46(2) 1 d D U P A 1
H17A H 0.9830 0.5371 0.0520 0.205 Uiso 0.46(2) 1 calc R U P A 1
H17B H 0.9472 0.5344 0.1554 0.205 Uiso 0.46(2) 1 calc R U P A 1
H17C H 1.0458 0.5857 0.1438 0.205 Uiso 0.46(2) 1 calc R U P A 1
C16B C 1.106(3) 0.5133(12) 0.1708(10) 0.073(9) Uani 0.54(2) 1 d D U P A 2
H16C H 1.1400 0.5555 0.1559 0.087 Uiso 0.54(2) 1 calc R U P A 2
H16D H 1.0182 0.5177 0.1489 0.087 Uiso 0.54(2) 1 calc R U P A 2
C17B C 1.139(2) 0.4617(13) 0.113(2) 0.177(14) Uani 0.54(2) 1 d D U P A 2
H17D H 1.1092 0.4723 0.0400 0.266 Uiso 0.54(2) 1 calc R U P A 2
H17E H 1.2263 0.4577 0.1326 0.266 Uiso 0.54(2) 1 calc R U P A 2
H17F H 1.1044 0.4199 0.1256 0.266 Uiso 0.54(2) 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 S2 2.1701(16) . ?
Cu1 S1 2.1722(17) 2_655 ?
Cu1 Cu2 2.7033(12) . ?
Cu1 Cu1 2.7140(14) 2_655 ?
Cu2 S3 2.1474(16) . ?
Cu2 S3 2.1474(16) 2_655 ?
Cu2 Cu1 2.7033(12) 2_655 ?
Co1 N1 1.979(4) . ?
Co1 N3 1.999(5) . ?
Co1 N2 2.009(5) . ?
Co1 S2 2.2498(16) . ?
Co1 S1 2.2634(17) . ?
Co1 S3 2.2641(17) . ?
S1 C1 1.886(6) . ?
S1 Cu1 2.1722(17) 2_655 ?
C1 C4 1.525(8) . ?
C1 C5 1.527(8) . ?
C1 C2 1.543(8) . ?
C2 N1 1.483(7) . ?
C2 C3 1.537(8) . ?
C3 O2 1.237(7) . ?
C3 O1 1.262(8) . ?
O2 Na2 2.220(5) . ?
S2 C6 1.860(6) . ?
C6 C10 1.526(8) . ?
C6 C7 1.533(8) . ?
C6 C9 1.534(8) . ?
C7 N2 1.494(7) . ?
C7 C8 1.556(8) . ?
C8 O4 1.239(7) . ?
C8 O3 1.266(7) . ?
C8 Na2 3.121(7) 2_656 ?
O3 Na2 2.343(5) 1_655 ?
O4 Na2 2.340(5) 2_656 ?
O4 Na1 2.537(5) 3_545 ?
S3 C11 1.861(6) . ?
C11 C15 1.515(8) . ?
C11 C14 1.535(8) . ?
C11 C12 1.544(8) . ?
C12 N3 1.487(7) . ?
C12 C13 1.558(8) . ?
C13 O5 1.236(7) . ?
C13 O6 1.242(7) . ?
O6 Na2 2.209(5) 3 ?
O6 Na1 2.569(5) . ?
Na1 O2W 2.413(5) 2_656 ?
Na1 O2W 2.413(5) . ?
Na1 O4 2.537(5) 4_656 ?
Na1 O4 2.537(5) 3_455 ?
Na1 O6 2.569(5) 2_656 ?
Na1 Na2 3.222(3) 3 ?
Na1 Na2 3.222(3) 4_556 ?
Na2 O6 2.209(5) 3_445 ?
Na2 O4 2.340(5) 2_656 ?
Na2 O3 2.343(5) 1_455 ?
Na2 O1W 2.423(5) 4_646 ?
Na2 C8 3.121(7) 2_656 ?
Na2 Na1 3.223(3) 3_445 ?
O1W Na2 2.423(5) 4_656 ?
O7A C16A 1.447(14) . ?
C16A C17A 1.521(18) . ?
C16B C17B 1.440(17) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S2 Cu1 S1 172.88(7) . 2_655 ?
S2 Cu1 Cu2 81.17(5) . . ?
S1 Cu1 Cu2 104.49(5) 2_655 . ?
S2 Cu1 Cu1 102.61(5) . 2_655 ?
S1 Cu1 Cu1 84.12(5) 2_655 2_655 ?
Cu2 Cu1 Cu1 59.869(19) . 2_655 ?
S3 Cu2 S3 172.31(10) . 2_655 ?
S3 Cu2 Cu1 81.58(5) . 2_655 ?
S3 Cu2 Cu1 105.22(5) 2_655 2_655 ?
S3 Cu2 Cu1 105.22(5) . . ?
S3 Cu2 Cu1 81.58(5) 2_655 . ?
Cu1 Cu2 Cu1 60.26(4) 2_655 . ?
N1 Co1 N3 90.1(2) . . ?
N1 Co1 N2 92.8(2) . . ?
N3 Co1 N2 89.38(18) . . ?
N1 Co1 S2 177.27(16) . . ?
N3 Co1 S2 91.74(14) . . ?
N2 Co1 S2 85.18(15) . . ?
N1 Co1 S1 84.76(15) . . ?
N3 Co1 S1 174.02(15) . . ?
N2 Co1 S1 93.94(14) . . ?
S2 Co1 S1 93.49(6) . . ?
N1 Co1 S3 89.59(15) . . ?
N3 Co1 S3 85.09(14) . . ?
N2 Co1 S3 173.97(14) . . ?
S2 Co1 S3 92.56(6) . . ?
S1 Co1 S3 91.77(6) . . ?
C1 S1 Cu1 106.25(19) . 2_655 ?
C1 S1 Co1 101.6(2) . . ?
Cu1 S1 Co1 107.96(7) 2_655 . ?
C4 C1 C5 110.1(5) . . ?
C4 C1 C2 112.2(5) . . ?
C5 C1 C2 112.0(5) . . ?
C4 C1 S1 111.9(4) . . ?
C5 C1 S1 106.5(4) . . ?
C2 C1 S1 103.8(4) . . ?
N1 C2 C3 110.6(5) . . ?
N1 C2 C1 109.8(4) . . ?
C3 C2 C1 112.3(5) . . ?
O2 C3 O1 125.5(6) . . ?
O2 C3 C2 117.6(6) . . ?
O1 C3 C2 116.8(6) . . ?
C2 N1 Co1 117.5(4) . . ?
C3 O2 Na2 165.4(4) . . ?
C6 S2 Cu1 107.9(2) . . ?
C6 S2 Co1 101.6(2) . . ?
Cu1 S2 Co1 110.14(7) . . ?
C10 C6 C7 111.2(5) . . ?
C10 C6 C9 110.3(5) . . ?
C7 C6 C9 112.1(5) . . ?
C10 C6 S2 107.7(4) . . ?
C7 C6 S2 104.1(4) . . ?
C9 C6 S2 111.2(4) . . ?
N2 C7 C6 109.4(4) . . ?
N2 C7 C8 114.1(5) . . ?
C6 C7 C8 111.9(5) . . ?
O4 C8 O3 127.3(6) . . ?
O4 C8 C7 118.1(5) . . ?
O3 C8 C7 114.6(5) . . ?
O4 C8 Na2 41.4(3) . 2_656 ?
O3 C8 Na2 128.1(4) . 2_656 ?
C7 C8 Na2 100.2(3) . 2_656 ?
C7 N2 Co1 114.5(3) . . ?
C8 O3 Na2 127.9(4) . 1_655 ?
C8 O4 Na2 118.1(4) . 2_656 ?
C8 O4 Na1 127.7(4) . 3_545 ?
Na2 O4 Na1 82.62(14) 2_656 3_545 ?
C11 S3 Cu2 107.4(2) . . ?
C11 S3 Co1 100.9(2) . . ?
Cu2 S3 Co1 108.58(7) . . ?
C15 C11 C14 110.5(5) . . ?
C15 C11 C12 112.3(5) . . ?
C14 C11 C12 112.0(5) . . ?
C15 C11 S3 112.6(4) . . ?
C14 C11 S3 106.6(4) . . ?
C12 C11 S3 102.6(4) . . ?
N3 C12 C11 108.2(5) . . ?
N3 C12 C13 112.4(5) . . ?
C11 C12 C13 111.6(5) . . ?
O5 C13 O6 128.5(6) . . ?
O5 C13 C12 117.6(6) . . ?
O6 C13 C12 113.9(6) . . ?
C12 N3 Co1 112.3(3) . . ?
C13 O6 Na2 135.6(4) . 3 ?
C13 O6 Na1 137.1(4) . . ?
Na2 O6 Na1 84.45(17) 3 . ?
O2W Na1 O2W 88.9(3) 2_656 . ?
O2W Na1 O4 94.77(15) 2_656 4_656 ?
O2W Na1 O4 175.95(17) . 4_656 ?
O2W Na1 O4 175.95(17) 2_656 3_455 ?
O2W Na1 O4 94.77(15) . 3_455 ?
O4 Na1 O4 81.6(2) 4_656 3_455 ?
O2W Na1 O6 83.66(16) 2_656 . ?
O2W Na1 O6 95.82(15) . . ?
O4 Na1 O6 86.33(14) 4_656 . ?
O4 Na1 O6 94.22(15) 3_455 . ?
O2W Na1 O6 95.82(16) 2_656 2_656 ?
O2W Na1 O6 83.66(16) . 2_656 ?
O4 Na1 O6 94.23(15) 4_656 2_656 ?
O4 Na1 O6 86.33(14) 3_455 2_656 ?
O6 Na1 O6 179.3(2) . 2_656 ?
O2W Na1 Na2 100.83(12) 2_656 3 ?
O2W Na1 Na2 134.86(12) . 3 ?
O4 Na1 Na2 46.06(11) 4_656 3 ?
O4 Na1 Na2 75.34(13) 3_455 3 ?
O6 Na1 Na2 43.03(11) . 3 ?
O6 Na1 Na2 137.65(16) 2_656 3 ?
O2W Na1 Na2 134.86(12) 2_656 4_556 ?
O2W Na1 Na2 100.83(12) . 4_556 ?
O4 Na1 Na2 75.34(13) 4_656 4_556 ?
O4 Na1 Na2 46.06(11) 3_455 4_556 ?
O6 Na1 Na2 137.65(16) . 4_556 ?
O6 Na1 Na2 43.03(11) 2_656 4_556 ?
Na2 Na1 Na2 102.55(13) 3 4_556 ?
O6 Na2 O2 127.7(2) 3_445 . ?
O6 Na2 O4 100.31(18) 3_445 2_656 ?
O2 Na2 O4 131.65(19) . 2_656 ?
O6 Na2 O3 104.14(18) 3_445 1_455 ?
O2 Na2 O3 88.20(17) . 1_455 ?
O4 Na2 O3 85.12(16) 2_656 1_455 ?
O6 Na2 O1W 98.25(18) 3_445 4_646 ?
O2 Na2 O1W 85.88(17) . 4_646 ?
O4 Na2 O1W 81.21(17) 2_656 4_646 ?
O3 Na2 O1W 155.52(19) 1_455 4_646 ?
O6 Na2 C8 117.65(19) 3_445 2_656 ?
O2 Na2 C8 114.49(19) . 2_656 ?
O4 Na2 C8 20.50(15) 2_656 2_656 ?
O3 Na2 C8 71.18(17) 1_455 2_656 ?
O1W Na2 C8 89.78(18) 4_646 2_656 ?
O6 Na2 Na1 52.52(13) 3_445 3_445 ?
O2 Na2 Na1 169.18(15) . 3_445 ?
O4 Na2 Na1 51.33(11) 2_656 3_445 ?
O3 Na2 Na1 81.62(13) 1_455 3_445 ?
O1W Na2 Na1 104.90(14) 4_646 3_445 ?
C8 Na2 Na1 65.60(13) 2_656 3_445 ?
O7A C16A C17A 104(2) . . ?

_refine_diff_density_max         0.904
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.090

_shelxl_version_number           2014-3

####################################################################### 
# 
# 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_[cr(h2o)6][1]_sq
_database_code_depnum_ccdc_archive 'CCDC 1581366'
_audit_update_record             
;
2017-12-18 deposited with the CCDC.
2018-01-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H67 Co2 Cr0.33 Cu3 N6 O20.50 S6'
_chemical_formula_weight         1358.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 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 0.3514 0.9518 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3195 0.6102 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3258 1.2392 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0059 0.0032 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0105 0.0059 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1222 0.1206 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           155
_space_group_name_H-M_alt        'R 3 2 :H'
_space_group_name_Hall           'R 3 2"'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'y+1/3, x+2/3, -z+2/3'

_cell_length_a                   24.812(5)
_cell_length_b                   24.812(5)
_cell_length_c                   67.434(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     35952(16)
_cell_formula_units_Z            18
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    117959
_cell_measurement_theta_min      0.893
_cell_measurement_theta_max      27.073

_exptl_crystal_description       plate
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_F_000             12564
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    1.334
_shelx_estimated_absorpt_T_min   0.815
_shelx_estimated_absorpt_T_max   0.949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4067
_exptl_absorpt_correction_T_max  0.9957
_exptl_absorpt_process_details   
;
(ABSCOR; Higashi, 1995)
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.701
_diffrn_radiation_type           synchrotron
_diffrn_radiation_monochromator  Si(311)
_diffrn_detector_area_resol_mean 14.69
_diffrn_source                   'SPring-8 BL02B1 bending magnet'
_diffrn_measurement_device_type  'Rigaku Mercury2CCD detector'
_diffrn_measurement_method       'w scan'
_diffrn_reflns_number            117959
_diffrn_reflns_av_unetI/netI     0.2277
_diffrn_reflns_av_R_equivalents  0.2954
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -87
_diffrn_reflns_limit_l_max       87
_diffrn_reflns_theta_min         0.893
_diffrn_reflns_theta_max         27.073
_diffrn_reflns_theta_full        24.872
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             18376
_reflns_number_gt                6101
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.870
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_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       'RAPID-AUTO (Rigaku Corporation)'
_computing_cell_refinement       'RAPID-AUTO (Rigaku Corporation)'
_computing_data_reduction        'RAPID-AUTO (Rigaku Corporation)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    Mercury
_computing_publication_material  WinGX

_refine_special_details          
;
 Several restraints (SADI, DELU, and SIMU) were applied
 to model molecules. SQUEEZE was applied for a huge vacant space 
 which was occuplied by a number of water molecules.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1896 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.032(16)
_chemical_absolute_configuration rmad
_refine_ls_number_reflns         18376
_refine_ls_number_parameters     554
_refine_ls_number_restraints     442
_refine_ls_R_factor_all          0.2139
_refine_ls_R_factor_gt           0.0760
_refine_ls_wR_factor_ref         0.2217
_refine_ls_wR_factor_gt          0.1667
_refine_ls_goodness_of_fit_ref   0.834
_refine_ls_restrained_S_all      0.835
_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
O1W O 0.3573(4) 0.7402(4) 0.02081(15) 0.080(3) Uani 1 1 d . . . . .
O2W O 0.2882(5) 0.6973(5) -0.01305(15) 0.098(3) Uani 1 1 d . . . . .
Cr1 Cr 0.3333 0.6667 0.00411(6) 0.0749(12) Uani 1 3 d S T P . .
Co1 Co 0.54120(9) 0.85348(9) 0.07856(3) 0.0722(6) Uani 1 1 d . . . . .
Co2 Co 0.68409(9) 1.14137(9) 0.09272(3) 0.0714(6) Uani 1 1 d . . . . .
Cu1 Cu 0.55386(9) 0.99728(8) 0.08306(3) 0.0800(6) Uani 1 1 d . . . . .
Cu2 Cu 0.65557(9) 1.00505(8) 0.06690(3) 0.0801(6) Uani 1 1 d . . . . .
Cu3 Cu 0.63847(9) 0.99062(8) 0.10563(3) 0.0814(6) Uani 1 1 d . . . . .
S1 S 0.51619(17) 0.91905(17) 0.06317(6) 0.0751(11) Uani 1 1 d D . . . .
C1 C 0.4306(6) 0.8792(6) 0.06693(19) 0.084(4) Uani 1 1 d D U . . .
C2 C 0.4156(6) 0.8098(5) 0.0674(2) 0.074(4) Uani 1 1 d D U . . .
H2 H 0.4292 0.8008 0.0545 0.089 Uiso 1 1 calc R U . . .
N1 N 0.4501(5) 0.8017(5) 0.08269(16) 0.072(3) Uani 1 1 d D . . . .
H1A H 0.4395 0.7610 0.0833 0.086 Uiso 1 1 calc R U . . .
H1B H 0.4400 0.8120 0.0945 0.086 Uiso 1 1 calc R U . . .
C3 C 0.3440(6) 0.7656(6) 0.0692(3) 0.076(5) Uani 1 1 d D U . . .
O1 O 0.3125(4) 0.7443(5) 0.05443(16) 0.082(3) Uani 1 1 d D . . . .
O2 O 0.3237(4) 0.7557(5) 0.08686(17) 0.085(3) Uani 1 1 d D . . . .
C4 C 0.4025(7) 0.8923(7) 0.0487(2) 0.099(5) Uani 1 1 d D U . . .
H4A H 0.4165 0.8806 0.0367 0.148 Uiso 1 1 calc R U . . .
H4B H 0.3570 0.8679 0.0495 0.148 Uiso 1 1 calc R U . . .
H4C H 0.4158 0.9367 0.0482 0.148 Uiso 1 1 calc R U . . .
C5 C 0.4101(7) 0.8965(7) 0.0858(2) 0.089(5) Uani 1 1 d D U . . .
H5A H 0.4288 0.8876 0.0972 0.133 Uiso 1 1 calc R U . . .
H5B H 0.4235 0.9410 0.0856 0.133 Uiso 1 1 calc R U . . .
H5C H 0.3646 0.8722 0.0868 0.133 Uiso 1 1 calc R U . . .
S2 S 0.64169(18) 0.91297(17) 0.07105(6) 0.0753(11) Uani 1 1 d D . . . .
C6 C 0.6477(7) 0.8836(6) 0.04618(18) 0.089(5) Uani 1 1 d D . . . .
C7 C 0.5936(5) 0.8151(6) 0.0470(2) 0.079(4) Uani 1 1 d D U . . .
H7 H 0.6046 0.7933 0.0574 0.094 Uiso 1 1 calc R U . . .
N2 N 0.5369(5) 0.8129(5) 0.05333(16) 0.072(3) Uani 1 1 d D . . . .
H2A H 0.5065 0.7723 0.0542 0.087 Uiso 1 1 calc R U . . .
H2B H 0.5253 0.8309 0.0438 0.087 Uiso 1 1 calc R U . . .
C8 C 0.5853(7) 0.7801(6) 0.0270(2) 0.076(5) Uani 1 1 d D U . . .
O3 O 0.5473(5) 0.7770(5) 0.01583(16) 0.092(3) Uani 1 1 d D . . . .
O4 O 0.6216(6) 0.7590(5) 0.02401(17) 0.106(4) Uani 1 1 d D U . . .
C9 C 0.6385(6) 0.9178(6) 0.02950(18) 0.072(4) Uani 1 1 d D . . . .
H9A H 0.5970 0.9132 0.0305 0.108 Uiso 1 1 calc R U . . .
H9B H 0.6701 0.9620 0.0302 0.108 Uiso 1 1 calc R U . . .
H9C H 0.6423 0.9006 0.0168 0.108 Uiso 1 1 calc R U . . .
C10 C 0.7114(6) 0.8893(7) 0.0453(2) 0.093(5) Uani 1 1 d D . . . .
H10A H 0.7160 0.8665 0.0564 0.139 Uiso 1 1 calc R U . . .
H10B H 0.7158 0.8719 0.0328 0.139 Uiso 1 1 calc R U . . .
H10C H 0.7436 0.9333 0.0461 0.139 Uiso 1 1 calc R U . . .
S3 S 0.55562(19) 0.90010(17) 0.10791(6) 0.0782(12) Uani 1 1 d D U . . .
C11 C 0.5786(7) 0.8539(6) 0.12369(19) 0.087(4) Uani 1 1 d D U . . .
C12 C 0.5416(8) 0.7879(6) 0.1143(2) 0.090(5) Uani 1 1 d D U . . .
H12 H 0.4963 0.7735 0.1158 0.108 Uiso 1 1 calc R U . . .
N3 N 0.5549(6) 0.7920(5) 0.09339(16) 0.077(4) Uani 1 1 d D . . . .
H3A H 0.5307 0.7538 0.0879 0.092 Uiso 1 1 calc R U . . .
H3B H 0.5953 0.8021 0.0918 0.092 Uiso 1 1 calc R U . . .
C13 C 0.5539(9) 0.7394(7) 0.1246(2) 0.097(6) Uani 1 1 d D . . . .
O5 O 0.5873(7) 0.7234(6) 0.1169(2) 0.132(5) Uani 1 1 d D . . . .
O6 O 0.5303(6) 0.7215(6) 0.1413(2) 0.128(5) Uani 1 1 d D . . . .
C14 C 0.6475(6) 0.8760(7) 0.1232(2) 0.092(5) Uani 1 1 d D . . . .
H14A H 0.6602 0.8745 0.1095 0.138 Uiso 1 1 calc R U . . .
H14B H 0.6708 0.9188 0.1281 0.138 Uiso 1 1 calc R U . . .
H14C H 0.6561 0.8490 0.1316 0.138 Uiso 1 1 calc R U . . .
C15 C 0.5600(8) 0.8565(8) 0.14479(19) 0.123(7) Uani 1 1 d D . . . .
H15A H 0.5154 0.8423 0.1453 0.185 Uiso 1 1 calc R U . . .
H15B H 0.5689 0.8295 0.1531 0.185 Uiso 1 1 calc R U . . .
H15C H 0.5836 0.8994 0.1497 0.185 Uiso 1 1 calc R U . . .
S4 S 0.58622(19) 1.07512(18) 0.10234(6) 0.0801(12) Uani 1 1 d D . . . .
C16 C 0.5458(6) 1.1168(6) 0.0946(2) 0.078(4) Uani 1 1 d D U . . .
C17 C 0.5962(6) 1.1858(6) 0.0950(2) 0.082(4) Uani 1 1 d D U . . .
H17 H 0.6096 1.1955 0.1092 0.098 Uiso 1 1 calc R U . . .
N4 N 0.6505(5) 1.1966(5) 0.08420(19) 0.089(4) Uani 1 1 d D . . . .
H4D H 0.6807 1.2370 0.0858 0.107 Uiso 1 1 calc R U . . .
H4E H 0.6410 1.1904 0.0711 0.107 Uiso 1 1 calc R U . . .
C18 C 0.5720(10) 1.2302(9) 0.0892(3) 0.117(9) Uani 1 1 d D . . . .
O7 O 0.5736(7) 1.2428(6) 0.0721(3) 0.137(6) Uani 1 1 d D . . . .
O8 O 0.5492(8) 1.2450(7) 0.1031(3) 0.153(7) Uani 1 1 d D . . . .
C19 C 0.4969(8) 1.1026(8) 0.1088(3) 0.129(7) Uani 1 1 d D U . . .
H19A H 0.5151 1.1158 0.1220 0.193 Uiso 1 1 calc R U . . .
H19B H 0.4748 1.1247 0.1051 0.193 Uiso 1 1 calc R U . . .
H19C H 0.4677 1.0577 0.1088 0.193 Uiso 1 1 calc R U . . .
C20 C 0.5222(8) 1.0980(7) 0.0736(2) 0.103(5) Uani 1 1 d D U . . .
H20A H 0.5575 1.1088 0.0647 0.155 Uiso 1 1 calc R U . . .
H20B H 0.4934 1.0530 0.0731 0.155 Uiso 1 1 calc R U . . .
H20C H 0.5006 1.1200 0.0694 0.155 Uiso 1 1 calc R U . . .
S5 S 0.6691(2) 1.09658(18) 0.06251(6) 0.0815(12) Uani 1 1 d D . . . .
C21 C 0.7470(6) 1.1434(7) 0.0511(2) 0.104(5) Uani 1 1 d D U . . .
C22 C 0.7722(6) 1.2080(6) 0.06150(19) 0.090(5) Uani 1 1 d D U . . .
H22 H 0.7474 1.2272 0.0568 0.107 Uiso 1 1 calc R U . . .
N5 N 0.7642(6) 1.1987(6) 0.08254(16) 0.100(4) Uani 1 1 d D U . . .
H5D H 0.7763 1.2363 0.0882 0.120 Uiso 1 1 calc R U . . .
H5E H 0.7911 1.1863 0.0868 0.120 Uiso 1 1 calc R U . . .
C23 C 0.8429(7) 1.2536(7) 0.0564(3) 0.097(5) Uani 1 1 d D U . . .
O9 O 0.8808(7) 1.2627(6) 0.06884(19) 0.134(5) Uani 1 1 d D U . . .
O10 O 0.8526(5) 1.2763(5) 0.03981(18) 0.111(4) Uani 1 1 d D U . . .
C24 C 0.7370(8) 1.1488(7) 0.02963(19) 0.113(6) Uani 1 1 d D U . . .
H24A H 0.7107 1.1677 0.0280 0.169 Uiso 1 1 calc R U . . .
H24B H 0.7771 1.1750 0.0231 0.169 Uiso 1 1 calc R U . . .
H24C H 0.7164 1.1074 0.0236 0.169 Uiso 1 1 calc R U . . .
C25 C 0.7864(8) 1.1154(8) 0.0556(2) 0.111(5) Uani 1 1 d D U . . .
H25A H 0.7905 1.1137 0.0700 0.166 Uiso 1 1 calc R U . . .
H25B H 0.7669 1.0733 0.0501 0.166 Uiso 1 1 calc R U . . .
H25C H 0.8276 1.1409 0.0497 0.166 Uiso 1 1 calc R U . . .
S6 S 0.71926(18) 1.08089(17) 0.10498(6) 0.0775(11) Uani 1 1 d D . . . .
C26 C 0.7387(7) 1.1085(6) 0.13081(18) 0.091(5) Uani 1 1 d D U . . .
C27 C 0.7538(8) 1.1777(6) 0.1291(2) 0.105(5) Uani 1 1 d D U . . .
H27 H 0.7932 1.2002 0.1213 0.126 Uiso 1 1 calc R U . . .
N6 N 0.7078(6) 1.1847(6) 0.11850(19) 0.100(4) Uani 1 1 d D . . . .
H6A H 0.7225 1.2260 0.1164 0.120 Uiso 1 1 calc R U . . .
H6B H 0.6731 1.1702 0.1262 0.120 Uiso 1 1 calc R U . . .
C28 C 0.7672(10) 1.2108(8) 0.1497(3) 0.136(8) Uani 1 1 d D U . . .
O11 O 0.8187(8) 1.2330(7) 0.1557(2) 0.155(6) Uani 1 1 d D U . . .
O12 O 0.7231(10) 1.2151(10) 0.1574(3) 0.264(14) Uani 1 1 d D U . . .
C29 C 0.7940(7) 1.1023(7) 0.1359(2) 0.100(6) Uani 1 1 d D . . . .
H29A H 0.8276 1.1262 0.1264 0.150 Uiso 1 1 calc R U . . .
H29B H 0.8082 1.1182 0.1493 0.150 Uiso 1 1 calc R U . . .
H29C H 0.7825 1.0583 0.1353 0.150 Uiso 1 1 calc R U . . .
C30 C 0.6850(7) 1.0733(7) 0.1446(2) 0.097(5) Uani 1 1 d D U . . .
H30A H 0.6503 1.0791 0.1405 0.145 Uiso 1 1 calc R U . . .
H30B H 0.6719 1.0290 0.1441 0.145 Uiso 1 1 calc R U . . .
H30C H 0.6976 1.0888 0.1581 0.145 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
O1W Cr1 1.966(9) . ?
O2W Cr1 2.006(10) . ?
Cr1 O1W 1.966(9) 2_665 ?
Cr1 O1W 1.966(9) 3_565 ?
Cr1 O2W 2.006(10) 3_565 ?
Cr1 O2W 2.006(10) 2_665 ?
Co1 N2 1.952(11) . ?
Co1 N1 1.983(11) . ?
Co1 N3 1.990(11) . ?
Co1 S3 2.229(4) . ?
Co1 S2 2.230(4) . ?
Co1 S1 2.263(4) . ?
Co2 N5 1.902(13) . ?
Co2 N6 1.973(13) . ?
Co2 N4 2.011(11) . ?
Co2 S6 2.237(4) . ?
Co2 S4 2.242(5) . ?
Co2 S5 2.261(5) . ?
Cu1 S4 2.125(4) . ?
Cu1 S1 2.151(4) . ?
Cu1 Cu3 2.664(3) . ?
Cu1 Cu2 2.666(3) . ?
Cu2 S5 2.143(4) . ?
Cu2 S2 2.152(4) . ?
Cu2 Cu3 2.641(3) . ?
Cu3 S6 2.132(4) . ?
Cu3 S3 2.162(4) . ?
S1 C1 1.858(13) . ?
C1 C5 1.511(14) . ?
C1 C4 1.526(14) . ?
C1 C2 1.568(15) . ?
C2 N1 1.419(13) . ?
C2 C3 1.556(15) . ?
C3 O1 1.214(13) . ?
C3 O2 1.266(14) . ?
S2 C6 1.864(12) . ?
C6 C9 1.493(14) . ?
C6 C10 1.514(14) . ?
C6 C7 1.553(14) . ?
C7 N2 1.445(13) . ?
C7 C8 1.564(15) . ?
C8 O3 1.179(14) . ?
C8 O4 1.261(14) . ?
S3 C11 1.851(13) . ?
C11 C15 1.508(14) . ?
C11 C14 1.511(14) . ?
C11 C12 1.558(15) . ?
C12 N3 1.438(13) . ?
C12 C13 1.546(16) . ?
C13 O5 1.198(15) . ?
C13 O6 1.244(14) . ?
S4 C16 1.841(12) . ?
C16 C19 1.444(14) . ?
C16 C20 1.512(14) . ?
C16 C17 1.536(15) . ?
C17 N4 1.433(14) . ?
C17 C18 1.545(17) . ?
C18 O7 1.191(16) . ?
C18 O8 1.240(16) . ?
S5 C21 1.853(14) . ?
C21 C25 1.485(15) . ?
C21 C24 1.486(14) . ?
C21 C22 1.566(15) . ?
C22 N5 1.435(13) . ?
C22 C23 1.577(16) . ?
C23 O9 1.193(14) . ?
C23 O10 1.224(14) . ?
S6 C26 1.846(13) . ?
C26 C30 1.495(14) . ?
C26 C29 1.497(14) . ?
C26 C27 1.566(15) . ?
C27 N6 1.432(14) . ?
C27 C28 1.561(17) . ?
C28 O11 1.182(16) . ?
C28 O12 1.263(18) . ?

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
O1W Cr1 O1W 90.4(4) 2_665 . ?
O1W Cr1 O1W 90.4(4) 2_665 3_565 ?
O1W Cr1 O1W 90.4(4) . 3_565 ?
O1W Cr1 O2W 175.8(4) 2_665 3_565 ?
O1W Cr1 O2W 92.8(4) . 3_565 ?
O1W Cr1 O2W 86.9(4) 3_565 3_565 ?
O1W Cr1 O2W 86.9(4) 2_665 2_665 ?
O1W Cr1 O2W 175.8(4) . 2_665 ?
O1W Cr1 O2W 92.8(4) 3_565 2_665 ?
O2W Cr1 O2W 90.0(4) 3_565 2_665 ?
O1W Cr1 O2W 92.8(4) 2_665 . ?
O1W Cr1 O2W 86.9(4) . . ?
O1W Cr1 O2W 175.8(4) 3_565 . ?
O2W Cr1 O2W 90.0(4) 3_565 . ?
O2W Cr1 O2W 90.0(4) 2_665 . ?
N2 Co1 N1 92.2(4) . . ?
N2 Co1 N3 91.7(5) . . ?
N1 Co1 N3 90.5(5) . . ?
N2 Co1 S3 173.9(3) . . ?
N1 Co1 S3 92.7(3) . . ?
N3 Co1 S3 84.7(3) . . ?
N2 Co1 S2 84.1(3) . . ?
N1 Co1 S2 174.7(3) . . ?
N3 Co1 S2 93.4(4) . . ?
S3 Co1 S2 91.26(16) . . ?
N2 Co1 S1 90.4(3) . . ?
N1 Co1 S1 84.1(3) . . ?
N3 Co1 S1 174.3(4) . . ?
S3 Co1 S1 93.71(16) . . ?
S2 Co1 S1 92.16(15) . . ?
N5 Co2 N6 89.7(5) . . ?
N5 Co2 N4 91.2(5) . . ?
N6 Co2 N4 89.5(5) . . ?
N5 Co2 S6 91.3(4) . . ?
N6 Co2 S6 86.0(4) . . ?
N4 Co2 S6 174.9(4) . . ?
N5 Co2 S4 175.1(4) . . ?
N6 Co2 S4 93.6(4) . . ?
N4 Co2 S4 85.2(4) . . ?
S6 Co2 S4 92.52(16) . . ?
N5 Co2 S5 84.0(4) . . ?
N6 Co2 S5 173.2(4) . . ?
N4 Co2 S5 93.2(4) . . ?
S6 Co2 S5 91.51(16) . . ?
S4 Co2 S5 92.81(17) . . ?
S4 Cu1 S1 176.49(19) . . ?
S4 Cu1 Cu3 75.84(13) . . ?
S1 Cu1 Cu3 107.50(13) . . ?
S4 Cu1 Cu2 105.70(14) . . ?
S1 Cu1 Cu2 77.22(12) . . ?
Cu3 Cu1 Cu2 59.42(7) . . ?
S5 Cu2 S2 179.5(2) . . ?
S5 Cu2 Cu3 102.10(14) . . ?
S2 Cu2 Cu3 78.35(12) . . ?
S5 Cu2 Cu1 76.97(14) . . ?
S2 Cu2 Cu1 103.11(13) . . ?
Cu3 Cu2 Cu1 60.25(7) . . ?
S6 Cu3 S3 176.91(19) . . ?
S6 Cu3 Cu2 80.46(13) . . ?
S3 Cu3 Cu2 102.47(14) . . ?
S6 Cu3 Cu1 106.21(13) . . ?
S3 Cu3 Cu1 74.68(13) . . ?
Cu2 Cu3 Cu1 60.33(7) . . ?
C1 S1 Cu1 105.1(4) . . ?
C1 S1 Co1 101.9(4) . . ?
Cu1 S1 Co1 102.18(17) . . ?
C5 C1 C4 111.2(12) . . ?
C5 C1 C2 111.6(11) . . ?
C4 C1 C2 111.5(11) . . ?
C5 C1 S1 115.0(9) . . ?
C4 C1 S1 107.4(9) . . ?
C2 C1 S1 99.7(8) . . ?
N1 C2 C3 113.6(11) . . ?
N1 C2 C1 109.8(10) . . ?
C3 C2 C1 109.6(11) . . ?
C2 N1 Co1 112.3(8) . . ?
O1 C3 O2 125.5(13) . . ?
O1 C3 C2 120.0(14) . . ?
O2 C3 C2 114.5(13) . . ?
C6 S2 Cu2 107.3(5) . . ?
C6 S2 Co1 103.2(5) . . ?
Cu2 S2 Co1 105.35(18) . . ?
C9 C6 C10 111.5(12) . . ?
C9 C6 C7 110.7(11) . . ?
C10 C6 C7 113.2(11) . . ?
C9 C6 S2 113.0(9) . . ?
C10 C6 S2 106.4(9) . . ?
C7 C6 S2 101.6(8) . . ?
N2 C7 C6 110.1(10) . . ?
N2 C7 C8 112.3(11) . . ?
C6 C7 C8 112.2(10) . . ?
C7 N2 Co1 115.9(8) . . ?
O3 C8 O4 125.8(15) . . ?
O3 C8 C7 117.7(14) . . ?
O4 C8 C7 116.4(14) . . ?
C11 S3 Cu3 104.9(5) . . ?
C11 S3 Co1 102.0(5) . . ?
Cu3 S3 Co1 107.36(19) . . ?
C15 C11 C14 108.7(12) . . ?
C15 C11 C12 113.4(11) . . ?
C14 C11 C12 109.8(12) . . ?
C15 C11 S3 108.7(10) . . ?
C14 C11 S3 113.9(9) . . ?
C12 C11 S3 102.4(9) . . ?
N3 C12 C13 111.5(11) . . ?
N3 C12 C11 109.3(11) . . ?
C13 C12 C11 113.2(12) . . ?
C12 N3 Co1 115.2(8) . . ?
O5 C13 O6 123.4(16) . . ?
O5 C13 C12 120.2(14) . . ?
O6 C13 C12 116.3(15) . . ?
C16 S4 Cu1 105.8(5) . . ?
C16 S4 Co2 101.6(5) . . ?
Cu1 S4 Co2 105.54(19) . . ?
C19 C16 C20 113.5(13) . . ?
C19 C16 C17 112.1(12) . . ?
C20 C16 C17 109.6(12) . . ?
C19 C16 S4 107.5(10) . . ?
C20 C16 S4 109.2(9) . . ?
C17 C16 S4 104.6(8) . . ?
N4 C17 C16 111.3(10) . . ?
N4 C17 C18 113.8(13) . . ?
C16 C17 C18 113.6(12) . . ?
C17 N4 Co2 113.5(8) . . ?
O7 C18 O8 127.7(18) . . ?
O7 C18 C17 117.3(17) . . ?
O8 C18 C17 114.7(16) . . ?
C21 S5 Cu2 106.5(5) . . ?
C21 S5 Co2 101.7(5) . . ?
Cu2 S5 Co2 107.26(18) . . ?
C25 C21 C24 115.0(13) . . ?
C25 C21 C22 111.5(12) . . ?
C24 C21 C22 110.1(12) . . ?
C25 C21 S5 110.1(11) . . ?
C24 C21 S5 107.0(11) . . ?
C22 C21 S5 102.3(9) . . ?
N5 C22 C21 109.0(11) . . ?
N5 C22 C23 110.2(12) . . ?
C21 C22 C23 111.7(12) . . ?
C22 N5 Co2 119.1(9) . . ?
O9 C23 O10 126.9(16) . . ?
O9 C23 C22 118.2(15) . . ?
O10 C23 C22 114.9(14) . . ?
C26 S6 Cu3 107.7(5) . . ?
C26 S6 Co2 102.5(4) . . ?
Cu3 S6 Co2 103.59(18) . . ?
C30 C26 C29 113.1(11) . . ?
C30 C26 C27 109.9(12) . . ?
C29 C26 C27 113.6(12) . . ?
C30 C26 S6 112.2(10) . . ?
C29 C26 S6 105.1(10) . . ?
C27 C26 S6 102.4(8) . . ?
N6 C27 C28 110.7(12) . . ?
N6 C27 C26 113.7(11) . . ?
C28 C27 C26 112.6(11) . . ?
C27 N6 Co2 114.4(9) . . ?
O11 C28 O12 126.9(19) . . ?
O11 C28 C27 116.5(18) . . ?
O12 C28 C27 116.3(16) . . ?

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
Cu1 S1 C1 C5 -17.2(11) . . . . ?
Co1 S1 C1 C5 89.0(10) . . . . ?
Cu1 S1 C1 C4 107.1(9) . . . . ?
Co1 S1 C1 C4 -146.7(8) . . . . ?
Cu1 S1 C1 C2 -136.6(7) . . . . ?
Co1 S1 C1 C2 -30.4(8) . . . . ?
C5 C1 C2 N1 -64.0(14) . . . . ?
C4 C1 C2 N1 171.1(11) . . . . ?
S1 C1 C2 N1 57.9(11) . . . . ?
C5 C1 C2 C3 61.4(14) . . . . ?
C4 C1 C2 C3 -63.5(15) . . . . ?
S1 C1 C2 C3 -176.7(10) . . . . ?
C3 C2 N1 Co1 175.0(9) . . . . ?
C1 C2 N1 Co1 -61.8(12) . . . . ?
N1 C2 C3 O1 -143.7(14) . . . . ?
C1 C2 C3 O1 93.0(16) . . . . ?
N1 C2 C3 O2 36.9(17) . . . . ?
C1 C2 C3 O2 -86.3(14) . . . . ?
Cu2 S2 C6 C9 -19.7(11) . . . . ?
Co1 S2 C6 C9 91.3(9) . . . . ?
Cu2 S2 C6 C10 103.0(9) . . . . ?
Co1 S2 C6 C10 -146.1(9) . . . . ?
Cu2 S2 C6 C7 -138.3(8) . . . . ?
Co1 S2 C6 C7 -27.4(9) . . . . ?
C9 C6 C7 N2 -69.9(14) . . . . ?
C10 C6 C7 N2 164.1(12) . . . . ?
S2 C6 C7 N2 50.4(13) . . . . ?
C9 C6 C7 C8 56.0(15) . . . . ?
C10 C6 C7 C8 -70.0(15) . . . . ?
S2 C6 C7 C8 176.2(10) . . . . ?
C6 C7 N2 Co1 -55.6(13) . . . . ?
C8 C7 N2 Co1 178.6(9) . . . . ?
N2 C7 C8 O3 27.8(19) . . . . ?
C6 C7 C8 O3 -96.9(16) . . . . ?
N2 C7 C8 O4 -154.1(13) . . . . ?
C6 C7 C8 O4 81.2(17) . . . . ?
Cu3 S3 C11 C15 95.8(10) . . . . ?
Co1 S3 C11 C15 -152.3(10) . . . . ?
Cu3 S3 C11 C14 -25.5(11) . . . . ?
Co1 S3 C11 C14 86.4(10) . . . . ?
Cu3 S3 C11 C12 -143.9(8) . . . . ?
Co1 S3 C11 C12 -32.1(9) . . . . ?
C15 C11 C12 N3 170.5(13) . . . . ?
C14 C11 C12 N3 -67.7(15) . . . . ?
S3 C11 C12 N3 53.6(13) . . . . ?
C15 C11 C12 C13 -64.5(17) . . . . ?
C14 C11 C12 C13 57.2(16) . . . . ?
S3 C11 C12 C13 178.6(11) . . . . ?
C13 C12 N3 Co1 -179.7(10) . . . . ?
C11 C12 N3 Co1 -53.8(15) . . . . ?
N3 C12 C13 O5 20(2) . . . . ?
C11 C12 C13 O5 -103.3(19) . . . . ?
N3 C12 C13 O6 -163.4(16) . . . . ?
C11 C12 C13 O6 73(2) . . . . ?
Cu1 S4 C16 C19 103.4(11) . . . . ?
Co2 S4 C16 C19 -146.6(11) . . . . ?
Cu1 S4 C16 C20 -20.0(11) . . . . ?
Co2 S4 C16 C20 90.0(10) . . . . ?
Cu1 S4 C16 C17 -137.2(8) . . . . ?
Co2 S4 C16 C17 -27.2(9) . . . . ?
C19 C16 C17 N4 167.1(13) . . . . ?
C20 C16 C17 N4 -66.0(14) . . . . ?
S4 C16 C17 N4 51.0(13) . . . . ?
C19 C16 C17 C18 -62.9(17) . . . . ?
C20 C16 C17 C18 64.0(16) . . . . ?
S4 C16 C17 C18 -179.1(11) . . . . ?
C16 C17 N4 Co2 -52.9(14) . . . . ?
C18 C17 N4 Co2 177.2(11) . . . . ?
N4 C17 C18 O7 39(3) . . . . ?
C16 C17 C18 O7 -89(2) . . . . ?
N4 C17 C18 O8 -145.5(19) . . . . ?
C16 C17 C18 O8 86(2) . . . . ?
Cu2 S5 C21 C25 -22.8(11) . . . . ?
Co2 S5 C21 C25 89.4(10) . . . . ?
Cu2 S5 C21 C24 102.8(10) . . . . ?
Co2 S5 C21 C24 -145.0(9) . . . . ?
Cu2 S5 C21 C22 -141.5(8) . . . . ?
Co2 S5 C21 C22 -29.3(9) . . . . ?
C25 C21 C22 N5 -68.1(16) . . . . ?
C24 C21 C22 N5 163.0(13) . . . . ?
S5 C21 C22 N5 49.5(13) . . . . ?
C25 C21 C22 C23 53.8(16) . . . . ?
C24 C21 C22 C23 -75.1(16) . . . . ?
S5 C21 C22 C23 171.5(10) . . . . ?
C21 C22 N5 Co2 -53.1(15) . . . . ?
C23 C22 N5 Co2 -176.0(10) . . . . ?
N5 C22 C23 O9 17(2) . . . . ?
C21 C22 C23 O9 -104.6(18) . . . . ?
N5 C22 C23 O10 -163.2(15) . . . . ?
C21 C22 C23 O10 75.5(18) . . . . ?
Cu3 S6 C26 C30 -18.4(10) . . . . ?
Co2 S6 C26 C30 90.5(9) . . . . ?
Cu3 S6 C26 C29 104.9(9) . . . . ?
Co2 S6 C26 C29 -146.2(9) . . . . ?
Cu3 S6 C26 C27 -136.2(8) . . . . ?
Co2 S6 C26 C27 -27.3(10) . . . . ?
C30 C26 C27 N6 -70.5(15) . . . . ?
C29 C26 C27 N6 161.6(13) . . . . ?
S6 C26 C27 N6 48.9(15) . . . . ?
C30 C26 C27 C28 56.3(16) . . . . ?
C29 C26 C27 C28 -71.6(17) . . . . ?
S6 C26 C27 C28 175.7(12) . . . . ?
C28 C27 N6 Co2 -177.3(11) . . . . ?
C26 C27 N6 Co2 -49.5(16) . . . . ?
N6 C27 C28 O11 -146.7(17) . . . . ?
C26 C27 C28 O11 85(2) . . . . ?
N6 C27 C28 O12 28(3) . . . . ?
C26 C27 C28 O12 -100(2) . . . . ?

_refine_diff_density_max         0.583
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.069

_shelxl_version_number           2014-3




