# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_160523d
_database_code_depnum_ccdc_archive 'CCDC 1482297'
_audit_update_record             
;
2016-05-27 deposited with the CCDC.
2017-07-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H48 Co3 N12 O24 S3'
_chemical_formula_weight         1233.77

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Rhombohedral
_symmetry_space_group_name_H-M   R3c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'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'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'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'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'

_cell_length_a                   23.635(2)
_cell_length_b                   23.635(2)
_cell_length_c                   13.7616(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     6657.4(11)
_cell_formula_units_Z            6
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    5413
_cell_measurement_theta_min      2.986
_cell_measurement_theta_max      27.955

_exptl_crystal_description       block-like
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      0
_exptl_crystal_density_diffrn    1.846
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3798
_exptl_absorpt_coefficient_mu    1.353
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6136
_exptl_absorpt_correction_T_max  0.7735
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10773
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.99
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2432
_reflns_number_gt                2226
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0283P)²+29.8552P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_number_reflns         2432
_refine_ls_number_parameters     218
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0308
_refine_ls_wR_factor_ref         0.0724
_refine_ls_wR_factor_gt          0.0685
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.10724(2) 0.33281(3) 0.98865(5) 0.01908(13) Uani 1 1 d . . .
S1 S 0.23094(5) 0.22379(5) 0.19213(7) 0.0211(2) Uani 1 1 d . . .
N1 N 0.21881(17) 0.54440(17) 0.9605(3) 0.0212(8) Uani 1 1 d . . .
N2 N 0.15269(17) 0.43772(17) 0.9744(3) 0.0228(8) Uani 1 1 d . . .
N3 N 0.00987(17) 0.12335(17) 1.0355(3) 0.0198(8) Uani 1 1 d . . .
N4 N 0.05043(18) 0.22985(18) 1.0184(3) 0.0245(9) Uani 1 1 d . . .
O1 O 0.24233(17) 0.29089(15) 0.1798(3) 0.0358(8) Uani 1 1 d . . .
O2 O 0.16709(16) 0.17564(17) 0.1577(4) 0.0515(9) Uani 1 1 d . . .
O3 O 0.23699(18) 0.21336(15) 0.2968(2) 0.0412(8) Uani 1 1 d . . .
O4 O 0.28116(19) 0.2172(2) 0.1389(3) 0.0504(10) Uani 1 1 d . . .
O5 O 0.07203(16) 0.34820(16) 1.1195(2) 0.0395(8) Uani 1 1 d . . .
H5C H 0.0974 0.3642 1.1680 0.047 Uiso 1 1 d R . .
H5D H 0.0331 0.3323 1.1399 0.047 Uiso 1 1 d R . .
O6 O 0.19230(14) 0.34138(17) 1.0451(3) 0.0469(10) Uani 1 1 d . . .
H6C H 0.2037 0.3232 1.0880 0.056 Uiso 1 1 d R . .
H6D H 0.2265 0.3697 1.0158 0.056 Uiso 1 1 d R . .
O7 O 0.13895(14) 0.32194(16) 0.8503(2) 0.0357(7) Uani 1 1 d . . .
H7C H 0.1153 0.3142 0.8000 0.043 Uiso 1 1 d R . .
H7D H 0.1788 0.3416 0.8330 0.043 Uiso 1 1 d R . .
O8 O 0.02340(13) 0.32020(13) 0.9110(2) 0.0252(6) Uani 1 1 d . . .
H8C H -0.0096 0.3128 0.9451 0.030 Uiso 1 1 d R . .
H8D H 0.0121 0.2881 0.8726 0.030 Uiso 1 1 d R . .
C1 C 0.2142(2) 0.4852(2) 0.9745(3) 0.0235(10) Uani 1 1 d . . .
H1 H 0.2497 0.4790 0.9830 0.028 Uiso 1 1 calc R . .
C2 C 0.1167(2) 0.4678(2) 0.9611(4) 0.0333(12) Uani 1 1 d . . .
H2 H 0.0713 0.4462 0.9589 0.040 Uiso 1 1 calc R . .
C3 C 0.1553(2) 0.5322(2) 0.9516(4) 0.0312(11) Uani 1 1 d . . .
H3 H 0.1422 0.5628 0.9411 0.037 Uiso 1 1 calc R . .
C4 C 0.2773(2) 0.60670(19) 0.9575(3) 0.0165(9) Uani 1 1 d . . .
C5 C 0.3376(2) 0.6100(2) 0.9564(3) 0.0204(9) Uani 1 1 d . . .
H5 H 0.3404 0.5721 0.9550 0.025 Uiso 1 1 calc R . .
C6 C 0.0629(2) 0.1820(2) 1.0123(3) 0.0222(10) Uani 1 1 d . . .
H6 H 0.1031 0.1873 0.9941 0.027 Uiso 1 1 calc R . .
C7 C -0.0147(2) 0.2003(2) 1.0479(4) 0.0294(11) Uani 1 1 d . . .
H7 H -0.0374 0.2225 1.0586 0.035 Uiso 1 1 calc R . .
C8 C -0.0402(2) 0.1360(2) 1.0586(3) 0.0255(10) Uani 1 1 d . . .
H8 H -0.0826 0.1059 1.0775 0.031 Uiso 1 1 calc R . .
C9 C 0.0049(2) 0.06059(19) 1.0358(3) 0.0182(9) Uani 1 1 d . . .
C10 C 0.0617(2) 0.0567(2) 1.0351(3) 0.0204(10) Uani 1 1 d . . .
H10 H 0.1026 0.0943 1.0342 0.025 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
Co1 O6 2.068(3) . ?
Co1 O5 2.090(3) . ?
Co1 O7 2.108(3) . ?
Co1 O8 2.137(3) . ?
Co1 N4 2.151(4) . ?
Co1 N2 2.163(4) . ?
S1 O2 1.442(3) . ?
S1 O4 1.468(4) . ?
S1 O1 1.480(3) . ?
S1 O3 1.480(4) . ?
N1 C1 1.361(5) . ?
N1 C3 1.385(6) . ?
N1 C4 1.430(5) . ?
N2 C1 1.319(5) . ?
N2 C2 1.367(6) . ?
N3 C6 1.362(5) . ?
N3 C8 1.395(5) . ?
N3 C9 1.429(5) . ?
N4 C6 1.305(6) . ?
N4 C7 1.396(6) . ?
O5 H5C 0.8501 . ?
O5 H5D 0.8500 . ?
O6 H6C 0.8501 . ?
O6 H6D 0.8501 . ?
O7 H7C 0.8500 . ?
O7 H7D 0.8501 . ?
O8 H8C 0.8500 . ?
O8 H8D 0.8500 . ?
C1 H1 0.9300 . ?
C2 C3 1.333(6) . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 C5 1.378(6) 3_565 ?
C4 C5 1.388(6) . ?
C5 C4 1.378(6) 2_665 ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.334(6) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 C10 1.389(6) . ?
C9 C10 1.391(6) 2 ?
C10 C9 1.391(6) 3 ?
C10 H10 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
O6 Co1 O5 96.40(15) . . ?
O6 Co1 O7 87.93(13) . . ?
O5 Co1 O7 174.70(14) . . ?
O6 Co1 O8 171.67(14) . . ?
O5 Co1 O8 91.89(13) . . ?
O7 Co1 O8 83.83(12) . . ?
O6 Co1 N4 93.76(14) . . ?
O5 Co1 N4 87.43(14) . . ?
O7 Co1 N4 95.34(14) . . ?
O8 Co1 N4 85.80(13) . . ?
O6 Co1 N2 91.17(14) . . ?
O5 Co1 N2 83.74(14) . . ?
O7 Co1 N2 93.15(14) . . ?
O8 Co1 N2 90.51(13) . . ?
N4 Co1 N2 170.32(14) . . ?
O2 S1 O4 109.6(3) . . ?
O2 S1 O1 111.5(2) . . ?
O4 S1 O1 109.5(2) . . ?
O2 S1 O3 109.8(2) . . ?
O4 S1 O3 108.5(2) . . ?
O1 S1 O3 107.99(19) . . ?
C1 N1 C3 106.0(4) . . ?
C1 N1 C4 127.0(3) . . ?
C3 N1 C4 127.0(3) . . ?
C1 N2 C2 105.4(4) . . ?
C1 N2 Co1 132.8(3) . . ?
C2 N2 Co1 121.8(3) . . ?
C6 N3 C8 106.4(4) . . ?
C6 N3 C9 127.8(4) . . ?
C8 N3 C9 125.8(4) . . ?
C6 N4 C7 104.8(4) . . ?
C6 N4 Co1 133.2(3) . . ?
C7 N4 Co1 122.0(3) . . ?
Co1 O5 H5C 120.0 . . ?
Co1 O5 H5D 130.2 . . ?
H5C O5 H5D 107.7 . . ?
Co1 O6 H6C 138.6 . . ?
Co1 O6 H6D 113.1 . . ?
H6C O6 H6D 108.2 . . ?
Co1 O7 H7C 121.8 . . ?
Co1 O7 H7D 123.4 . . ?
H7C O7 H7D 108.5 . . ?
Co1 O8 H8C 116.3 . . ?
Co1 O8 H8D 106.9 . . ?
H8C O8 H8D 108.2 . . ?
N2 C1 N1 111.3(4) . . ?
N2 C1 H1 124.4 . . ?
N1 C1 H1 124.4 . . ?
C3 C2 N2 110.9(4) . . ?
C3 C2 H2 124.5 . . ?
N2 C2 H2 124.5 . . ?
C2 C3 N1 106.4(4) . . ?
C2 C3 H3 126.8 . . ?
N1 C3 H3 126.8 . . ?
C5 C4 C5 121.4(4) 3_565 . ?
C5 C4 N1 119.0(4) 3_565 . ?
C5 C4 N1 119.7(4) . . ?
C4 C5 C4 118.6(4) 2_665 . ?
C4 C5 H5 120.7 2_665 . ?
C4 C5 H5 120.7 . . ?
N4 C6 N3 112.1(4) . . ?
N4 C6 H6 124.0 . . ?
N3 C6 H6 124.0 . . ?
C8 C7 N4 111.0(4) . . ?
C8 C7 H7 124.5 . . ?
N4 C7 H7 124.5 . . ?
C7 C8 N3 105.7(4) . . ?
C7 C8 H8 127.1 . . ?
N3 C8 H8 127.1 . . ?
C10 C9 C10 121.8(4) . 2 ?
C10 C9 N3 119.3(4) . . ?
C10 C9 N3 119.0(4) 2 . ?
C9 C10 C9 118.2(4) . 3 ?
C9 C10 H10 120.9 . . ?
C9 C10 H10 120.9 3 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O6 Co1 N2 C1 17.2(5) . . . . ?
O5 Co1 N2 C1 113.5(5) . . . . ?
O7 Co1 N2 C1 -70.8(5) . . . . ?
O8 Co1 N2 C1 -154.7(5) . . . . ?
N4 Co1 N2 C1 137.8(8) . . . . ?
O6 Co1 N2 C2 -163.8(4) . . . . ?
O5 Co1 N2 C2 -67.5(4) . . . . ?
O7 Co1 N2 C2 108.2(4) . . . . ?
O8 Co1 N2 C2 24.3(4) . . . . ?
N4 Co1 N2 C2 -43.1(12) . . . . ?
O6 Co1 N4 C6 -39.2(4) . . . . ?
O5 Co1 N4 C6 -135.4(4) . . . . ?
O7 Co1 N4 C6 49.1(4) . . . . ?
O8 Co1 N4 C6 132.5(4) . . . . ?
N2 Co1 N4 C6 -159.7(8) . . . . ?
O6 Co1 N4 C7 143.5(4) . . . . ?
O5 Co1 N4 C7 47.3(4) . . . . ?
O7 Co1 N4 C7 -128.2(4) . . . . ?
O8 Co1 N4 C7 -44.8(4) . . . . ?
N2 Co1 N4 C7 23.0(12) . . . . ?
C2 N2 C1 N1 -0.7(6) . . . . ?
Co1 N2 C1 N1 178.4(3) . . . . ?
C3 N1 C1 N2 0.2(5) . . . . ?
C4 N1 C1 N2 179.2(4) . . . . ?
C1 N2 C2 C3 1.0(6) . . . . ?
Co1 N2 C2 C3 -178.3(3) . . . . ?
N2 C2 C3 N1 -0.8(6) . . . . ?
C1 N1 C3 C2 0.4(5) . . . . ?
C4 N1 C3 C2 -178.5(4) . . . . ?
C1 N1 C4 C5 -170.9(4) . . . 3_565 ?
C3 N1 C4 C5 7.8(7) . . . 3_565 ?
C1 N1 C4 C5 8.7(7) . . . . ?
C3 N1 C4 C5 -172.6(4) . . . . ?
C5 C4 C5 C4 2.2(9) 3_565 . . 2_665 ?
N1 C4 C5 C4 -177.4(3) . . . 2_665 ?
C7 N4 C6 N3 0.2(5) . . . . ?
Co1 N4 C6 N3 -177.4(3) . . . . ?
C8 N3 C6 N4 -0.2(5) . . . . ?
C9 N3 C6 N4 179.2(4) . . . . ?
C6 N4 C7 C8 -0.2(6) . . . . ?
Co1 N4 C7 C8 177.8(3) . . . . ?
N4 C7 C8 N3 0.0(6) . . . . ?
C6 N3 C8 C7 0.1(5) . . . . ?
C9 N3 C8 C7 -179.3(4) . . . . ?
C6 N3 C9 C10 16.6(7) . . . . ?
C8 N3 C9 C10 -164.1(4) . . . . ?
C6 N3 C9 C10 -162.3(4) . . . 2 ?
C8 N3 C9 C10 17.0(6) . . . 2 ?
C10 C9 C10 C9 -1.4(9) 2 . . 3 ?
N3 C9 C10 C9 179.8(3) . . . 3 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.058
