# 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 
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data_1-2CH2CL2-120K
_database_code_depnum_ccdc_archive 'CCDC 1865577'
_audit_update_record             
;
2018-09-03 deposited with the CCDC.
2018-11-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C40 H32 Co3 F2 N12, 2(C H2 Cl2)'
_chemical_formula_sum            'C42 H36 Cl4 Co3 F2 N12'
_chemical_formula_weight         1065.42

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'
Cl Cl 0.1484 0.1585 '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'
F F 0.0171 0.0103 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

_cell_length_a                   20.3854(6)
_cell_length_b                   13.8382(6)
_cell_length_c                   17.0652(7)
_cell_angle_alpha                90
_cell_angle_beta                 118.457(3)
_cell_angle_gamma                90
_cell_volume                     4232.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9199
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      26.26

_exptl_crystal_description       needle
_exptl_crystal_colour            'dark reddish brown'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_F_000             2156
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    1.473
_shelx_estimated_absorpt_T_min   0.788
_shelx_estimated_absorpt_T_max   0.943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5413
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_process_details   'SADABS (Bruker, 2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            63362
_diffrn_reflns_av_unetI/netI     0.0155
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.957
_diffrn_reflns_theta_max         26.261
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4278
_reflns_number_gt                3603
_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       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_structure_solution    'SHELXS2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_publication_material  'SHELXL-2016/4 (Sheldrick, 2016)'
_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)+(0.0460P)²+12.4206P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_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_number_reflns         4278
_refine_ls_number_parameters     287
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0340
_refine_ls_wR_factor_ref         0.0968
_refine_ls_wR_factor_gt          0.0918
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_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
C1 C 0.64014(14) 0.94692(18) 0.27302(17) 0.0215(5) Uani 1 1 d . . . . .
H1 H 0.621194 1.005252 0.283817 0.026 Uiso 1 1 calc R U . . .
C1S C 0.40973(16) 0.20745(19) 0.1664(2) 0.0328(7) Uani 1 1 d . . . . .
H1SA H 0.435933 0.264852 0.202353 0.039 Uiso 1 1 calc R U . . .
H1SB H 0.436974 0.149144 0.199580 0.039 Uiso 1 1 calc R U . . .
C2 C 0.71005(14) 0.94840(19) 0.27927(18) 0.0267(6) Uani 1 1 d . . . . .
H2 H 0.737724 1.006768 0.291190 0.032 Uiso 1 1 calc R U . . .
C3 C 0.73886(14) 0.86159(19) 0.26754(18) 0.0256(6) Uani 1 1 d . . . . .
H3 H 0.787687 0.859436 0.273738 0.031 Uiso 1 1 calc R U . . .
C4 C 0.69642(14) 0.77923(19) 0.24701(17) 0.0232(5) Uani 1 1 d . . . . .
H4 H 0.716399 0.719591 0.240493 0.028 Uiso 1 1 calc R U . . .
C5 C 0.62283(14) 0.78280(16) 0.23548(16) 0.0178(5) Uani 1 1 d . . . . .
C6 C 0.57919(13) 0.62825(17) 0.16567(16) 0.0189(5) Uani 1 1 d . . . . .
C7 C 0.61085(14) 0.6296(2) 0.10778(17) 0.0247(6) Uani 1 1 d . . . . .
H7 H 0.631962 0.687671 0.099988 0.030 Uiso 1 1 calc R U . . .
C8 C 0.61125(14) 0.5481(2) 0.06303(17) 0.0297(6) Uani 1 1 d . . . . .
H8 H 0.633258 0.548953 0.024923 0.036 Uiso 1 1 calc R U . . .
C9 C 0.57934(15) 0.4639(2) 0.07350(18) 0.0304(6) Uani 1 1 d . . . . .
H9 H 0.580370 0.405924 0.044258 0.036 Uiso 1 1 calc R U . . .
C10 C 0.54621(14) 0.46638(19) 0.12722(17) 0.0246(6) Uani 1 1 d . . . . .
H10 H 0.522772 0.409463 0.132931 0.029 Uiso 1 1 calc R U . . .
C11 C 0.44964(13) 0.94650(18) 0.07298(17) 0.0205(5) Uani 1 1 d . . . . .
H11 H 0.473534 1.003243 0.105346 0.025 Uiso 1 1 calc R U . . .
C12 C 0.58384(14) 0.94954(19) 0.51873(17) 0.0247(6) Uani 1 1 d . . . . .
H12 H 0.584378 1.007294 0.549125 0.030 Uiso 1 1 calc R U . . .
C13 C 0.61677(15) 0.8654(2) 0.56523(18) 0.0264(6) Uani 1 1 d . . . . .
H13 H 0.639333 0.864541 0.628446 0.032 Uiso 1 1 calc R U . . .
C14 C 0.61668(14) 0.78352(18) 0.51974(17) 0.0220(5) Uani 1 1 d . . . . .
H14 H 0.639213 0.726029 0.551690 0.026 Uiso 1 1 calc R U . . .
C15 C 0.58331(13) 0.78419(16) 0.42573(16) 0.0173(5) Uani 1 1 d . . . . .
C16 C 0.62580(13) 0.62943(16) 0.40123(16) 0.0168(5) Uani 1 1 d . . . . .
C17 C 0.70012(14) 0.63115(18) 0.47210(17) 0.0208(5) Uani 1 1 d . . . . .
H17 H 0.718206 0.686756 0.508953 0.025 Uiso 1 1 calc R U . . .
C18 C 0.74593(13) 0.55295(19) 0.48764(17) 0.0234(5) Uani 1 1 d . . . . .
H18 H 0.795802 0.554774 0.534827 0.028 Uiso 1 1 calc R U . . .
C19 C 0.71968(14) 0.47107(18) 0.43463(17) 0.0232(5) Uani 1 1 d . . . . .
H19 H 0.750800 0.416374 0.444348 0.028 Uiso 1 1 calc R U . . .
C20 C 0.64686(13) 0.47208(17) 0.36743(17) 0.0201(5) Uani 1 1 d . . . . .
H20 H 0.628370 0.416460 0.330692 0.024 Uiso 1 1 calc R U . . .
Cl1 Cl 0.31712(5) 0.20441(6) 0.15079(8) 0.0579(3) Uani 1 1 d . . . . .
Cl2 Cl 0.40975(9) 0.21197(7) 0.06419(8) 0.0768(4) Uani 1 1 d . . . . .
Co1 Co 0.500000 0.87470(3) 0.250000 0.01340(12) Uani 1 2 d S T P . .
Co2 Co 0.500000 0.70663(3) 0.250000 0.01293(12) Uani 1 2 d S T P . .
Co3 Co 0.500000 0.53929(3) 0.250000 0.01475(12) Uani 1 2 d S T P . .
F1 F 0.500000 1.01985(13) 0.250000 0.0206(4) Uani 1 2 d S T P . .
F2 F 0.500000 0.39442(14) 0.250000 0.0253(5) Uani 1 2 d S T P . .
N1 N 0.59710(11) 0.86695(14) 0.25237(13) 0.0167(4) Uani 1 1 d . . . . .
N2 N 0.45024(11) 0.86683(14) 0.11932(13) 0.0165(4) Uani 1 1 d . . . . .
N3 N 0.57509(11) 0.70590(13) 0.21277(13) 0.0170(4) Uani 1 1 d . . . . .
N4 N 0.57701(11) 0.70613(13) 0.37306(13) 0.0165(4) Uani 1 1 d . . . . .
N5 N 0.54553(11) 0.54633(14) 0.17227(13) 0.0181(4) Uani 1 1 d . . . . .
N6 N 0.60033(11) 0.54778(13) 0.35092(13) 0.0161(4) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.350(3) . ?
C1 C2 1.378(4) . ?
C1 H1 0.9500 . ?
C1S Cl2 1.746(3) . ?
C1S Cl1 1.777(3) . ?
C1S H1SA 0.9900 . ?
C1S H1SB 0.9900 . ?
C2 C3 1.393(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.372(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.418(3) . ?
C4 H4 0.9500 . ?
C5 N1 1.363(3) . ?
C5 N3 1.368(3) . ?
C6 N5 1.357(3) . ?
C6 N3 1.368(3) . ?
C6 C7 1.414(3) . ?
C7 C8 1.365(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.386(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.374(4) . ?
C9 H9 0.9500 . ?
C10 N5 1.351(3) . ?
C10 H10 0.9500 . ?
C11 N2 1.353(3) . ?
C11 C12 1.378(4) 2_655 ?
C11 H11 0.9500 . ?
C12 C13 1.388(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.373(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.413(3) . ?
C14 H14 0.9500 . ?
C15 N2 1.366(3) 2_655 ?
C15 N4 1.372(3) . ?
C16 N6 1.363(3) . ?
C16 N4 1.375(3) . ?
C16 C17 1.419(3) . ?
C17 C18 1.370(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.388(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.377(3) . ?
C19 H19 0.9500 . ?
C20 N6 1.350(3) . ?
C20 H20 0.9500 . ?
Co1 N1 1.963(2) . ?
Co1 N1 1.963(2) 2_655 ?
Co1 N2 1.964(2) 2_655 ?
Co1 N2 1.964(2) . ?
Co1 F1 2.0086(19) . ?
Co1 Co2 2.3257(6) . ?
Co2 N3 1.917(2) 2_655 ?
Co2 N3 1.917(2) . ?
Co2 N4 1.932(2) . ?
Co2 N4 1.932(2) 2_655 ?
Co2 Co3 2.3158(6) . ?
Co3 N5 1.950(2) . ?
Co3 N5 1.950(2) 2_655 ?
Co3 N6 1.9509(19) 2_655 ?
Co3 N6 1.9509(19) . ?
Co3 F2 2.005(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 123.5(2) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
Cl2 C1S Cl1 110.92(17) . . ?
Cl2 C1S H1SA 109.5 . . ?
Cl1 C1S H1SA 109.5 . . ?
Cl2 C1S H1SB 109.5 . . ?
Cl1 C1S H1SB 109.5 . . ?
H1SA C1S H1SB 108.0 . . ?
C1 C2 C3 117.9(2) . . ?
C1 C2 H2 121.1 . . ?
C3 C2 H2 121.1 . . ?
C4 C3 C2 119.7(2) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C3 C4 C5 120.2(2) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
N1 C5 N3 115.5(2) . . ?
N1 C5 C4 119.3(2) . . ?
N3 C5 C4 125.1(2) . . ?
N5 C6 N3 115.6(2) . . ?
N5 C6 C7 119.1(2) . . ?
N3 C6 C7 125.1(2) . . ?
C8 C7 C6 120.4(3) . . ?
C8 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
C7 C8 C9 119.6(3) . . ?
C7 C8 H8 120.2 . . ?
C9 C8 H8 120.2 . . ?
C10 C9 C8 118.3(2) . . ?
C10 C9 H9 120.8 . . ?
C8 C9 H9 120.8 . . ?
N5 C10 C9 122.8(3) . . ?
N5 C10 H10 118.6 . . ?
C9 C10 H10 118.6 . . ?
N2 C11 C12 123.4(2) . 2_655 ?
N2 C11 H11 118.3 . . ?
C12 C11 H11 118.3 2_655 . ?
C11 C12 C13 117.8(2) 2_655 . ?
C11 C12 H12 121.1 2_655 . ?
C13 C12 H12 121.1 . . ?
C14 C13 C12 119.9(2) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C13 C14 C15 120.4(2) . . ?
C13 C14 H14 119.8 . . ?
C15 C14 H14 119.8 . . ?
N2 C15 N4 115.2(2) 2_655 . ?
N2 C15 C14 119.1(2) 2_655 . ?
N4 C15 C14 125.7(2) . . ?
N6 C16 N4 115.1(2) . . ?
N6 C16 C17 118.8(2) . . ?
N4 C16 C17 125.9(2) . . ?
C18 C17 C16 120.3(2) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
C17 C18 C19 120.2(2) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
C20 C19 C18 117.5(2) . . ?
C20 C19 H19 121.2 . . ?
C18 C19 H19 121.2 . . ?
N6 C20 C19 123.6(2) . . ?
N6 C20 H20 118.2 . . ?
C19 C20 H20 118.2 . . ?
N1 Co1 N1 173.74(11) . 2_655 ?
N1 Co1 N2 90.20(8) . 2_655 ?
N1 Co1 N2 89.45(8) 2_655 2_655 ?
N1 Co1 N2 89.45(8) . . ?
N1 Co1 N2 90.20(8) 2_655 . ?
N2 Co1 N2 173.65(11) 2_655 . ?
N1 Co1 F1 93.13(6) . . ?
N1 Co1 F1 93.13(6) 2_655 . ?
N2 Co1 F1 93.18(6) 2_655 . ?
N2 Co1 F1 93.18(6) . . ?
N1 Co1 Co2 86.87(6) . . ?
N1 Co1 Co2 86.87(6) 2_655 . ?
N2 Co1 Co2 86.82(6) 2_655 . ?
N2 Co1 Co2 86.82(6) . . ?
F1 Co1 Co2 180.0 . . ?
N3 Co2 N3 179.39(11) 2_655 . ?
N3 Co2 N4 90.19(8) 2_655 . ?
N3 Co2 N4 89.81(8) . . ?
N3 Co2 N4 89.81(8) 2_655 2_655 ?
N3 Co2 N4 90.19(8) . 2_655 ?
N4 Co2 N4 179.59(11) . 2_655 ?
N3 Co2 Co3 89.69(6) 2_655 . ?
N3 Co2 Co3 89.70(6) . . ?
N4 Co2 Co3 89.79(5) . . ?
N4 Co2 Co3 89.79(5) 2_655 . ?
N3 Co2 Co1 90.31(6) 2_655 . ?
N3 Co2 Co1 90.30(6) . . ?
N4 Co2 Co1 90.21(5) . . ?
N4 Co2 Co1 90.21(5) 2_655 . ?
Co3 Co2 Co1 180.0 . . ?
N5 Co3 N5 174.28(12) . 2_655 ?
N5 Co3 N6 92.01(8) . 2_655 ?
N5 Co3 N6 87.64(8) 2_655 2_655 ?
N5 Co3 N6 87.64(8) . . ?
N5 Co3 N6 92.01(8) 2_655 . ?
N6 Co3 N6 173.09(11) 2_655 . ?
N5 Co3 F2 92.86(6) . . ?
N5 Co3 F2 92.86(6) 2_655 . ?
N6 Co3 F2 93.45(6) 2_655 . ?
N6 Co3 F2 93.45(6) . . ?
N5 Co3 Co2 87.14(6) . . ?
N5 Co3 Co2 87.14(6) 2_655 . ?
N6 Co3 Co2 86.55(6) 2_655 . ?
N6 Co3 Co2 86.55(6) . . ?
F2 Co3 Co2 180.0 . . ?
C1 N1 C5 119.2(2) . . ?
C1 N1 Co1 118.93(16) . . ?
C5 N1 Co1 121.87(16) . . ?
C11 N2 C15 119.4(2) . 2_655 ?
C11 N2 Co1 118.31(16) . . ?
C15 N2 Co1 122.32(16) 2_655 . ?
C5 N3 C6 122.9(2) . . ?
C5 N3 Co2 118.34(16) . . ?
C6 N3 Co2 118.74(16) . . ?
C15 N4 C16 123.5(2) . . ?
C15 N4 Co2 118.90(15) . . ?
C16 N4 Co2 117.42(15) . . ?
C10 N5 C6 119.6(2) . . ?
C10 N5 Co3 118.90(18) . . ?
C6 N5 Co3 121.42(16) . . ?
C20 N6 C16 119.5(2) . . ?
C20 N6 Co3 118.32(16) . . ?
C16 N6 Co3 122.03(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
N1 C1 C2 C3 -3.0(4) . . . . ?
C1 C2 C3 C4 2.5(4) . . . . ?
C2 C3 C4 C5 1.6(4) . . . . ?
C3 C4 C5 N1 -5.5(4) . . . . ?
C3 C4 C5 N3 178.2(2) . . . . ?
N5 C6 C7 C8 -3.7(4) . . . . ?
N3 C6 C7 C8 -179.2(2) . . . . ?
C6 C7 C8 C9 1.0(4) . . . . ?
C7 C8 C9 C10 1.8(4) . . . . ?
C8 C9 C10 N5 -2.2(4) . . . . ?
C11 C12 C13 C14 1.5(4) 2_655 . . . ?
C12 C13 C14 C15 0.0(4) . . . . ?
C13 C14 C15 N2 -1.4(4) . . . 2_655 ?
C13 C14 C15 N4 -177.1(2) . . . . ?
N6 C16 C17 C18 2.0(3) . . . . ?
N4 C16 C17 C18 -172.9(2) . . . . ?
C16 C17 C18 C19 -0.6(4) . . . . ?
C17 C18 C19 C20 -0.3(4) . . . . ?
C18 C19 C20 N6 -0.1(4) . . . . ?
C2 C1 N1 C5 -0.9(4) . . . . ?
C2 C1 N1 Co1 177.9(2) . . . . ?
N3 C5 N1 C1 -178.3(2) . . . . ?
C4 C5 N1 C1 5.1(3) . . . . ?
N3 C5 N1 Co1 3.0(3) . . . . ?
C4 C5 N1 Co1 -173.63(17) . . . . ?
C12 C11 N2 C15 0.4(4) 2_655 . . 2_655 ?
C12 C11 N2 Co1 -179.67(19) 2_655 . . . ?
N1 C5 N3 C6 157.2(2) . . . . ?
C4 C5 N3 C6 -26.4(4) . . . . ?
N1 C5 N3 Co2 -23.6(3) . . . . ?
C4 C5 N3 Co2 152.8(2) . . . . ?
N5 C6 N3 C5 159.9(2) . . . . ?
C7 C6 N3 C5 -24.4(4) . . . . ?
N5 C6 N3 Co2 -19.3(3) . . . . ?
C7 C6 N3 Co2 156.4(2) . . . . ?
N2 C15 N4 C16 156.7(2) 2_655 . . . ?
C14 C15 N4 C16 -27.5(4) . . . . ?
N2 C15 N4 Co2 -18.8(3) 2_655 . . . ?
C14 C15 N4 Co2 157.0(2) . . . . ?
N6 C16 N4 C15 162.4(2) . . . . ?
C17 C16 N4 C15 -22.5(4) . . . . ?
N6 C16 N4 Co2 -22.0(3) . . . . ?
C17 C16 N4 Co2 153.1(2) . . . . ?
C9 C10 N5 C6 -0.5(4) . . . . ?
C9 C10 N5 Co3 -177.67(19) . . . . ?
N3 C6 N5 C10 179.3(2) . . . . ?
C7 C6 N5 C10 3.4(3) . . . . ?
N3 C6 N5 Co3 -3.6(3) . . . . ?
C7 C6 N5 Co3 -179.54(17) . . . . ?
C19 C20 N6 C16 1.5(4) . . . . ?
C19 C20 N6 Co3 177.58(19) . . . . ?
N4 C16 N6 C20 173.0(2) . . . . ?
C17 C16 N6 C20 -2.4(3) . . . . ?
N4 C16 N6 Co3 -2.9(3) . . . . ?
C17 C16 N6 Co3 -178.30(16) . . . . ?

_refine_diff_density_max         1.123
_refine_diff_density_min         -0.856
_refine_diff_density_rms         0.081


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dichloromethane'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_1-2CH2CL2-250K
_database_code_depnum_ccdc_archive 'CCDC 1865578'
_audit_update_record             
;
2018-09-03 deposited with the CCDC.
2018-11-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C40 H32 Co3 F2 N12, 2(C H2 Cl2)'
_chemical_formula_sum            'C42 H36 Cl4 Co3 F2 N12'
_chemical_formula_weight         1065.42

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'
Cl Cl 0.1484 0.1585 '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'
F F 0.0171 0.0103 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

_cell_length_a                   20.4657(15)
_cell_length_b                   13.9159(8)
_cell_length_c                   17.1718(12)
_cell_angle_alpha                90
_cell_angle_beta                 118.216(2)
_cell_angle_gamma                90
_cell_volume                     4309.4(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    5829
_cell_measurement_theta_min      2.57
_cell_measurement_theta_max      25.07

_exptl_crystal_description       needles
_exptl_crystal_colour            'dark reddish-brown'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_F_000             2156
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    1.447
_shelx_estimated_absorpt_T_min   0.846
_shelx_estimated_absorpt_T_max   0.944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6863
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   'SADABS (Bruker, 2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            33158
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.947
_diffrn_reflns_theta_max         25.378
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3954
_reflns_number_gt                2751
_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       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_structure_solution    'SHELXS2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_publication_material  'SHELXL-2016/4 (Sheldrick, 2016)'
_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)+(0.0570P)²+19.7046P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3954
_refine_ls_number_parameters     287
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0459
_refine_ls_wR_factor_ref         0.1328
_refine_ls_wR_factor_gt          0.1169
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.000
_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
C1 C 0.6395(2) 0.9474(3) 0.2734(3) 0.0360(10) Uani 1 1 d . . . . .
H1 H 0.620725 1.004671 0.284130 0.043 Uiso 1 1 calc R U . . .
C1S C 0.4107(3) 0.2088(3) 0.1638(4) 0.0583(15) Uani 1 1 d . . . . .
H1SA H 0.437362 0.265381 0.198015 0.070 Uiso 1 1 calc R U . . .
H1SB H 0.438031 0.151491 0.195819 0.070 Uiso 1 1 calc R U . . .
C2 C 0.7093(3) 0.9484(3) 0.2803(3) 0.0444(12) Uani 1 1 d . . . . .
H2 H 0.736796 1.005674 0.292440 0.053 Uiso 1 1 calc R U . . .
C3 C 0.7378(3) 0.8622(3) 0.2686(3) 0.0439(12) Uani 1 1 d . . . . .
H3 H 0.786051 0.859876 0.275053 0.053 Uiso 1 1 calc R U . . .
C4 C 0.6955(2) 0.7810(3) 0.2477(3) 0.0387(11) Uani 1 1 d . . . . .
H4 H 0.715132 0.722407 0.241023 0.046 Uiso 1 1 calc R U . . .
C5 C 0.6228(2) 0.7843(3) 0.2360(3) 0.0264(9) Uani 1 1 d . . . . .
C6 C 0.5792(2) 0.6306(3) 0.1663(3) 0.0289(9) Uani 1 1 d . . . . .
C7 C 0.6106(2) 0.6321(3) 0.1089(3) 0.0388(11) Uani 1 1 d . . . . .
H7 H 0.631092 0.689365 0.100927 0.047 Uiso 1 1 calc R U . . .
C8 C 0.6113(3) 0.5512(4) 0.0647(3) 0.0493(13) Uani 1 1 d . . . . .
H8 H 0.633107 0.552298 0.027245 0.059 Uiso 1 1 calc R U . . .
C9 C 0.5800(3) 0.4675(4) 0.0751(3) 0.0479(13) Uani 1 1 d . . . . .
H9 H 0.581099 0.410686 0.046197 0.057 Uiso 1 1 calc R U . . .
C10 C 0.5472(2) 0.4695(3) 0.1288(3) 0.0380(11) Uani 1 1 d . . . . .
H10 H 0.524334 0.413401 0.134558 0.046 Uiso 1 1 calc R U . . .
C11 C 0.4496(2) 0.9464(3) 0.0739(3) 0.0336(10) Uani 1 1 d . . . . .
H11 H 0.472637 1.002512 0.105441 0.040 Uiso 1 1 calc R U . . .
C12 C 0.5832(3) 0.9490(3) 0.5167(3) 0.0410(11) Uani 1 1 d . . . . .
H12 H 0.584202 1.005933 0.546682 0.049 Uiso 1 1 calc R U . . .
C13 C 0.6146(3) 0.8656(3) 0.5622(3) 0.0411(11) Uani 1 1 d . . . . .
H13 H 0.636495 0.864577 0.624207 0.049 Uiso 1 1 calc R U . . .
C14 C 0.6139(3) 0.7843(3) 0.5170(3) 0.0356(10) Uani 1 1 d . . . . .
H14 H 0.634875 0.727263 0.548143 0.043 Uiso 1 1 calc R U . . .
C15 C 0.5817(2) 0.7854(3) 0.4239(3) 0.0263(9) Uani 1 1 d . . . . .
C16 C 0.6244(2) 0.6316(3) 0.4000(3) 0.0256(9) Uani 1 1 d . . . . .
C17 C 0.6979(2) 0.6335(3) 0.4697(3) 0.0326(10) Uani 1 1 d . . . . .
H17 H 0.715570 0.688571 0.505401 0.039 Uiso 1 1 calc R U . . .
C18 C 0.7432(2) 0.5562(3) 0.4858(3) 0.0377(10) Uani 1 1 d . . . . .
H18 H 0.792054 0.558089 0.532415 0.045 Uiso 1 1 calc R U . . .
C19 C 0.7177(2) 0.4750(3) 0.4336(3) 0.0388(11) Uani 1 1 d . . . . .
H19 H 0.748503 0.421331 0.443309 0.047 Uiso 1 1 calc R U . . .
C20 C 0.6457(2) 0.4754(3) 0.3670(3) 0.0336(10) Uani 1 1 d . . . . .
H20 H 0.627889 0.420501 0.331053 0.040 Uiso 1 1 calc R U . . .
Cl1 Cl 0.32100(13) 0.20650(14) 0.1539(2) 0.1303(10) Uani 1 1 d . . . . .
Cl2 Cl 0.4074(2) 0.21214(16) 0.06350(19) 0.1651(15) Uani 1 1 d . . . . .
Co1 Co 0.500000 0.87563(5) 0.250000 0.0230(2) Uani 1 2 d S T P . .
Co2 Co 0.500000 0.70816(5) 0.250000 0.0217(2) Uani 1 2 d S T P . .
Co3 Co 0.500000 0.54179(5) 0.250000 0.0243(2) Uani 1 2 d S T P . .
F1 F 0.500000 1.0205(2) 0.250000 0.0331(8) Uani 1 2 d S T P . .
F2 F 0.500000 0.3976(2) 0.250000 0.0401(9) Uani 1 2 d S T P . .
N1 N 0.59667(18) 0.8678(2) 0.2521(2) 0.0264(7) Uani 1 1 d . . . . .
N2 N 0.45055(18) 0.8672(2) 0.1201(2) 0.0262(7) Uani 1 1 d . . . . .
N3 N 0.57522(18) 0.7078(2) 0.2133(2) 0.0264(7) Uani 1 1 d . . . . .
N4 N 0.57618(18) 0.7074(2) 0.3723(2) 0.0244(7) Uani 1 1 d . . . . .
N5 N 0.54654(18) 0.5490(2) 0.1735(2) 0.0276(8) Uani 1 1 d . . . . .
N6 N 0.59923(18) 0.5501(2) 0.3503(2) 0.0250(7) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.351(5) . ?
C1 C2 1.378(6) . ?
C1 H1 0.9400 . ?
C1S Cl2 1.692(6) . ?
C1S Cl1 1.762(6) . ?
C1S H1SA 0.9800 . ?
C1S H1SB 0.9800 . ?
C2 C3 1.389(7) . ?
C2 H2 0.9400 . ?
C3 C4 1.365(6) . ?
C3 H3 0.9400 . ?
C4 C5 1.405(6) . ?
C4 H4 0.9400 . ?
C5 N1 1.360(5) . ?
C5 N3 1.369(5) . ?
C6 N5 1.353(5) . ?
C6 N3 1.369(5) . ?
C6 C7 1.409(6) . ?
C7 C8 1.362(6) . ?
C7 H7 0.9400 . ?
C8 C9 1.381(7) . ?
C8 H8 0.9400 . ?
C9 C10 1.373(6) . ?
C9 H9 0.9400 . ?
C10 N5 1.350(5) . ?
C10 H10 0.9400 . ?
C11 N2 1.353(5) . ?
C11 C12 1.372(6) 2_655 ?
C11 H11 0.9400 . ?
C12 C13 1.377(6) . ?
C12 H12 0.9400 . ?
C13 C14 1.369(6) . ?
C13 H13 0.9400 . ?
C14 C15 1.413(6) . ?
C14 H14 0.9400 . ?
C15 N2 1.353(5) 2_655 ?
C15 N4 1.371(5) . ?
C16 N6 1.365(5) . ?
C16 N4 1.367(5) . ?
C16 C17 1.412(6) . ?
C17 C18 1.361(6) . ?
C17 H17 0.9400 . ?
C18 C19 1.383(6) . ?
C18 H18 0.9400 . ?
C19 C20 1.373(6) . ?
C19 H19 0.9400 . ?
C20 N6 1.345(5) . ?
C20 H20 0.9400 . ?
Co1 N1 1.965(3) 2_655 ?
Co1 N1 1.965(3) . ?
Co1 N2 1.969(3) 2_655 ?
Co1 N2 1.969(3) . ?
Co1 F1 2.016(3) . ?
Co1 Co2 2.3304(9) . ?
Co2 N3 1.919(3) . ?
Co2 N3 1.919(3) 2_655 ?
Co2 N4 1.936(3) . ?
Co2 N4 1.936(3) 2_655 ?
Co2 Co3 2.3153(9) . ?
Co3 N6 1.949(3) 2_655 ?
Co3 N6 1.949(3) . ?
Co3 N5 1.956(3) 2_655 ?
Co3 N5 1.956(3) . ?
Co3 F2 2.007(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 123.1(4) . . ?
N1 C1 H1 118.5 . . ?
C2 C1 H1 118.5 . . ?
Cl2 C1S Cl1 111.4(4) . . ?
Cl2 C1S H1SA 109.4 . . ?
Cl1 C1S H1SA 109.4 . . ?
Cl2 C1S H1SB 109.4 . . ?
Cl1 C1S H1SB 109.4 . . ?
H1SA C1S H1SB 108.0 . . ?
C1 C2 C3 117.9(4) . . ?
C1 C2 H2 121.0 . . ?
C3 C2 H2 121.0 . . ?
C4 C3 C2 119.7(4) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C3 C4 C5 120.5(4) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
N1 C5 N3 115.2(3) . . ?
N1 C5 C4 119.4(4) . . ?
N3 C5 C4 125.3(4) . . ?
N5 C6 N3 115.8(3) . . ?
N5 C6 C7 119.0(4) . . ?
N3 C6 C7 125.1(4) . . ?
C8 C7 C6 120.4(4) . . ?
C8 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
C7 C8 C9 119.8(4) . . ?
C7 C8 H8 120.1 . . ?
C9 C8 H8 120.1 . . ?
C10 C9 C8 118.3(4) . . ?
C10 C9 H9 120.9 . . ?
C8 C9 H9 120.9 . . ?
N5 C10 C9 122.6(4) . . ?
N5 C10 H10 118.7 . . ?
C9 C10 H10 118.7 . . ?
N2 C11 C12 123.4(4) . 2_655 ?
N2 C11 H11 118.3 . . ?
C12 C11 H11 118.3 2_655 . ?
C11 C12 C13 117.9(4) 2_655 . ?
C11 C12 H12 121.0 2_655 . ?
C13 C12 H12 121.0 . . ?
C14 C13 C12 119.9(4) . . ?
C14 C13 H13 120.1 . . ?
C12 C13 H13 120.1 . . ?
C13 C14 C15 120.5(4) . . ?
C13 C14 H14 119.8 . . ?
C15 C14 H14 119.8 . . ?
N2 C15 N4 115.9(3) 2_655 . ?
N2 C15 C14 119.0(4) 2_655 . ?
N4 C15 C14 125.0(4) . . ?
N6 C16 N4 115.3(3) . . ?
N6 C16 C17 118.8(4) . . ?
N4 C16 C17 125.8(4) . . ?
C18 C17 C16 120.5(4) . . ?
C18 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
C17 C18 C19 120.1(4) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
C20 C19 C18 117.7(4) . . ?
C20 C19 H19 121.2 . . ?
C18 C19 H19 121.2 . . ?
N6 C20 C19 123.5(4) . . ?
N6 C20 H20 118.2 . . ?
C19 C20 H20 118.2 . . ?
N1 Co1 N1 173.61(18) 2_655 . ?
N1 Co1 N2 89.50(13) 2_655 2_655 ?
N1 Co1 N2 90.12(13) . 2_655 ?
N1 Co1 N2 90.12(13) 2_655 . ?
N1 Co1 N2 89.50(13) . . ?
N2 Co1 N2 173.15(18) 2_655 . ?
N1 Co1 F1 93.20(9) 2_655 . ?
N1 Co1 F1 93.20(9) . . ?
N2 Co1 F1 93.42(9) 2_655 . ?
N2 Co1 F1 93.42(9) . . ?
N1 Co1 Co2 86.80(9) 2_655 . ?
N1 Co1 Co2 86.80(9) . . ?
N2 Co1 Co2 86.58(9) 2_655 . ?
N2 Co1 Co2 86.58(9) . . ?
F1 Co1 Co2 180.0 . . ?
N3 Co2 N3 179.73(18) . 2_655 ?
N3 Co2 N4 89.80(14) . . ?
N3 Co2 N4 90.19(14) 2_655 . ?
N3 Co2 N4 90.19(14) . 2_655 ?
N3 Co2 N4 89.81(14) 2_655 2_655 ?
N4 Co2 N4 179.38(18) . 2_655 ?
N3 Co2 Co3 89.87(9) . . ?
N3 Co2 Co3 89.87(9) 2_655 . ?
N4 Co2 Co3 89.69(9) . . ?
N4 Co2 Co3 89.69(9) 2_655 . ?
N3 Co2 Co1 90.13(9) . . ?
N3 Co2 Co1 90.13(9) 2_655 . ?
N4 Co2 Co1 90.31(9) . . ?
N4 Co2 Co1 90.31(9) 2_655 . ?
Co3 Co2 Co1 180.0 . . ?
N6 Co3 N6 173.20(18) 2_655 . ?
N6 Co3 N5 87.47(13) 2_655 2_655 ?
N6 Co3 N5 92.18(13) . 2_655 ?
N6 Co3 N5 92.18(13) 2_655 . ?
N6 Co3 N5 87.47(13) . . ?
N5 Co3 N5 174.14(18) 2_655 . ?
N6 Co3 F2 93.40(9) 2_655 . ?
N6 Co3 F2 93.40(9) . . ?
N5 Co3 F2 92.93(9) 2_655 . ?
N5 Co3 F2 92.93(9) . . ?
N6 Co3 Co2 86.60(9) 2_655 . ?
N6 Co3 Co2 86.60(9) . . ?
N5 Co3 Co2 87.07(9) 2_655 . ?
N5 Co3 Co2 87.07(9) . . ?
F2 Co3 Co2 180.0 . . ?
C1 N1 C5 119.2(3) . . ?
C1 N1 Co1 118.5(3) . . ?
C5 N1 Co1 122.2(3) . . ?
C15 N2 C11 119.3(4) 2_655 . ?
C15 N2 Co1 122.4(3) 2_655 . ?
C11 N2 Co1 118.2(3) . . ?
C5 N3 C6 123.0(3) . . ?
C5 N3 Co2 118.5(2) . . ?
C6 N3 Co2 118.4(3) . . ?
C16 N4 C15 124.1(3) . . ?
C16 N4 Co2 117.4(3) . . ?
C15 N4 Co2 118.3(3) . . ?
C10 N5 C6 119.8(4) . . ?
C10 N5 Co3 118.7(3) . . ?
C6 N5 Co3 121.5(3) . . ?
C20 N6 C16 119.3(3) . . ?
C20 N6 Co3 118.6(3) . . ?
C16 N6 Co3 121.9(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
N1 C1 C2 C3 -3.1(7) . . . . ?
C1 C2 C3 C4 2.5(7) . . . . ?
C2 C3 C4 C5 1.4(7) . . . . ?
C3 C4 C5 N1 -4.8(7) . . . . ?
C3 C4 C5 N3 178.6(4) . . . . ?
N5 C6 C7 C8 -3.4(6) . . . . ?
N3 C6 C7 C8 -179.6(4) . . . . ?
C6 C7 C8 C9 1.2(7) . . . . ?
C7 C8 C9 C10 1.5(7) . . . . ?
C8 C9 C10 N5 -2.1(7) . . . . ?
C11 C12 C13 C14 1.5(7) 2_655 . . . ?
C12 C13 C14 C15 0.6(7) . . . . ?
C13 C14 C15 N2 -2.3(6) . . . 2_655 ?
C13 C14 C15 N4 -177.9(4) . . . . ?
N6 C16 C17 C18 1.5(6) . . . . ?
N4 C16 C17 C18 -173.4(4) . . . . ?
C16 C17 C18 C19 0.1(6) . . . . ?
C17 C18 C19 C20 -0.8(6) . . . . ?
C18 C19 C20 N6 -0.2(7) . . . . ?
C2 C1 N1 C5 -0.3(7) . . . . ?
C2 C1 N1 Co1 177.3(4) . . . . ?
N3 C5 N1 C1 -178.9(4) . . . . ?
C4 C5 N1 C1 4.2(6) . . . . ?
N3 C5 N1 Co1 3.6(5) . . . . ?
C4 C5 N1 Co1 -173.3(3) . . . . ?
C12 C11 N2 C15 0.5(6) 2_655 . . 2_655 ?
C12 C11 N2 Co1 -179.9(3) 2_655 . . . ?
N1 C5 N3 C6 156.6(4) . . . . ?
C4 C5 N3 C6 -26.7(6) . . . . ?
N1 C5 N3 Co2 -24.0(5) . . . . ?
C4 C5 N3 Co2 152.7(4) . . . . ?
N5 C6 N3 C5 159.1(4) . . . . ?
C7 C6 N3 C5 -24.5(6) . . . . ?
N5 C6 N3 Co2 -20.2(5) . . . . ?
C7 C6 N3 Co2 156.1(3) . . . . ?
N6 C16 N4 C15 162.3(3) . . . . ?
C17 C16 N4 C15 -22.6(6) . . . . ?
N6 C16 N4 Co2 -22.4(4) . . . . ?
C17 C16 N4 Co2 152.7(3) . . . . ?
N2 C15 N4 C16 155.9(3) 2_655 . . . ?
C14 C15 N4 C16 -28.3(6) . . . . ?
N2 C15 N4 Co2 -19.3(4) 2_655 . . . ?
C14 C15 N4 Co2 156.5(3) . . . . ?
C9 C10 N5 C6 -0.1(6) . . . . ?
C9 C10 N5 Co3 -178.6(3) . . . . ?
N3 C6 N5 C10 179.4(4) . . . . ?
C7 C6 N5 C10 2.8(6) . . . . ?
N3 C6 N5 Co3 -2.2(5) . . . . ?
C7 C6 N5 Co3 -178.7(3) . . . . ?
C19 C20 N6 C16 1.8(6) . . . . ?
C19 C20 N6 Co3 177.3(3) . . . . ?
N4 C16 N6 C20 173.0(3) . . . . ?
C17 C16 N6 C20 -2.4(5) . . . . ?
N4 C16 N6 Co3 -2.3(5) . . . . ?
C17 C16 N6 Co3 -177.7(3) . . . . ?

_refine_diff_density_max         1.201
_refine_diff_density_min         -0.921
_refine_diff_density_rms         0.082


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dichloromethane'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_2-Et2O-298K
_database_code_depnum_ccdc_archive 'CCDC 1865582'
_audit_update_record             
;
2018-09-03 deposited with the CCDC.
2018-11-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C40 H32 Cl2 Co3 N12, C4 H10 O'
_chemical_formula_sum            'C44 H42 Cl2 Co3 N12 O'
_chemical_formula_weight         1002.58

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'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   15.9782(17)
_cell_length_b                   15.8417(18)
_cell_length_c                   17.110(2)
_cell_angle_alpha                90
_cell_angle_beta                 98.357(5)
_cell_angle_gamma                90
_cell_volume                     4284.9(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9857
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      27.412

_exptl_crystal_description       Blocks
_exptl_crystal_colour            'Dark green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_F_000             2052
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.062
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.033
_exptl_absorpt_coefficient_mu    1.324
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6861
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'SADABS (Bruker, 2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            111519
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.761
_diffrn_reflns_theta_max         28.344
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             10646
_reflns_number_gt                7704
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0404P)²+3.6258P] 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_number_reflns         10646
_refine_ls_number_parameters     561
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0371
_refine_ls_wR_factor_ref         0.0985
_refine_ls_wR_factor_gt          0.0868
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.002
_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
C1 C 0.73426(19) -0.15680(19) 0.42445(16) 0.0428(7) Uani 1 1 d . . . . .
H1 H 0.684827 -0.150883 0.446695 0.051 Uiso 1 1 calc R U . . .
C2 C 0.7984(2) -0.2033(2) 0.46450(17) 0.0498(8) Uani 1 1 d . . . . .
H2 H 0.792095 -0.230502 0.511445 0.060 Uiso 1 1 calc R U . . .
C3 C 0.8737(2) -0.20870(19) 0.43292(16) 0.0472(7) Uani 1 1 d . . . . .
H3 H 0.919001 -0.239272 0.459040 0.057 Uiso 1 1 calc R U . . .
C4 C 0.88066(17) -0.16907(17) 0.36362(16) 0.0386(6) Uani 1 1 d . . . . .
H4 H 0.931402 -0.171429 0.343082 0.046 Uiso 1 1 calc R U . . .
C5 C 0.81132(15) -0.12437(15) 0.32270(14) 0.0283(5) Uani 1 1 d . . . . .
C6 C 0.86648(14) -0.09774(15) 0.20077(14) 0.0265(5) Uani 1 1 d . . . . .
C7 C 0.89845(17) -0.17884(17) 0.18851(16) 0.0377(6) Uani 1 1 d . . . . .
H7 H 0.885298 -0.223933 0.219345 0.045 Uiso 1 1 calc R U . . .
C8 C 0.94899(18) -0.19141(19) 0.13115(17) 0.0432(7) Uani 1 1 d . . . . .
H8 H 0.971842 -0.244444 0.124378 0.052 Uiso 1 1 calc R U . . .
C9 C 0.96573(18) -0.12483(19) 0.08348(17) 0.0445(7) Uani 1 1 d . . . . .
H9 H 0.999478 -0.132357 0.044090 0.053 Uiso 1 1 calc R U . . .
C10 C 0.93141(16) -0.04747(18) 0.09566(16) 0.0376(6) Uani 1 1 d . . . . .
H10 H 0.941014 -0.003169 0.062426 0.045 Uiso 1 1 calc R U . . .
C11 C 0.61629(19) 0.06101(18) 0.43695(17) 0.0441(7) Uani 1 1 d . . . . .
H11 H 0.563205 0.035743 0.428604 0.053 Uiso 1 1 calc R U . . .
C12 C 0.6339(2) 0.1154(2) 0.49911(19) 0.0552(8) Uani 1 1 d . . . . .
H12 H 0.594462 0.125858 0.532911 0.066 Uiso 1 1 calc R U . . .
C13 C 0.7121(2) 0.1545(2) 0.51026(18) 0.0539(8) Uani 1 1 d . . . . .
H13 H 0.726770 0.190466 0.552988 0.065 Uiso 1 1 calc R U . . .
C14 C 0.76832(19) 0.13984(18) 0.45785(16) 0.0430(7) Uani 1 1 d . . . . .
H14 H 0.819745 0.168327 0.463564 0.052 Uiso 1 1 calc R U . . .
C15 C 0.74801(16) 0.08189(15) 0.39571(14) 0.0302(5) Uani 1 1 d . . . . .
C16 C 0.88360(15) 0.07367(15) 0.34777(14) 0.0283(5) Uani 1 1 d . . . . .
C17 C 0.93772(17) 0.07168(18) 0.42057(16) 0.0413(6) Uani 1 1 d . . . . .
H17 H 0.915061 0.072029 0.467662 0.050 Uiso 1 1 calc R U . . .
C18 C 1.02392(19) 0.0692(2) 0.42206(19) 0.0517(8) Uani 1 1 d . . . . .
H18 H 1.059667 0.068651 0.470076 0.062 Uiso 1 1 calc R U . . .
C19 C 1.05716(18) 0.0677(2) 0.3522(2) 0.0538(8) Uani 1 1 d . . . . .
H19 H 1.115255 0.063891 0.352217 0.065 Uiso 1 1 calc R U . . .
C20 C 1.00262(16) 0.07181(19) 0.28238(18) 0.0416(6) Uani 1 1 d . . . . .
H20 H 1.025107 0.070774 0.235213 0.050 Uiso 1 1 calc R U . . .
C21 C 0.47762(16) 0.0200(2) 0.22553(18) 0.0428(7) Uani 1 1 d . . . . .
H21 H 0.458309 -0.029479 0.246078 0.051 Uiso 1 1 calc R U . . .
C22 C 0.41992(17) 0.0708(2) 0.18199(19) 0.0493(8) Uani 1 1 d . . . . .
H22 H 0.362753 0.056963 0.173937 0.059 Uiso 1 1 calc R U . . .
C23 C 0.44857(17) 0.1433(2) 0.15022(17) 0.0454(7) Uani 1 1 d . . . . .
H23 H 0.410522 0.179269 0.120379 0.055 Uiso 1 1 calc R U . . .
C24 C 0.53355(16) 0.16257(18) 0.16257(16) 0.0382(6) Uani 1 1 d . . . . .
H24 H 0.553316 0.210713 0.140080 0.046 Uiso 1 1 calc R U . . .
C25 C 0.59029(14) 0.10861(15) 0.20965(14) 0.0285(5) Uani 1 1 d . . . . .
C26 C 0.71530(15) 0.19577(15) 0.22178(14) 0.0285(5) Uani 1 1 d . . . . .
C27 C 0.67982(18) 0.27360(17) 0.24038(16) 0.0404(6) Uani 1 1 d . . . . .
H27 H 0.623755 0.276041 0.249085 0.049 Uiso 1 1 calc R U . . .
C28 C 0.7279(2) 0.34532(19) 0.24559(18) 0.0495(7) Uani 1 1 d . . . . .
H28 H 0.704513 0.396877 0.256926 0.059 Uiso 1 1 calc R U . . .
C29 C 0.8115(2) 0.34045(19) 0.2338(2) 0.0531(8) Uani 1 1 d . . . . .
H29 H 0.845452 0.388420 0.238262 0.064 Uiso 1 1 calc R U . . .
C30 C 0.84373(18) 0.26422(18) 0.21559(17) 0.0419(7) Uani 1 1 d . . . . .
H30 H 0.900373 0.261308 0.208837 0.050 Uiso 1 1 calc R U . . .
C31 C 0.57807(18) -0.19609(18) 0.20597(18) 0.0439(7) Uani 1 1 d . . . . .
H31 H 0.562176 -0.214045 0.253437 0.053 Uiso 1 1 calc R U . . .
C32 C 0.5566(2) -0.2454(2) 0.1409(2) 0.0541(8) Uani 1 1 d . . . . .
H32 H 0.524387 -0.293944 0.143333 0.065 Uiso 1 1 calc R U . . .
C33 C 0.5842(2) -0.22140(19) 0.07055(19) 0.0525(8) Uani 1 1 d . . . . .
H33 H 0.571347 -0.254179 0.025311 0.063 Uiso 1 1 calc R U . . .
C34 C 0.63025(18) -0.14922(18) 0.06900(16) 0.0419(6) Uani 1 1 d . . . . .
H34 H 0.650841 -0.133838 0.022907 0.050 Uiso 1 1 calc R U . . .
C35 C 0.64703(15) -0.09751(16) 0.13670(15) 0.0301(5) Uani 1 1 d . . . . .
C36 C 0.69238(15) 0.02747(15) 0.07509(14) 0.0296(5) Uani 1 1 d . . . . .
C37 C 0.62544(18) 0.03306(18) 0.01202(17) 0.0432(7) Uani 1 1 d . . . . .
H37 H 0.579034 -0.002645 0.010562 0.052 Uiso 1 1 calc R U . . .
C38 C 0.6281(2) 0.0904(2) -0.04690(17) 0.0528(8) Uani 1 1 d . . . . .
H38 H 0.583372 0.094683 -0.088030 0.063 Uiso 1 1 calc R U . . .
C39 C 0.6982(2) 0.1423(2) -0.04494(17) 0.0559(9) Uani 1 1 d . . . . .
H39 H 0.702260 0.180532 -0.085424 0.067 Uiso 1 1 calc R U . . .
C40 C 0.7616(2) 0.13572(18) 0.01843(16) 0.0430(7) Uani 1 1 d . . . . .
H40 H 0.808220 0.171240 0.020153 0.052 Uiso 1 1 calc R U . . .
C100 C 0.3144(3) 0.0587(3) 0.3770(3) 0.0868(13) Uani 1 1 d . . . . .
H10A H 0.272195 0.025796 0.397744 0.130 Uiso 1 1 calc R U . . .
H10B H 0.343561 0.093516 0.418187 0.130 Uiso 1 1 calc R U . . .
H10C H 0.354145 0.021630 0.357418 0.130 Uiso 1 1 calc R U . . .
C101 C 0.2725(2) 0.1140(2) 0.3104(2) 0.0684(10) Uani 1 1 d . . . . .
H10D H 0.230641 0.150043 0.329394 0.082 Uiso 1 1 calc R U . . .
H10E H 0.314405 0.149657 0.291191 0.082 Uiso 1 1 calc R U . . .
C102 C 0.1973(2) 0.1115(3) 0.1843(2) 0.0729(12) Uani 1 1 d . . . . .
H10F H 0.238401 0.150771 0.168715 0.088 Uiso 1 1 calc R U . . .
H10G H 0.148900 0.142853 0.196932 0.088 Uiso 1 1 calc R U . . .
C103 C 0.1695(3) 0.0441(3) 0.1166(2) 0.0930(15) Uani 1 1 d . . . . .
H10H H 0.218947 0.018792 0.100610 0.140 Uiso 1 1 calc R U . . .
H10I H 0.137231 0.071616 0.072126 0.140 Uiso 1 1 calc R U . . .
H10J H 0.135611 0.001118 0.136189 0.140 Uiso 1 1 calc R U . . .
N1 N 0.73821(13) -0.11864(13) 0.35404(12) 0.0305(4) Uani 1 1 d . . . . .
N2 N 0.67183(13) 0.04169(13) 0.38662(12) 0.0313(5) Uani 1 1 d . . . . .
N3 N 0.56119(12) 0.03711(13) 0.24070(13) 0.0319(5) Uani 1 1 d . . . . .
N4 N 0.62108(12) -0.12255(13) 0.20564(12) 0.0317(5) Uani 1 1 d . . . . .
N5 N 0.81347(12) -0.07885(12) 0.25480(11) 0.0265(4) Uani 1 1 d . . . . .
N6 N 0.79766(12) 0.06465(13) 0.33810(11) 0.0279(4) Uani 1 1 d . . . . .
N7 N 0.67605(12) 0.11913(12) 0.22259(12) 0.0272(4) Uani 1 1 d . . . . .
N8 N 0.69159(12) -0.02366(13) 0.13983(11) 0.0273(4) Uani 1 1 d . . . . .
N9 N 0.88413(12) -0.03251(13) 0.15389(11) 0.0278(4) Uani 1 1 d . . . . .
N10 N 0.91784(12) 0.07731(13) 0.27913(12) 0.0297(4) Uani 1 1 d . . . . .
N11 N 0.79686(13) 0.19274(13) 0.20691(12) 0.0298(4) Uani 1 1 d . . . . .
N12 N 0.75981(13) 0.08040(13) 0.07823(12) 0.0296(4) Uani 1 1 d . . . . .
O100 O 0.23325(14) 0.06203(15) 0.24890(14) 0.0590(6) Uani 1 1 d . . . . .
CL1 Cl 0.53343(4) -0.11697(5) 0.37044(5) 0.04798(18) Uani 1 1 d . . . . .
CL2 Cl 0.95283(4) 0.15637(5) 0.10932(4) 0.04598(17) Uani 1 1 d . . . . .
CO1 Co 0.63996(2) -0.04738(2) 0.30250(2) 0.03045(9) Uani 1 1 d . . . . .
CO2 Co 0.74467(2) 0.02023(2) 0.23931(2) 0.02302(8) Uani 1 1 d . . . . .
CO3 Co 0.84644(2) 0.08417(2) 0.17440(2) 0.02657(8) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.357(3) . ?
C1 C2 1.364(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.390(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.361(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.412(3) . ?
C4 H4 0.9300 . ?
C5 N1 1.357(3) . ?
C5 N5 1.372(3) . ?
C6 N9 1.363(3) . ?
C6 N5 1.374(3) . ?
C6 C7 1.410(3) . ?
C7 C8 1.373(4) . ?
C7 H7 0.9300 . ?
C8 C9 1.383(4) . ?
C8 H8 0.9300 . ?
C9 C10 1.371(4) . ?
C9 H9 0.9300 . ?
C10 N9 1.356(3) . ?
C10 H10 0.9300 . ?
C11 N2 1.358(3) . ?
C11 C12 1.366(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.383(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.377(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.406(4) . ?
C14 H14 0.9300 . ?
C15 N2 1.363(3) . ?
C15 N6 1.379(3) . ?
C16 N6 1.367(3) . ?
C16 N10 1.367(3) . ?
C16 C17 1.410(3) . ?
C17 C18 1.374(4) . ?
C17 H17 0.9300 . ?
C18 C19 1.378(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.374(4) . ?
C19 H19 0.9300 . ?
C20 N10 1.350(3) . ?
C20 H20 0.9300 . ?
C21 N3 1.350(3) . ?
C21 C22 1.361(4) . ?
C21 H21 0.9300 . ?
C22 C23 1.377(4) . ?
C22 H22 0.9300 . ?
C23 C24 1.378(4) . ?
C23 H23 0.9300 . ?
C24 C25 1.410(3) . ?
C24 H24 0.9300 . ?
C25 N3 1.361(3) . ?
C25 N7 1.366(3) . ?
C26 N11 1.364(3) . ?
C26 N7 1.368(3) . ?
C26 C27 1.413(4) . ?
C27 C28 1.367(4) . ?
C27 H27 0.9300 . ?
C28 C29 1.383(4) . ?
C28 H28 0.9300 . ?
C29 C30 1.366(4) . ?
C29 H29 0.9300 . ?
C30 N11 1.354(3) . ?
C30 H30 0.9300 . ?
C31 N4 1.353(3) . ?
C31 C32 1.363(4) . ?
C31 H31 0.9300 . ?
C32 C33 1.393(5) . ?
C32 H32 0.9300 . ?
C33 C34 1.362(4) . ?
C33 H33 0.9300 . ?
C34 C35 1.412(4) . ?
C34 H34 0.9300 . ?
C35 N4 1.365(3) . ?
C35 N8 1.367(3) . ?
C36 N12 1.360(3) . ?
C36 N8 1.374(3) . ?
C36 C37 1.407(4) . ?
C37 C38 1.362(4) . ?
C37 H37 0.9300 . ?
C38 C39 1.385(5) . ?
C38 H38 0.9300 . ?
C39 C40 1.376(4) . ?
C39 H39 0.9300 . ?
C40 N12 1.351(3) . ?
C40 H40 0.9300 . ?
C100 C101 1.515(5) . ?
C100 H10A 0.9600 . ?
C100 H10B 0.9600 . ?
C100 H10C 0.9600 . ?
C101 O100 1.410(4) . ?
C101 H10D 0.9700 . ?
C101 H10E 0.9700 . ?
C102 O100 1.407(4) . ?
C102 C103 1.591(6) . ?
C102 H10F 0.9700 . ?
C102 H10G 0.9700 . ?
C103 H10H 0.9600 . ?
C103 H10I 0.9600 . ?
C103 H10J 0.9600 . ?
N1 CO1 2.028(2) . ?
N2 CO1 2.027(2) . ?
N3 CO1 2.027(2) . ?
N4 CO1 2.027(2) . ?
N5 CO2 1.9125(19) . ?
N6 CO2 1.911(2) . ?
N7 CO2 1.9098(19) . ?
N8 CO2 1.918(2) . ?
N9 CO3 1.991(2) . ?
N10 CO3 1.982(2) . ?
N11 CO3 2.006(2) . ?
N12 CO3 1.991(2) . ?
CL1 CO1 2.4574(7) . ?
CL2 CO3 2.4471(7) . ?
CO1 CO2 2.3752(5) . ?
CO2 CO3 2.3299(5) . ?

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
N1 C1 C2 123.9(3) . . ?
N1 C1 H1 118.0 . . ?
C2 C1 H1 118.0 . . ?
C1 C2 C3 117.9(3) . . ?
C1 C2 H2 121.1 . . ?
C3 C2 H2 121.1 . . ?
C4 C3 C2 119.7(3) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C3 C4 C5 120.4(3) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
N1 C5 N5 115.4(2) . . ?
N1 C5 C4 119.7(2) . . ?
N5 C5 C4 124.7(2) . . ?
N9 C6 N5 115.5(2) . . ?
N9 C6 C7 119.5(2) . . ?
N5 C6 C7 124.8(2) . . ?
C8 C7 C6 120.1(3) . . ?
C8 C7 H7 119.9 . . ?
C6 C7 H7 119.9 . . ?
C7 C8 C9 119.7(3) . . ?
C7 C8 H8 120.2 . . ?
C9 C8 H8 120.2 . . ?
C10 C9 C8 118.4(2) . . ?
C10 C9 H9 120.8 . . ?
C8 C9 H9 120.8 . . ?
N9 C10 C9 123.1(3) . . ?
N9 C10 H10 118.5 . . ?
C9 C10 H10 118.5 . . ?
N2 C11 C12 123.8(3) . . ?
N2 C11 H11 118.1 . . ?
C12 C11 H11 118.1 . . ?
C11 C12 C13 118.0(3) . . ?
C11 C12 H12 121.0 . . ?
C13 C12 H12 121.0 . . ?
C14 C13 C12 119.8(3) . . ?
C14 C13 H13 120.1 . . ?
C12 C13 H13 120.1 . . ?
C13 C14 C15 120.1(3) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
N2 C15 N6 115.0(2) . . ?
N2 C15 C14 119.7(2) . . ?
N6 C15 C14 125.2(2) . . ?
N6 C16 N10 114.9(2) . . ?
N6 C16 C17 125.5(2) . . ?
N10 C16 C17 119.3(2) . . ?
C18 C17 C16 120.1(3) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C17 C18 C19 119.8(3) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 H18 120.1 . . ?
C20 C19 C18 118.5(3) . . ?
C20 C19 H19 120.7 . . ?
C18 C19 H19 120.7 . . ?
N10 C20 C19 123.0(3) . . ?
N10 C20 H20 118.5 . . ?
C19 C20 H20 118.5 . . ?
N3 C21 C22 124.0(3) . . ?
N3 C21 H21 118.0 . . ?
C22 C21 H21 118.0 . . ?
C21 C22 C23 118.1(3) . . ?
C21 C22 H22 120.9 . . ?
C23 C22 H22 120.9 . . ?
C22 C23 C24 120.1(3) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C23 C24 C25 119.4(3) . . ?
C23 C24 H24 120.3 . . ?
C25 C24 H24 120.3 . . ?
N3 C25 N7 115.4(2) . . ?
N3 C25 C24 120.0(2) . . ?
N7 C25 C24 124.4(2) . . ?
N11 C26 N7 115.0(2) . . ?
N11 C26 C27 119.9(2) . . ?
N7 C26 C27 125.0(2) . . ?
C28 C27 C26 120.0(3) . . ?
C28 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
C27 C28 C29 119.3(3) . . ?
C27 C28 H28 120.3 . . ?
C29 C28 H28 120.3 . . ?
C30 C29 C28 119.1(3) . . ?
C30 C29 H29 120.4 . . ?
C28 C29 H29 120.4 . . ?
N11 C30 C29 122.9(3) . . ?
N11 C30 H30 118.5 . . ?
C29 C30 H30 118.5 . . ?
N4 C31 C32 123.9(3) . . ?
N4 C31 H31 118.1 . . ?
C32 C31 H31 118.1 . . ?
C31 C32 C33 118.4(3) . . ?
C31 C32 H32 120.8 . . ?
C33 C32 H32 120.8 . . ?
C34 C33 C32 119.1(3) . . ?
C34 C33 H33 120.5 . . ?
C32 C33 H33 120.5 . . ?
C33 C34 C35 120.6(3) . . ?
C33 C34 H34 119.7 . . ?
C35 C34 H34 119.7 . . ?
N4 C35 N8 115.9(2) . . ?
N4 C35 C34 119.7(2) . . ?
N8 C35 C34 124.4(2) . . ?
N12 C36 N8 115.6(2) . . ?
N12 C36 C37 120.1(2) . . ?
N8 C36 C37 124.1(2) . . ?
C38 C37 C36 120.5(3) . . ?
C38 C37 H37 119.8 . . ?
C36 C37 H37 119.8 . . ?
C37 C38 C39 119.3(3) . . ?
C37 C38 H38 120.3 . . ?
C39 C38 H38 120.3 . . ?
C40 C39 C38 118.3(3) . . ?
C40 C39 H39 120.8 . . ?
C38 C39 H39 120.8 . . ?
N12 C40 C39 123.4(3) . . ?
N12 C40 H40 118.3 . . ?
C39 C40 H40 118.3 . . ?
C101 C100 H10A 109.5 . . ?
C101 C100 H10B 109.5 . . ?
H10A C100 H10B 109.5 . . ?
C101 C100 H10C 109.5 . . ?
H10A C100 H10C 109.5 . . ?
H10B C100 H10C 109.5 . . ?
O100 C101 C100 108.9(3) . . ?
O100 C101 H10D 109.9 . . ?
C100 C101 H10D 109.9 . . ?
O100 C101 H10E 109.9 . . ?
C100 C101 H10E 109.9 . . ?
H10D C101 H10E 108.3 . . ?
O100 C102 C103 103.7(3) . . ?
O100 C102 H10F 111.0 . . ?
C103 C102 H10F 111.0 . . ?
O100 C102 H10G 111.0 . . ?
C103 C102 H10G 111.0 . . ?
H10F C102 H10G 109.0 . . ?
C102 C103 H10H 109.5 . . ?
C102 C103 H10I 109.5 . . ?
H10H C103 H10I 109.5 . . ?
C102 C103 H10J 109.5 . . ?
H10H C103 H10J 109.5 . . ?
H10I C103 H10J 109.5 . . ?
C1 N1 C5 118.3(2) . . ?
C1 N1 CO1 120.06(17) . . ?
C5 N1 CO1 121.44(16) . . ?
C11 N2 C15 118.5(2) . . ?
C11 N2 CO1 119.16(18) . . ?
C15 N2 CO1 122.31(16) . . ?
C21 N3 C25 118.4(2) . . ?
C21 N3 CO1 119.31(19) . . ?
C25 N3 CO1 122.12(15) . . ?
C31 N4 C35 118.2(2) . . ?
C31 N4 CO1 121.17(18) . . ?
C35 N4 CO1 120.53(16) . . ?
C5 N5 C6 123.3(2) . . ?
C5 N5 CO2 117.64(15) . . ?
C6 N5 CO2 118.92(15) . . ?
C16 N6 C15 124.4(2) . . ?
C16 N6 CO2 116.98(15) . . ?
C15 N6 CO2 118.56(16) . . ?
C25 N7 C26 123.9(2) . . ?
C25 N7 CO2 117.70(16) . . ?
C26 N7 CO2 118.40(15) . . ?
C35 N8 C36 122.6(2) . . ?
C35 N8 CO2 120.38(16) . . ?
C36 N8 CO2 116.55(16) . . ?
C10 N9 C6 119.0(2) . . ?
C10 N9 CO3 120.46(17) . . ?
C6 N9 CO3 120.44(15) . . ?
C20 N10 C16 119.1(2) . . ?
C20 N10 CO3 118.87(18) . . ?
C16 N10 CO3 121.96(15) . . ?
C30 N11 C26 118.6(2) . . ?
C30 N11 CO3 120.87(18) . . ?
C26 N11 CO3 120.55(16) . . ?
C40 N12 C36 118.3(2) . . ?
C40 N12 CO3 121.16(18) . . ?
C36 N12 CO3 120.17(16) . . ?
C102 O100 C101 110.4(3) . . ?
N3 CO1 N2 89.05(8) . . ?
N3 CO1 N4 87.37(8) . . ?
N2 CO1 N4 168.95(8) . . ?
N3 CO1 N1 167.74(8) . . ?
N2 CO1 N1 88.86(8) . . ?
N4 CO1 N1 92.43(8) . . ?
N3 CO1 CO2 83.67(6) . . ?
N2 CO1 CO2 83.59(6) . . ?
N4 CO1 CO2 85.63(6) . . ?
N1 CO1 CO2 84.09(6) . . ?
N3 CO1 CL1 97.05(6) . . ?
N2 CO1 CL1 95.52(6) . . ?
N4 CO1 CL1 95.29(6) . . ?
N1 CO1 CL1 95.18(6) . . ?
CO2 CO1 CL1 178.86(3) . . ?
N7 CO2 N6 90.08(9) . . ?
N7 CO2 N5 179.35(8) . . ?
N6 CO2 N5 90.45(8) . . ?
N7 CO2 N8 89.67(8) . . ?
N6 CO2 N8 179.63(9) . . ?
N5 CO2 N8 89.80(8) . . ?
N7 CO2 CO3 89.84(6) . . ?
N6 CO2 CO3 90.65(6) . . ?
N5 CO2 CO3 89.76(6) . . ?
N8 CO2 CO3 89.07(6) . . ?
N7 CO2 CO1 90.63(6) . . ?
N6 CO2 CO1 90.82(6) . . ?
N5 CO2 CO1 89.75(6) . . ?
N8 CO2 CO1 89.46(6) . . ?
CO3 CO2 CO1 178.454(19) . . ?
N10 CO3 N9 87.67(8) . . ?
N10 CO3 N12 170.03(8) . . ?
N9 CO3 N12 91.05(8) . . ?
N10 CO3 N11 89.71(8) . . ?
N9 CO3 N11 170.65(8) . . ?
N12 CO3 N11 89.98(8) . . ?
N10 CO3 CO2 83.98(6) . . ?
N9 CO3 CO2 86.01(6) . . ?
N12 CO3 CO2 86.06(6) . . ?
N11 CO3 CO2 84.80(6) . . ?
N10 CO3 CL2 95.19(6) . . ?
N9 CO3 CL2 96.08(6) . . ?
N12 CO3 CL2 94.79(6) . . ?
N11 CO3 CL2 93.09(6) . . ?
CO2 CO3 CL2 177.73(2) . . ?

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
N1 C1 C2 C3 3.0(5) . . . . ?
C1 C2 C3 C4 -0.8(5) . . . . ?
C2 C3 C4 C5 -1.6(5) . . . . ?
C3 C4 C5 N1 2.2(4) . . . . ?
C3 C4 C5 N5 176.4(3) . . . . ?
N9 C6 C7 C8 1.8(4) . . . . ?
N5 C6 C7 C8 177.9(2) . . . . ?
C6 C7 C8 C9 -2.4(4) . . . . ?
C7 C8 C9 C10 0.5(4) . . . . ?
C8 C9 C10 N9 2.2(4) . . . . ?
N2 C11 C12 C13 1.5(5) . . . . ?
C11 C12 C13 C14 2.0(5) . . . . ?
C12 C13 C14 C15 -3.4(5) . . . . ?
C13 C14 C15 N2 1.4(4) . . . . ?
C13 C14 C15 N6 177.3(3) . . . . ?
N6 C16 C17 C18 170.6(3) . . . . ?
N10 C16 C17 C18 -3.2(4) . . . . ?
C16 C17 C18 C19 -0.8(5) . . . . ?
C17 C18 C19 C20 2.4(5) . . . . ?
C18 C19 C20 N10 0.0(5) . . . . ?
N3 C21 C22 C23 1.2(5) . . . . ?
C21 C22 C23 C24 0.2(4) . . . . ?
C22 C23 C24 C25 -1.7(4) . . . . ?
C23 C24 C25 N3 1.7(4) . . . . ?
C23 C24 C25 N7 176.5(2) . . . . ?
N11 C26 C27 C28 -1.8(4) . . . . ?
N7 C26 C27 C28 173.3(3) . . . . ?
C26 C27 C28 C29 -1.1(4) . . . . ?
C27 C28 C29 C30 1.4(5) . . . . ?
C28 C29 C30 N11 1.3(5) . . . . ?
N4 C31 C32 C33 3.5(5) . . . . ?
C31 C32 C33 C34 -1.0(5) . . . . ?
C32 C33 C34 C35 -2.5(5) . . . . ?
C33 C34 C35 N4 3.8(4) . . . . ?
C33 C34 C35 N8 -179.1(3) . . . . ?
N12 C36 C37 C38 1.0(4) . . . . ?
N8 C36 C37 C38 174.5(3) . . . . ?
C36 C37 C38 C39 1.2(5) . . . . ?
C37 C38 C39 C40 -2.2(5) . . . . ?
C38 C39 C40 N12 1.1(5) . . . . ?
C2 C1 N1 C5 -2.4(4) . . . . ?
C2 C1 N1 CO1 -177.6(2) . . . . ?
N5 C5 N1 C1 -175.0(2) . . . . ?
C4 C5 N1 C1 -0.2(4) . . . . ?
N5 C5 N1 CO1 0.1(3) . . . . ?
C4 C5 N1 CO1 174.93(18) . . . . ?
C12 C11 N2 C15 -3.6(4) . . . . ?
C12 C11 N2 CO1 175.1(2) . . . . ?
N6 C15 N2 C11 -174.3(2) . . . . ?
C14 C15 N2 C11 2.0(4) . . . . ?
N6 C15 N2 CO1 7.1(3) . . . . ?
C14 C15 N2 CO1 -176.58(19) . . . . ?
C22 C21 N3 C25 -1.2(4) . . . . ?
C22 C21 N3 CO1 -177.3(2) . . . . ?
N7 C25 N3 C21 -175.6(2) . . . . ?
C24 C25 N3 C21 -0.3(3) . . . . ?
N7 C25 N3 CO1 0.4(3) . . . . ?
C24 C25 N3 CO1 175.69(18) . . . . ?
C32 C31 N4 C35 -2.2(4) . . . . ?
C32 C31 N4 CO1 173.8(2) . . . . ?
N8 C35 N4 C31 -178.8(2) . . . . ?
C34 C35 N4 C31 -1.4(4) . . . . ?
N8 C35 N4 CO1 5.2(3) . . . . ?
C34 C35 N4 CO1 -177.45(19) . . . . ?
N1 C5 N5 C6 -156.9(2) . . . . ?
C4 C5 N5 C6 28.6(4) . . . . ?
N1 C5 N5 CO2 27.6(3) . . . . ?
C4 C5 N5 CO2 -146.9(2) . . . . ?
N9 C6 N5 C5 -156.8(2) . . . . ?
C7 C6 N5 C5 26.9(4) . . . . ?
N9 C6 N5 CO2 18.6(3) . . . . ?
C7 C6 N5 CO2 -157.7(2) . . . . ?
N10 C16 N6 C15 -161.9(2) . . . . ?
C17 C16 N6 C15 24.1(4) . . . . ?
N10 C16 N6 CO2 21.1(3) . . . . ?
C17 C16 N6 CO2 -152.9(2) . . . . ?
N2 C15 N6 C16 -157.2(2) . . . . ?
C14 C15 N6 C16 26.7(4) . . . . ?
N2 C15 N6 CO2 19.8(3) . . . . ?
C14 C15 N6 CO2 -156.3(2) . . . . ?
N3 C25 N7 C26 -156.3(2) . . . . ?
C24 C25 N7 C26 28.7(4) . . . . ?
N3 C25 N7 CO2 25.9(3) . . . . ?
C24 C25 N7 CO2 -149.2(2) . . . . ?
N11 C26 N7 C25 -157.0(2) . . . . ?
C27 C26 N7 C25 27.7(4) . . . . ?
N11 C26 N7 CO2 20.9(3) . . . . ?
C27 C26 N7 CO2 -154.4(2) . . . . ?
N4 C35 N8 C36 -152.5(2) . . . . ?
C34 C35 N8 C36 30.2(4) . . . . ?
N4 C35 N8 CO2 19.4(3) . . . . ?
C34 C35 N8 CO2 -157.8(2) . . . . ?
N12 C36 N8 C35 -157.5(2) . . . . ?
C37 C36 N8 C35 28.7(4) . . . . ?
N12 C36 N8 CO2 30.3(3) . . . . ?
C37 C36 N8 CO2 -143.5(2) . . . . ?
C9 C10 N9 C6 -2.9(4) . . . . ?
C9 C10 N9 CO3 173.8(2) . . . . ?
N5 C6 N9 C10 -175.7(2) . . . . ?
C7 C6 N9 C10 0.8(3) . . . . ?
N5 C6 N9 CO3 7.7(3) . . . . ?
C7 C6 N9 CO3 -175.86(18) . . . . ?
C19 C20 N10 C16 -4.0(4) . . . . ?
C19 C20 N10 CO3 179.3(2) . . . . ?
N6 C16 N10 C20 -168.9(2) . . . . ?
C17 C16 N10 C20 5.5(4) . . . . ?
N6 C16 N10 CO3 7.7(3) . . . . ?
C17 C16 N10 CO3 -177.92(19) . . . . ?
C29 C30 N11 C26 -4.2(4) . . . . ?
C29 C30 N11 CO3 176.7(2) . . . . ?
N7 C26 N11 C30 -171.2(2) . . . . ?
C27 C26 N11 C30 4.3(3) . . . . ?
N7 C26 N11 CO3 8.0(3) . . . . ?
C27 C26 N11 CO3 -176.52(18) . . . . ?
C39 C40 N12 C36 1.1(4) . . . . ?
C39 C40 N12 CO3 -172.2(2) . . . . ?
N8 C36 N12 C40 -176.2(2) . . . . ?
C37 C36 N12 C40 -2.1(3) . . . . ?
N8 C36 N12 CO3 -2.8(3) . . . . ?
C37 C36 N12 CO3 171.23(19) . . . . ?
C103 C102 O100 C101 171.3(3) . . . . ?
C100 C101 O100 C102 -177.0(3) . . . . ?

_refine_diff_density_max         0.935
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.065


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: DMF, ether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_Co3_dpa4F2BF4-4CH2CL2-120K
_database_code_depnum_ccdc_archive 'CCDC 1865580'
_audit_update_record             
;
2018-09-03 deposited with the CCDC.
2018-11-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C40 H32 Co3 F2 N12, B F4, 4(C H2 Cl2)'
_chemical_formula_sum            'C44 H40 B Cl8 Co3 F6 N12'
_chemical_formula_weight         1322.08

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   11.5876(4)
_cell_length_b                   14.3205(5)
_cell_length_c                   17.8580(5)
_cell_angle_alpha                71.833(1)
_cell_angle_beta                 76.570(1)
_cell_angle_gamma                67.623(1)
_cell_volume                     2581.78(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9964
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      25.36

_exptl_crystal_description       plates
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_F_000             1328
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.152
_exptl_crystal_size_mid          0.063
_exptl_crystal_size_min          0.052
_exptl_absorpt_coefficient_mu    1.436
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6900
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            50398
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.210
_diffrn_reflns_theta_max         25.403
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9460
_reflns_number_gt                7871
_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       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_structure_solution    'SHELXS2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_publication_material  'SHELXL-2016/4 (Sheldrick, 2016)'
_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)+(0.0570P)²+7.3969P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9460
_refine_ls_number_parameters     667
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0423
_refine_ls_wR_factor_ref         0.1175
_refine_ls_wR_factor_gt          0.1116
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_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
C1 C 0.6757(3) 0.0329(3) 0.2966(2) 0.0162(8) Uani 1 1 d . . . . .
H1 H 0.611393 0.030904 0.273130 0.019 Uiso 1 1 calc R U . . .
C2 C 0.7673(3) -0.0589(3) 0.3251(2) 0.0194(8) Uani 1 1 d . . . . .
H2 H 0.765577 -0.123516 0.322219 0.023 Uiso 1 1 calc R U . . .
C3 C 0.8628(3) -0.0556(3) 0.3583(2) 0.0214(8) Uani 1 1 d . . . . .
H3 H 0.927815 -0.118111 0.377603 0.026 Uiso 1 1 calc R U . . .
C4 C 0.8625(3) 0.0389(3) 0.3630(2) 0.0186(8) Uani 1 1 d . . . . .
H4 H 0.927256 0.041947 0.385483 0.022 Uiso 1 1 calc R U . . .
C5 C 0.7655(3) 0.1307(3) 0.33417(19) 0.0126(7) Uani 1 1 d . . . . .
C6 C 0.8082(3) 0.2533(3) 0.3832(2) 0.0140(7) Uani 1 1 d . . . . .
C7 C 0.8171(3) 0.1967(3) 0.4626(2) 0.0179(8) Uani 1 1 d . . . . .
H7 H 0.796381 0.134541 0.481913 0.021 Uiso 1 1 calc R U . . .
C8 C 0.8565(3) 0.2323(3) 0.5127(2) 0.0226(9) Uani 1 1 d . . . . .
H8 H 0.862883 0.194953 0.566683 0.027 Uiso 1 1 calc R U . . .
C9 C 0.8868(4) 0.3236(3) 0.4829(2) 0.0249(9) Uani 1 1 d . . . . .
H9 H 0.915334 0.348621 0.516150 0.030 Uiso 1 1 calc R U . . .
C10 C 0.8748(4) 0.3768(3) 0.4053(2) 0.0209(8) Uani 1 1 d . . . . .
H10 H 0.894028 0.439647 0.385591 0.025 Uiso 1 1 calc R U . . .
C11 C 0.4084(3) 0.2205(3) 0.4073(2) 0.0171(8) Uani 1 1 d . . . . .
H11 H 0.396304 0.168419 0.390546 0.021 Uiso 1 1 calc R U . . .
C12 C 0.3581(4) 0.2325(3) 0.4824(2) 0.0227(9) Uani 1 1 d . . . . .
H12 H 0.309371 0.191563 0.516308 0.027 Uiso 1 1 calc R U . . .
C13 C 0.3797(4) 0.3056(3) 0.5079(2) 0.0230(9) Uani 1 1 d . . . . .
H13 H 0.347947 0.313604 0.560416 0.028 Uiso 1 1 calc R U . . .
C14 C 0.4472(3) 0.3668(3) 0.4571(2) 0.0184(8) Uani 1 1 d . . . . .
H14 H 0.462649 0.416992 0.474242 0.022 Uiso 1 1 calc R U . . .
C15 C 0.4928(3) 0.3538(3) 0.3795(2) 0.0145(7) Uani 1 1 d . . . . .
C16 C 0.5598(3) 0.5065(3) 0.3222(2) 0.0142(7) Uani 1 1 d . . . . .
C17 C 0.4509(3) 0.5824(3) 0.3472(2) 0.0199(8) Uani 1 1 d . . . . .
H17 H 0.376836 0.565659 0.371667 0.024 Uiso 1 1 calc R U . . .
C18 C 0.4529(4) 0.6821(3) 0.3357(2) 0.0228(9) Uani 1 1 d . . . . .
H18 H 0.379843 0.734491 0.351955 0.027 Uiso 1 1 calc R U . . .
C19 C 0.5625(4) 0.7049(3) 0.3000(2) 0.0228(8) Uani 1 1 d . . . . .
H19 H 0.565635 0.772697 0.292286 0.027 Uiso 1 1 calc R U . . .
C20 C 0.6659(3) 0.6280(3) 0.2764(2) 0.0180(8) Uani 1 1 d . . . . .
H20 H 0.740257 0.644007 0.251428 0.022 Uiso 1 1 calc R U . . .
C21 C 0.5829(3) 0.2097(3) 0.0998(2) 0.0165(8) Uani 1 1 d . . . . .
H21 H 0.500062 0.206835 0.116632 0.020 Uiso 1 1 calc R U . . .
C22 C 0.6430(4) 0.1890(3) 0.0279(2) 0.0201(8) Uani 1 1 d . . . . .
H22 H 0.603190 0.171082 -0.003800 0.024 Uiso 1 1 calc R U . . .
C23 C 0.7640(4) 0.1950(3) 0.0025(2) 0.0181(8) Uani 1 1 d . . . . .
H23 H 0.808532 0.179918 -0.046523 0.022 Uiso 1 1 calc R U . . .
C24 C 0.8178(3) 0.2228(3) 0.0493(2) 0.0168(8) Uani 1 1 d . . . . .
H24 H 0.898776 0.229682 0.031564 0.020 Uiso 1 1 calc R U . . .
C25 C 0.7541(3) 0.2410(3) 0.1228(2) 0.0120(7) Uani 1 1 d . . . . .
C26 C 0.9237(3) 0.2505(3) 0.1754(2) 0.0130(7) Uani 1 1 d . . . . .
C27 C 1.0196(3) 0.1635(3) 0.1557(2) 0.0159(8) Uani 1 1 d . . . . .
H27 H 1.000674 0.116258 0.137043 0.019 Uiso 1 1 calc R U . . .
C28 C 1.1423(3) 0.1467(3) 0.1635(2) 0.0189(8) Uani 1 1 d . . . . .
H28 H 1.208580 0.088725 0.149020 0.023 Uiso 1 1 calc R U . . .
C29 C 1.1685(3) 0.2146(3) 0.1926(2) 0.0174(8) Uani 1 1 d . . . . .
H29 H 1.252676 0.205311 0.196796 0.021 Uiso 1 1 calc R U . . .
C30 C 1.0698(3) 0.2956(3) 0.2153(2) 0.0149(7) Uani 1 1 d . . . . .
H30 H 1.086823 0.339970 0.238151 0.018 Uiso 1 1 calc R U . . .
C31 C 0.3109(3) 0.4024(3) 0.2091(2) 0.0145(7) Uani 1 1 d . . . . .
H31 H 0.282971 0.344553 0.235353 0.017 Uiso 1 1 calc R U . . .
C32 C 0.2238(3) 0.4967(3) 0.1796(2) 0.0174(8) Uani 1 1 d . . . . .
H32 H 0.138211 0.503269 0.182556 0.021 Uiso 1 1 calc R U . . .
C33 C 0.2643(3) 0.5824(3) 0.1451(2) 0.0192(8) Uani 1 1 d . . . . .
H33 H 0.205525 0.649186 0.126235 0.023 Uiso 1 1 calc R U . . .
C34 C 0.3894(3) 0.5702(3) 0.1384(2) 0.0171(8) Uani 1 1 d . . . . .
H34 H 0.417173 0.628563 0.115043 0.020 Uiso 1 1 calc R U . . .
C35 C 0.4758(3) 0.4716(3) 0.16602(19) 0.0129(7) Uani 1 1 d . . . . .
C36 C 0.6716(3) 0.5085(3) 0.1130(2) 0.0124(7) Uani 1 1 d . . . . .
C37 C 0.6463(3) 0.5630(3) 0.0350(2) 0.0165(8) Uani 1 1 d . . . . .
H37 H 0.574630 0.564861 0.016622 0.020 Uiso 1 1 calc R U . . .
C38 C 0.7261(4) 0.6137(3) -0.0147(2) 0.0206(8) Uani 1 1 d . . . . .
H38 H 0.708486 0.652325 -0.067056 0.025 Uiso 1 1 calc R U . . .
C39 C 0.8327(3) 0.6081(3) 0.0122(2) 0.0199(8) Uani 1 1 d . . . . .
H39 H 0.888932 0.642342 -0.021437 0.024 Uiso 1 1 calc R U . . .
C40 C 0.8546(3) 0.5521(3) 0.0883(2) 0.0163(8) Uani 1 1 d . . . . .
H40 H 0.927833 0.547407 0.106547 0.020 Uiso 1 1 calc R U . . .
C101 C 0.2907(4) 0.0277(3) 0.3527(2) 0.0214(8) Uani 1 1 d . . . . .
H10A H 0.326234 0.079496 0.313819 0.026 Uiso 1 1 calc R U . . .
H10B H 0.265470 -0.007450 0.322646 0.026 Uiso 1 1 calc R U . . .
C102 C 0.0429(4) 0.5908(3) 0.3302(2) 0.0208(8) Uani 1 1 d . . . . .
H10C H 0.017351 0.566653 0.292404 0.025 Uiso 1 1 calc R U . . .
H10D H 0.085796 0.641623 0.299114 0.025 Uiso 1 1 calc R U . . .
C104 C 0.4624(4) -0.0901(4) 0.1171(3) 0.0431(12) Uani 1 1 d . . . . .
H10E H 0.422835 -0.137836 0.157747 0.052 Uiso 1 1 calc R U . . .
H10F H 0.403223 -0.046843 0.077553 0.052 Uiso 1 1 calc R U . . .
C200 C 0.8604(5) -0.1046(4) 0.1172(3) 0.0419(12) Uani 1 1 d . . . . .
H20A H 0.771888 -0.075846 0.140438 0.050 Uiso 1 1 calc R U . . .
H20B H 0.911946 -0.076565 0.135601 0.050 Uiso 1 1 calc R U . . .
N1 N 0.6738(3) 0.1260(2) 0.30085(16) 0.0124(6) Uani 1 1 d . . . . .
N2 N 0.6362(3) 0.2338(2) 0.14754(16) 0.0124(6) Uani 1 1 d . . . . .
N3 N 0.4350(3) 0.3885(2) 0.20235(16) 0.0116(6) Uani 1 1 d . . . . .
N4 N 0.4746(3) 0.2797(2) 0.35588(17) 0.0128(6) Uani 1 1 d . . . . .
N5 N 0.7603(3) 0.2296(2) 0.33028(16) 0.0128(6) Uani 1 1 d . . . . .
N6 N 0.7975(3) 0.2728(2) 0.17286(16) 0.0125(6) Uani 1 1 d . . . . .
N7 N 0.6025(3) 0.4505(2) 0.16654(17) 0.0128(6) Uani 1 1 d . . . . .
N8 N 0.5659(3) 0.4075(2) 0.32467(17) 0.0131(6) Uani 1 1 d . . . . .
N9 N 0.8364(3) 0.3430(2) 0.35527(17) 0.0145(6) Uani 1 1 d . . . . .
N10 N 0.9489(3) 0.3151(2) 0.20653(16) 0.0123(6) Uani 1 1 d . . . . .
N11 N 0.7764(3) 0.5033(2) 0.13832(17) 0.0124(6) Uani 1 1 d . . . . .
N12 N 0.6663(3) 0.5302(2) 0.28707(16) 0.0130(6) Uani 1 1 d . . . . .
F1 F 0.43381(18) 0.18026(16) 0.25260(12) 0.0157(4) Uani 1 1 d . . . . .
F2 F 0.92906(18) 0.50008(16) 0.24333(12) 0.0168(4) Uani 1 1 d . . . . .
F100 F 0.9173(3) 0.0841(2) -0.1834(2) 0.0594(9) Uani 1 1 d . . . . .
F101 F 0.7729(3) 0.0986(2) -0.25576(17) 0.0410(7) Uani 1 1 d . . . . .
F102 F 0.7291(3) 0.2115(2) -0.17998(17) 0.0460(7) Uani 1 1 d . . . . .
F103 F 0.8659(3) 0.2196(2) -0.29225(18) 0.0530(8) Uani 1 1 d . . . . .
CL1 Cl 0.91252(13) -0.24164(11) 0.15116(9) 0.0552(4) Uani 1 1 d . . . . .
CL2 Cl 0.87108(12) -0.06398(10) 0.01292(8) 0.0469(3) Uani 1 1 d . . . . .
CL3 Cl 0.15658(10) 0.09259(9) 0.41148(6) 0.0330(3) Uani 1 1 d . . . . .
CL4 Cl 0.40748(10) -0.06577(9) 0.41165(7) 0.0380(3) Uani 1 1 d . . . . .
CL5 Cl 0.14788(10) 0.48342(9) 0.38958(6) 0.0345(3) Uani 1 1 d . . . . .
CL6 Cl -0.09239(9) 0.65220(8) 0.39033(6) 0.0301(2) Uani 1 1 d . . . . .
CL7 Cl 0.48850(11) -0.00853(10) 0.16273(7) 0.0394(3) Uani 1 1 d . . . . .
CL8 Cl 0.60267(12) -0.16377(13) 0.06948(9) 0.0556(4) Uani 1 1 d . . . . .
CO1 Co 0.54710(4) 0.25299(4) 0.25156(3) 0.01015(12) Uani 1 1 d . . . . .
CO2 Co 0.68145(4) 0.34006(4) 0.24852(3) 0.01007(12) Uani 1 1 d . . . . .
CO3 Co 0.81495(4) 0.42744(4) 0.24647(3) 0.01115(12) Uani 1 1 d . . . . .
B100 B 0.8220(4) 0.1535(4) -0.2273(3) 0.0229(10) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.349(5) . ?
C1 C2 1.374(5) . ?
C1 H1 0.9500 . ?
C2 C3 1.392(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.381(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.406(5) . ?
C4 H4 0.9500 . ?
C5 N1 1.365(4) . ?
C5 N5 1.375(5) . ?
C6 N9 1.361(5) . ?
C6 N5 1.379(4) . ?
C6 C7 1.402(5) . ?
C7 C8 1.386(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.394(6) . ?
C8 H8 0.9500 . ?
C9 C10 1.369(5) . ?
C9 H9 0.9500 . ?
C10 N9 1.359(5) . ?
C10 H10 0.9500 . ?
C11 N4 1.354(5) . ?
C11 C12 1.368(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.384(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.378(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.407(5) . ?
C14 H14 0.9500 . ?
C15 N4 1.356(5) . ?
C15 N8 1.382(4) . ?
C16 N12 1.363(4) . ?
C16 N8 1.380(5) . ?
C16 C17 1.403(5) . ?
C17 C18 1.386(6) . ?
C17 H17 0.9500 . ?
C18 C19 1.392(6) . ?
C18 H18 0.9500 . ?
C19 C20 1.371(6) . ?
C19 H19 0.9500 . ?
C20 N12 1.351(5) . ?
C20 H20 0.9500 . ?
C21 N2 1.349(4) . ?
C21 C22 1.372(5) . ?
C21 H21 0.9500 . ?
C22 C23 1.397(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.372(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.398(5) . ?
C24 H24 0.9500 . ?
C25 N2 1.368(4) . ?
C25 N6 1.377(4) . ?
C26 N10 1.361(5) . ?
C26 N6 1.381(4) . ?
C26 C27 1.397(5) . ?
C27 C28 1.383(5) . ?
C27 H27 0.9500 . ?
C28 C29 1.386(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.374(5) . ?
C29 H29 0.9500 . ?
C30 N10 1.356(4) . ?
C30 H30 0.9500 . ?
C31 N3 1.356(4) . ?
C31 C32 1.373(5) . ?
C31 H31 0.9500 . ?
C32 C33 1.392(5) . ?
C32 H32 0.9500 . ?
C33 C34 1.372(5) . ?
C33 H33 0.9500 . ?
C34 C35 1.399(5) . ?
C34 H34 0.9500 . ?
C35 N3 1.366(4) . ?
C35 N7 1.383(4) . ?
C36 N11 1.361(4) . ?
C36 N7 1.379(4) . ?
C36 C37 1.404(5) . ?
C37 C38 1.378(5) . ?
C37 H37 0.9500 . ?
C38 C39 1.392(5) . ?
C38 H38 0.9500 . ?
C39 C40 1.371(5) . ?
C39 H39 0.9500 . ?
C40 N11 1.351(4) . ?
C40 H40 0.9500 . ?
C101 CL3 1.770(4) . ?
C101 CL4 1.770(4) . ?
C101 H10A 0.9900 . ?
C101 H10B 0.9900 . ?
C102 CL5 1.768(4) . ?
C102 CL6 1.772(4) . ?
C102 H10C 0.9900 . ?
C102 H10D 0.9900 . ?
C104 CL8 1.758(5) . ?
C104 CL7 1.760(5) . ?
C104 H10E 0.9900 . ?
C104 H10F 0.9900 . ?
C200 CL2 1.760(5) . ?
C200 CL1 1.764(5) . ?
C200 H20A 0.9900 . ?
C200 H20B 0.9900 . ?
N1 CO1 1.951(3) . ?
N2 CO1 1.950(3) . ?
N3 CO1 1.942(3) . ?
N4 CO1 1.948(3) . ?
N5 CO2 1.883(3) . ?
N6 CO2 1.882(3) . ?
N7 CO2 1.886(3) . ?
N8 CO2 1.888(3) . ?
N9 CO3 1.957(3) . ?
N10 CO3 1.951(3) . ?
N11 CO3 1.958(3) . ?
N12 CO3 1.953(3) . ?
F1 CO1 1.9560(19) . ?
F2 CO3 1.9521(19) . ?
F100 B100 1.380(5) . ?
F101 B100 1.387(5) . ?
F102 B100 1.377(5) . ?
F103 B100 1.382(5) . ?
CO1 CO2 2.3191(6) . ?
CO2 CO3 2.3192(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 122.4(3) . . ?
N1 C1 H1 118.8 . . ?
C2 C1 H1 118.8 . . ?
C1 C2 C3 118.7(4) . . ?
C1 C2 H2 120.6 . . ?
C3 C2 H2 120.6 . . ?
C4 C3 C2 119.7(3) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C3 C4 C5 119.5(3) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
N1 C5 N5 115.2(3) . . ?
N1 C5 C4 119.9(3) . . ?
N5 C5 C4 124.7(3) . . ?
N9 C6 N5 115.0(3) . . ?
N9 C6 C7 120.7(3) . . ?
N5 C6 C7 124.1(3) . . ?
C8 C7 C6 119.4(4) . . ?
C8 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
C7 C8 C9 119.2(3) . . ?
C7 C8 H8 120.4 . . ?
C9 C8 H8 120.4 . . ?
C10 C9 C8 119.1(3) . . ?
C10 C9 H9 120.4 . . ?
C8 C9 H9 120.4 . . ?
N9 C10 C9 122.5(4) . . ?
N9 C10 H10 118.8 . . ?
C9 C10 H10 118.8 . . ?
N4 C11 C12 122.7(3) . . ?
N4 C11 H11 118.7 . . ?
C12 C11 H11 118.7 . . ?
C11 C12 C13 118.7(3) . . ?
C11 C12 H12 120.6 . . ?
C13 C12 H12 120.6 . . ?
C14 C13 C12 120.0(3) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C13 C14 C15 118.9(3) . . ?
C13 C14 H14 120.5 . . ?
C15 C14 H14 120.5 . . ?
N4 C15 N8 115.2(3) . . ?
N4 C15 C14 120.6(3) . . ?
N8 C15 C14 124.0(3) . . ?
N12 C16 N8 114.9(3) . . ?
N12 C16 C17 120.7(3) . . ?
N8 C16 C17 124.2(3) . . ?
C18 C17 C16 119.1(3) . . ?
C18 C17 H17 120.4 . . ?
C16 C17 H17 120.4 . . ?
C17 C18 C19 119.6(4) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 H18 120.2 . . ?
C20 C19 C18 118.8(4) . . ?
C20 C19 H19 120.6 . . ?
C18 C19 H19 120.6 . . ?
N12 C20 C19 122.7(3) . . ?
N12 C20 H20 118.7 . . ?
C19 C20 H20 118.7 . . ?
N2 C21 C22 123.0(3) . . ?
N2 C21 H21 118.5 . . ?
C22 C21 H21 118.5 . . ?
C21 C22 C23 118.5(3) . . ?
C21 C22 H22 120.8 . . ?
C23 C22 H22 120.8 . . ?
C24 C23 C22 119.2(3) . . ?
C24 C23 H23 120.4 . . ?
C22 C23 H23 120.4 . . ?
C23 C24 C25 120.3(3) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 H24 119.8 . . ?
N2 C25 N6 114.9(3) . . ?
N2 C25 C24 120.0(3) . . ?
N6 C25 C24 125.0(3) . . ?
N10 C26 N6 114.8(3) . . ?
N10 C26 C27 120.7(3) . . ?
N6 C26 C27 124.3(3) . . ?
C28 C27 C26 119.3(3) . . ?
C28 C27 H27 120.3 . . ?
C26 C27 H27 120.3 . . ?
C27 C28 C29 119.9(4) . . ?
C27 C28 H28 120.0 . . ?
C29 C28 H28 120.0 . . ?
C30 C29 C28 118.3(3) . . ?
C30 C29 H29 120.8 . . ?
C28 C29 H29 120.8 . . ?
N10 C30 C29 122.8(3) . . ?
N10 C30 H30 118.6 . . ?
C29 C30 H30 118.6 . . ?
N3 C31 C32 122.8(3) . . ?
N3 C31 H31 118.6 . . ?
C32 C31 H31 118.6 . . ?
C31 C32 C33 118.2(3) . . ?
C31 C32 H32 120.9 . . ?
C33 C32 H32 120.9 . . ?
C34 C33 C32 119.9(3) . . ?
C34 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
C33 C34 C35 119.9(3) . . ?
C33 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
N3 C35 N7 114.5(3) . . ?
N3 C35 C34 120.0(3) . . ?
N7 C35 C34 125.2(3) . . ?
N11 C36 N7 115.0(3) . . ?
N11 C36 C37 120.0(3) . . ?
N7 C36 C37 124.8(3) . . ?
C38 C37 C36 119.6(3) . . ?
C38 C37 H37 120.2 . . ?
C36 C37 H37 120.2 . . ?
C37 C38 C39 119.7(3) . . ?
C37 C38 H38 120.1 . . ?
C39 C38 H38 120.1 . . ?
C40 C39 C38 118.4(3) . . ?
C40 C39 H39 120.8 . . ?
C38 C39 H39 120.8 . . ?
N11 C40 C39 122.7(3) . . ?
N11 C40 H40 118.6 . . ?
C39 C40 H40 118.6 . . ?
CL3 C101 CL4 111.6(2) . . ?
CL3 C101 H10A 109.3 . . ?
CL4 C101 H10A 109.3 . . ?
CL3 C101 H10B 109.3 . . ?
CL4 C101 H10B 109.3 . . ?
H10A C101 H10B 108.0 . . ?
CL5 C102 CL6 110.6(2) . . ?
CL5 C102 H10C 109.5 . . ?
CL6 C102 H10C 109.5 . . ?
CL5 C102 H10D 109.5 . . ?
CL6 C102 H10D 109.5 . . ?
H10C C102 H10D 108.1 . . ?
CL8 C104 CL7 112.1(3) . . ?
CL8 C104 H10E 109.2 . . ?
CL7 C104 H10E 109.2 . . ?
CL8 C104 H10F 109.2 . . ?
CL7 C104 H10F 109.2 . . ?
H10E C104 H10F 107.9 . . ?
CL2 C200 CL1 111.7(3) . . ?
CL2 C200 H20A 109.3 . . ?
CL1 C200 H20A 109.3 . . ?
CL2 C200 H20B 109.3 . . ?
CL1 C200 H20B 109.3 . . ?
H20A C200 H20B 107.9 . . ?
C1 N1 C5 119.7(3) . . ?
C1 N1 CO1 119.3(2) . . ?
C5 N1 CO1 120.8(2) . . ?
C21 N2 C25 119.0(3) . . ?
C21 N2 CO1 119.8(2) . . ?
C25 N2 CO1 121.3(2) . . ?
C31 N3 C35 119.1(3) . . ?
C31 N3 CO1 118.7(2) . . ?
C35 N3 CO1 122.0(2) . . ?
C11 N4 C15 119.0(3) . . ?
C11 N4 CO1 119.4(2) . . ?
C15 N4 CO1 121.5(2) . . ?
C5 N5 C6 124.0(3) . . ?
C5 N5 CO2 118.2(2) . . ?
C6 N5 CO2 117.8(2) . . ?
C25 N6 C26 123.5(3) . . ?
C25 N6 CO2 119.1(2) . . ?
C26 N6 CO2 117.2(2) . . ?
C36 N7 C35 123.6(3) . . ?
C36 N7 CO2 118.8(2) . . ?
C35 N7 CO2 117.5(2) . . ?
C16 N8 C15 124.3(3) . . ?
C16 N8 CO2 118.3(2) . . ?
C15 N8 CO2 117.4(2) . . ?
C10 N9 C6 119.1(3) . . ?
C10 N9 CO3 119.5(3) . . ?
C6 N9 CO3 121.3(2) . . ?
C30 N10 C26 118.8(3) . . ?
C30 N10 CO3 119.3(2) . . ?
C26 N10 CO3 121.7(2) . . ?
C40 N11 C36 119.5(3) . . ?
C40 N11 CO3 119.4(2) . . ?
C36 N11 CO3 121.1(2) . . ?
C20 N12 C16 119.2(3) . . ?
C20 N12 CO3 119.9(2) . . ?
C16 N12 CO3 120.9(2) . . ?
N3 CO1 N4 89.72(12) . . ?
N3 CO1 N2 90.64(12) . . ?
N4 CO1 N2 172.47(12) . . ?
N3 CO1 N1 172.86(12) . . ?
N4 CO1 N1 89.72(12) . . ?
N2 CO1 N1 88.98(12) . . ?
N3 CO1 F1 93.42(10) . . ?
N4 CO1 F1 94.42(10) . . ?
N2 CO1 F1 93.07(10) . . ?
N1 CO1 F1 93.72(10) . . ?
N3 CO1 CO2 86.17(8) . . ?
N4 CO1 CO2 86.21(8) . . ?
N2 CO1 CO2 86.31(8) . . ?
N1 CO1 CO2 86.69(8) . . ?
F1 CO1 CO2 179.25(6) . . ?
N6 CO2 N5 89.49(12) . . ?
N6 CO2 N7 90.45(12) . . ?
N5 CO2 N7 179.90(13) . . ?
N6 CO2 N8 179.64(12) . . ?
N5 CO2 N8 90.30(12) . . ?
N7 CO2 N8 89.76(13) . . ?
N6 CO2 CO1 90.24(9) . . ?
N5 CO2 CO1 89.71(9) . . ?
N7 CO2 CO1 90.21(9) . . ?
N8 CO2 CO1 90.05(9) . . ?
N6 CO2 CO3 90.20(9) . . ?
N5 CO2 CO3 90.15(9) . . ?
N7 CO2 CO3 89.93(9) . . ?
N8 CO2 CO3 89.50(9) . . ?
CO1 CO2 CO3 179.53(3) . . ?
N10 CO3 F2 93.27(10) . . ?
N10 CO3 N12 172.60(12) . . ?
F2 CO3 N12 94.13(10) . . ?
N10 CO3 N9 89.52(12) . . ?
F2 CO3 N9 94.54(10) . . ?
N12 CO3 N9 89.76(12) . . ?
N10 CO3 N11 90.66(12) . . ?
F2 CO3 N11 93.22(10) . . ?
N12 CO3 N11 89.06(12) . . ?
N9 CO3 N11 172.21(12) . . ?
N10 CO3 CO2 85.92(8) . . ?
F2 CO3 CO2 179.08(7) . . ?
N12 CO3 CO2 86.67(8) . . ?
N9 CO3 CO2 85.90(9) . . ?
N11 CO3 CO2 86.34(8) . . ?
F102 B100 F100 109.5(4) . . ?
F102 B100 F103 109.3(4) . . ?
F100 B100 F103 111.4(4) . . ?
F102 B100 F101 109.9(4) . . ?
F100 B100 F101 109.2(4) . . ?
F103 B100 F101 107.4(4) . . ?

_refine_diff_density_max         1.155
_refine_diff_density_min         -0.877
_refine_diff_density_rms         0.095

####################################################################### 
# 
# 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_2-Et2O-120K
_database_code_depnum_ccdc_archive 'CCDC 1865581'
_audit_update_record             
;
2018-09-03 deposited with the CCDC.
2018-11-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C40 H32 Cl2 Co3 N12, C4 H10 O'
_chemical_formula_sum            'C44 H42 Cl2 Co3 N12 O'
_chemical_formula_weight         1002.58

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   15.8217(14)
_cell_length_b                   15.6581(12)
_cell_length_c                   16.9215(14)
_cell_angle_alpha                90
_cell_angle_beta                 98.916(3)
_cell_angle_gamma                90
_cell_volume                     4141.4(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9993
_cell_measurement_theta_min      2.61
_cell_measurement_theta_max      30.05

_exptl_crystal_description       block
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_F_000             2052
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    1.370
_shelx_estimated_absorpt_T_min   0.800
_shelx_estimated_absorpt_T_max   0.842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6764
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_process_details   '(SADABS; Bruker, 2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            68162
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.093
_diffrn_reflns_theta_max         30.081
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             12158
_reflns_number_gt                10531
_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       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_structure_solution    'SHELXS2013 (Sheldrick, 2008)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_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)+(0.0268P)²+2.9399P] 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_number_reflns         12158
_refine_ls_number_parameters     559
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0246
_refine_ls_wR_factor_ref         0.0622
_refine_ls_wR_factor_gt          0.0587
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.006
_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
C1 C 0.42563(8) -0.19324(8) 0.29263(8) 0.0138(2) Uani 1 1 d . . . . .
H1 H 0.441810 -0.210902 0.243384 0.017 Uiso 1 1 calc R U . . .
C2 C 0.44893(9) -0.24387(8) 0.35876(8) 0.0169(3) Uani 1 1 d . . . . .
H2 H 0.483013 -0.293393 0.355939 0.020 Uiso 1 1 calc R U . . .
C3 C 0.42115(9) -0.22060(8) 0.43036(8) 0.0175(3) Uani 1 1 d . . . . .
H3 H 0.435238 -0.254709 0.476977 0.021 Uiso 1 1 calc R U . . .
C4 C 0.37322(9) -0.14772(8) 0.43220(8) 0.0151(2) Uani 1 1 d . . . . .
H4 H 0.352177 -0.132417 0.479874 0.018 Uiso 1 1 calc R U . . .
C5 C 0.35493(8) -0.09519(7) 0.36353(7) 0.0106(2) Uani 1 1 d . . . . .
C6 C 0.30697(8) 0.02918(7) 0.42656(7) 0.0109(2) Uani 1 1 d . . . . .
C7 C 0.37471(9) 0.03496(8) 0.49100(8) 0.0160(2) Uani 1 1 d . . . . .
H7 H 0.423307 -0.000996 0.492535 0.019 Uiso 1 1 calc R U . . .
C8 C 0.37071(10) 0.09256(8) 0.55175(8) 0.0182(3) Uani 1 1 d . . . . .
H8 H 0.416608 0.097157 0.594949 0.022 Uiso 1 1 calc R U . . .
C9 C 0.29853(10) 0.14402(8) 0.54910(8) 0.0188(3) Uani 1 1 d . . . . .
H9 H 0.293386 0.182910 0.591177 0.023 Uiso 1 1 calc R U . . .
C10 C 0.23481(9) 0.13720(8) 0.48407(8) 0.0147(2) Uani 1 1 d . . . . .
H10 H 0.186201 0.173241 0.481853 0.018 Uiso 1 1 calc R U . . .
C11 C 0.27066(9) -0.15574(8) 0.07521(8) 0.0143(2) Uani 1 1 d . . . . .
H11 H 0.321879 -0.148402 0.053190 0.017 Uiso 1 1 calc R U . . .
C12 C 0.20668(9) -0.20488(8) 0.03366(8) 0.0163(3) Uani 1 1 d . . . . .
H12 H 0.214260 -0.232356 -0.014806 0.020 Uiso 1 1 calc R U . . .
C13 C 0.13021(9) -0.21332(8) 0.06464(8) 0.0154(2) Uani 1 1 d . . . . .
H13 H 0.084694 -0.246776 0.037421 0.018 Uiso 1 1 calc R U . . .
C14 C 0.12158(8) -0.17265(8) 0.13497(7) 0.0131(2) Uani 1 1 d . . . . .
H14 H 0.069238 -0.176629 0.155683 0.016 Uiso 1 1 calc R U . . .
C15 C 0.19022(8) -0.12500(7) 0.17651(7) 0.0102(2) Uani 1 1 d . . . . .
C16 C 0.13288(8) -0.09847(7) 0.29829(7) 0.0095(2) Uani 1 1 d . . . . .
C17 C 0.10103(9) -0.18124(8) 0.30978(8) 0.0135(2) Uani 1 1 d . . . . .
H17 H 0.115449 -0.227517 0.278087 0.016 Uiso 1 1 calc R U . . .
C18 C 0.04923(9) -0.19481(8) 0.36677(8) 0.0155(2) Uani 1 1 d . . . . .
H18 H 0.026142 -0.249923 0.373263 0.019 Uiso 1 1 calc R U . . .
C19 C 0.03077(9) -0.12715(8) 0.41500(8) 0.0158(2) Uani 1 1 d . . . . .
H19 H -0.004813 -0.135138 0.454752 0.019 Uiso 1 1 calc R U . . .
C20 C 0.06564(8) -0.04850(8) 0.40328(7) 0.0128(2) Uani 1 1 d . . . . .
H20 H 0.055107 -0.002856 0.437432 0.015 Uiso 1 1 calc R U . . .
C21 C 0.38420(9) 0.06378(8) 0.06467(8) 0.0142(2) Uani 1 1 d . . . . .
H21 H 0.439678 0.039146 0.075113 0.017 Uiso 1 1 calc R U . . .
C22 C 0.36585(9) 0.11805(8) 0.00030(8) 0.0177(3) Uani 1 1 d . . . . .
H22 H 0.406945 0.129144 -0.033820 0.021 Uiso 1 1 calc R U . . .
C23 C 0.28556(9) 0.15619(8) -0.01343(8) 0.0172(3) Uani 1 1 d . . . . .
H23 H 0.270235 0.192565 -0.058293 0.021 Uiso 1 1 calc R U . . .
C24 C 0.22833(9) 0.14073(8) 0.03868(8) 0.0145(2) Uani 1 1 d . . . . .
H24 H 0.174494 0.168888 0.031255 0.017 Uiso 1 1 calc R U . . .
C25 C 0.24939(8) 0.08331(7) 0.10292(7) 0.0104(2) Uani 1 1 d . . . . .
C26 C 0.11236(8) 0.07493(7) 0.15048(7) 0.0105(2) Uani 1 1 d . . . . .
C27 C 0.05650(9) 0.07419(8) 0.07664(8) 0.0144(2) Uani 1 1 d . . . . .
H27 H 0.079180 0.076751 0.027891 0.017 Uiso 1 1 calc R U . . .
C28 C -0.03061(9) 0.06977(8) 0.07517(8) 0.0167(3) Uani 1 1 d . . . . .
H28 H -0.068039 0.069594 0.025514 0.020 Uiso 1 1 calc R U . . .
C29 C -0.06380(9) 0.06554(9) 0.14676(8) 0.0174(3) Uani 1 1 d . . . . .
H29 H -0.123551 0.059897 0.146957 0.021 Uiso 1 1 calc R U . . .
C30 C -0.00724(8) 0.06980(8) 0.21702(8) 0.0140(2) Uani 1 1 d . . . . .
H30 H -0.029506 0.067344 0.265984 0.017 Uiso 1 1 calc R U . . .
C31 C 0.52320(8) 0.02224(8) 0.27532(8) 0.0144(2) Uani 1 1 d . . . . .
H31 H 0.543172 -0.029052 0.254578 0.017 Uiso 1 1 calc R U . . .
C32 C 0.58182(9) 0.07494(9) 0.31962(8) 0.0163(2) Uani 1 1 d . . . . .
H32 H 0.640996 0.061086 0.328188 0.020 Uiso 1 1 calc R U . . .
C33 C 0.55237(9) 0.14924(8) 0.35168(8) 0.0154(2) Uani 1 1 d . . . . .
H33 H 0.591475 0.186949 0.382445 0.018 Uiso 1 1 calc R U . . .
C34 C 0.46642(8) 0.16759(8) 0.33851(8) 0.0133(2) Uani 1 1 d . . . . .
H34 H 0.445702 0.217330 0.361330 0.016 Uiso 1 1 calc R U . . .
C35 C 0.40886(8) 0.11234(7) 0.29095(7) 0.0105(2) Uani 1 1 d . . . . .
C36 C 0.28160(8) 0.19940(7) 0.27930(7) 0.0104(2) Uani 1 1 d . . . . .
C37 C 0.31672(9) 0.27899(8) 0.26187(8) 0.0141(2) Uani 1 1 d . . . . .
H37 H 0.374707 0.282377 0.253743 0.017 Uiso 1 1 calc R U . . .
C38 C 0.26706(9) 0.35158(8) 0.25666(8) 0.0173(3) Uani 1 1 d . . . . .
H38 H 0.290738 0.405344 0.245993 0.021 Uiso 1 1 calc R U . . .
C39 C 0.18167(9) 0.34527(8) 0.26722(8) 0.0180(3) Uani 1 1 d . . . . .
H39 H 0.145758 0.394213 0.262437 0.022 Uiso 1 1 calc R U . . .
C40 C 0.15049(9) 0.26659(8) 0.28471(8) 0.0146(2) Uani 1 1 d . . . . .
H40 H 0.091955 0.262277 0.290819 0.018 Uiso 1 1 calc R U . . .
C100 C 0.16728(10) 0.54982(11) 0.11465(10) 0.0264(3) Uani 1 1 d . . . . .
H10H H 0.140524 0.582303 0.067874 0.040 Uiso 1 1 calc R U . . .
H10I H 0.216725 0.518433 0.101209 0.040 Uiso 1 1 calc R U . . .
H10J H 0.125741 0.509387 0.130580 0.040 Uiso 1 1 calc R U . . .
C101 C 0.19632(9) 0.61044(9) 0.18287(8) 0.0180(3) Uani 1 1 d . . . . .
H10F H 0.238010 0.651781 0.167072 0.022 Uiso 1 1 calc R U . . .
H10G H 0.146748 0.642707 0.196533 0.022 Uiso 1 1 calc R U . . .
C102 C 0.27678(10) 0.61578(9) 0.31252(8) 0.0196(3) Uani 1 1 d . . . . .
H10D H 0.234457 0.653216 0.332740 0.023 Uiso 1 1 calc R U . . .
H10E H 0.319499 0.652337 0.291841 0.023 Uiso 1 1 calc R U . . .
C103 C 0.32038(10) 0.55970(10) 0.37907(9) 0.0252(3) Uani 1 1 d . . . . .
H10A H 0.349474 0.595516 0.422444 0.038 Uiso 1 1 calc R U . . .
H10B H 0.277621 0.524001 0.399388 0.038 Uiso 1 1 calc R U . . .
H10C H 0.362380 0.523125 0.358626 0.038 Uiso 1 1 calc R U . . .
Co1 Co 0.35923(2) -0.04334(2) 0.19911(2) 0.00878(4) Uani 1 1 d . . . . .
Co2 Co 0.25386(2) 0.02229(2) 0.26012(2) 0.00791(4) Uani 1 1 d . . . . .
Co3 Co 0.15104(2) 0.08455(2) 0.32556(2) 0.00823(4) Uani 1 1 d . . . . .
N1 N 0.38089(7) -0.11953(6) 0.29367(6) 0.01038(19) Uani 1 1 d . . . . .
N2 N 0.43851(7) 0.03962(6) 0.25973(6) 0.01103(19) Uani 1 1 d . . . . .
N3 N 0.32725(7) 0.04358(6) 0.11401(6) 0.01074(19) Uani 1 1 d . . . . .
N4 N 0.26470(7) -0.11716(6) 0.14592(6) 0.01022(19) Uani 1 1 d . . . . .
N5 N 0.30859(7) -0.02144(6) 0.36070(6) 0.01020(19) Uani 1 1 d . . . . .
N6 N 0.32215(7) 0.12248(6) 0.27762(6) 0.00985(19) Uani 1 1 d . . . . .
N7 N 0.19917(7) 0.06645(6) 0.16034(6) 0.00999(19) Uani 1 1 d . . . . .
N8 N 0.18617(7) -0.07889(6) 0.24451(6) 0.00969(19) Uani 1 1 d . . . . .
N9 N 0.23778(7) 0.08178(6) 0.42307(6) 0.01054(19) Uani 1 1 d . . . . .
N10 N 0.19918(7) 0.19487(6) 0.29368(6) 0.01023(19) Uani 1 1 d . . . . .
N11 N 0.07842(7) 0.07732(6) 0.22025(6) 0.01042(19) Uani 1 1 d . . . . .
N12 N 0.11417(7) -0.03273(6) 0.34561(6) 0.00982(19) Uani 1 1 d . . . . .
O100 O 0.23499(6) 0.56226(6) 0.25024(6) 0.01675(19) Uani 1 1 d . . . . .
Cl1 Cl 0.46890(2) -0.11240(2) 0.13032(2) 0.01584(6) Uani 1 1 d . . . . .
Cl2 Cl 0.04258(2) 0.15634(2) 0.38995(2) 0.01474(6) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.3555(16) . ?
C1 C2 1.3742(18) . ?
C1 H1 0.9500 . ?
C2 C3 1.3997(19) . ?
C2 H2 0.9500 . ?
C3 C4 1.3732(18) . ?
C3 H3 0.9500 . ?
C4 C5 1.4164(17) . ?
C4 H4 0.9500 . ?
C5 N1 1.3645(15) . ?
C5 N5 1.3647(15) . ?
C6 N9 1.3639(16) . ?
C6 N5 1.3709(15) . ?
C6 C7 1.4085(18) . ?
C7 C8 1.3764(18) . ?
C7 H7 0.9500 . ?
C8 C9 1.393(2) . ?
C8 H8 0.9500 . ?
C9 C10 1.3763(19) . ?
C9 H9 0.9500 . ?
C10 N9 1.3549(15) . ?
C10 H10 0.9500 . ?
C11 N4 1.3565(15) . ?
C11 C12 1.3749(19) . ?
C11 H11 0.9500 . ?
C12 C13 1.3974(19) . ?
C12 H12 0.9500 . ?
C13 C14 1.3750(17) . ?
C13 H13 0.9500 . ?
C14 C15 1.4119(17) . ?
C14 H14 0.9500 . ?
C15 N4 1.3642(16) . ?
C15 N8 1.3683(15) . ?
C16 N12 1.3646(15) . ?
C16 N8 1.3677(15) . ?
C16 C17 1.4149(16) . ?
C17 C18 1.3755(17) . ?
C17 H17 0.9500 . ?
C18 C19 1.3956(18) . ?
C18 H18 0.9500 . ?
C19 C20 1.3762(18) . ?
C19 H19 0.9500 . ?
C20 N12 1.3546(15) . ?
C20 H20 0.9500 . ?
C21 N3 1.3571(16) . ?
C21 C22 1.3765(18) . ?
C21 H21 0.9500 . ?
C22 C23 1.390(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.3797(18) . ?
C23 H23 0.9500 . ?
C24 C25 1.4102(17) . ?
C24 H24 0.9500 . ?
C25 N3 1.3667(16) . ?
C25 N7 1.3727(15) . ?
C26 N7 1.3642(16) . ?
C26 N11 1.3711(15) . ?
C26 C27 1.4143(18) . ?
C27 C28 1.3764(19) . ?
C27 H27 0.9500 . ?
C28 C29 1.3945(19) . ?
C28 H28 0.9500 . ?
C29 C30 1.3744(19) . ?
C29 H29 0.9500 . ?
C30 N11 1.3530(16) . ?
C30 H30 0.9500 . ?
C31 N2 1.3526(17) . ?
C31 C32 1.3739(19) . ?
C31 H31 0.9500 . ?
C32 C33 1.3941(19) . ?
C32 H32 0.9500 . ?
C33 C34 1.3738(19) . ?
C33 H33 0.9500 . ?
C34 C35 1.4136(17) . ?
C34 H34 0.9500 . ?
C35 N6 1.3647(16) . ?
C35 N2 1.3684(15) . ?
C36 N10 1.3650(16) . ?
C36 N6 1.3669(15) . ?
C36 C37 1.4141(16) . ?
C37 C38 1.3768(18) . ?
C37 H37 0.9500 . ?
C38 C39 1.394(2) . ?
C38 H38 0.9500 . ?
C39 C40 1.3762(18) . ?
C39 H39 0.9500 . ?
C40 N10 1.3570(16) . ?
C40 H40 0.9500 . ?
C100 C101 1.510(2) . ?
C100 H10H 0.9800 . ?
C100 H10I 0.9800 . ?
C100 H10J 0.9800 . ?
C101 O100 1.4237(16) . ?
C101 H10F 0.9900 . ?
C101 H10G 0.9900 . ?
C102 O100 1.4263(17) . ?
C102 C103 1.508(2) . ?
C102 H10D 0.9900 . ?
C102 H10E 0.9900 . ?
C103 H10A 0.9800 . ?
C103 H10B 0.9800 . ?
C103 H10C 0.9800 . ?
Co1 N2 1.9784(11) . ?
Co1 N1 1.9827(10) . ?
Co1 N3 1.9891(11) . ?
Co1 N4 1.9915(11) . ?
Co1 Co2 2.3312(3) . ?
Co1 Cl1 2.4823(4) . ?
Co2 N6 1.9019(10) . ?
Co2 N7 1.9039(10) . ?
Co2 N8 1.9076(10) . ?
Co2 N5 1.9128(10) . ?
Co2 Co3 2.3198(3) . ?
Co3 N11 1.9682(11) . ?
Co3 N12 1.9721(10) . ?
Co3 N9 1.9763(11) . ?
Co3 N10 1.9955(10) . ?
Co3 Cl2 2.4443(4) . ?

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
N1 C1 C2 123.73(12) . . ?
N1 C1 H1 118.1 . . ?
C2 C1 H1 118.1 . . ?
C1 C2 C3 118.31(12) . . ?
C1 C2 H2 120.8 . . ?
C3 C2 H2 120.8 . . ?
C4 C3 C2 118.97(12) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C3 C4 C5 120.50(12) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
N1 C5 N5 115.99(11) . . ?
N1 C5 C4 119.85(11) . . ?
N5 C5 C4 124.09(11) . . ?
N9 C6 N5 115.47(11) . . ?
N9 C6 C7 120.27(11) . . ?
N5 C6 C7 123.95(12) . . ?
C8 C7 C6 120.18(13) . . ?
C8 C7 H7 119.9 . . ?
C6 C7 H7 119.9 . . ?
C7 C8 C9 119.18(13) . . ?
C7 C8 H8 120.4 . . ?
C9 C8 H8 120.4 . . ?
C10 C9 C8 118.44(12) . . ?
C10 C9 H9 120.8 . . ?
C8 C9 H9 120.8 . . ?
N9 C10 C9 123.45(12) . . ?
N9 C10 H10 118.3 . . ?
C9 C10 H10 118.3 . . ?
N4 C11 C12 123.64(12) . . ?
N4 C11 H11 118.2 . . ?
C12 C11 H11 118.2 . . ?
C11 C12 C13 118.20(12) . . ?
C11 C12 H12 120.9 . . ?
C13 C12 H12 120.9 . . ?
C14 C13 C12 119.27(12) . . ?
C14 C13 H13 120.4 . . ?
C12 C13 H13 120.4 . . ?
C13 C14 C15 120.25(12) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
N4 C15 N8 115.31(11) . . ?
N4 C15 C14 120.10(11) . . ?
N8 C15 C14 124.40(11) . . ?
N12 C16 N8 115.69(10) . . ?
N12 C16 C17 119.74(11) . . ?
N8 C16 C17 124.49(11) . . ?
C18 C17 C16 120.10(11) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C17 C18 C19 119.61(12) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 H18 120.2 . . ?
C20 C19 C18 118.04(12) . . ?
C20 C19 H19 121.0 . . ?
C18 C19 H19 121.0 . . ?
N12 C20 C19 123.48(12) . . ?
N12 C20 H20 118.3 . . ?
C19 C20 H20 118.3 . . ?
N3 C21 C22 123.51(12) . . ?
N3 C21 H21 118.2 . . ?
C22 C21 H21 118.2 . . ?
C21 C22 C23 118.19(12) . . ?
C21 C22 H22 120.9 . . ?
C23 C22 H22 120.9 . . ?
C24 C23 C22 119.41(12) . . ?
C24 C23 H23 120.3 . . ?
C22 C23 H23 120.3 . . ?
C23 C24 C25 120.29(12) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
N3 C25 N7 115.06(10) . . ?
N3 C25 C24 119.75(11) . . ?
N7 C25 C24 125.07(11) . . ?
N7 C26 N11 114.75(11) . . ?
N7 C26 C27 125.92(11) . . ?
N11 C26 C27 119.11(11) . . ?
C28 C27 C26 120.21(12) . . ?
C28 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
C27 C28 C29 119.84(12) . . ?
C27 C28 H28 120.1 . . ?
C29 C28 H28 120.1 . . ?
C30 C29 C28 117.83(12) . . ?
C30 C29 H29 121.1 . . ?
C28 C29 H29 121.1 . . ?
N11 C30 C29 123.57(12) . . ?
N11 C30 H30 118.2 . . ?
C29 C30 H30 118.2 . . ?
N2 C31 C32 123.38(12) . . ?
N2 C31 H31 118.3 . . ?
C32 C31 H31 118.3 . . ?
C31 C32 C33 118.39(12) . . ?
C31 C32 H32 120.8 . . ?
C33 C32 H32 120.8 . . ?
C34 C33 C32 119.57(12) . . ?
C34 C33 H33 120.2 . . ?
C32 C33 H33 120.2 . . ?
C33 C34 C35 119.91(12) . . ?
C33 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
N6 C35 N2 115.40(11) . . ?
N6 C35 C34 124.43(11) . . ?
N2 C35 C34 119.99(11) . . ?
N10 C36 N6 114.99(10) . . ?
N10 C36 C37 120.01(11) . . ?
N6 C36 C37 124.84(11) . . ?
C38 C37 C36 120.14(12) . . ?
C38 C37 H37 119.9 . . ?
C36 C37 H37 119.9 . . ?
C37 C38 C39 119.22(12) . . ?
C37 C38 H38 120.4 . . ?
C39 C38 H38 120.4 . . ?
C40 C39 C38 118.56(12) . . ?
C40 C39 H39 120.7 . . ?
C38 C39 H39 120.7 . . ?
N10 C40 C39 123.27(12) . . ?
N10 C40 H40 118.4 . . ?
C39 C40 H40 118.4 . . ?
C101 C100 H10H 109.5 . . ?
C101 C100 H10I 109.5 . . ?
H10H C100 H10I 109.5 . . ?
C101 C100 H10J 109.5 . . ?
H10H C100 H10J 109.5 . . ?
H10I C100 H10J 109.5 . . ?
O100 C101 C100 108.73(11) . . ?
O100 C101 H10F 109.9 . . ?
C100 C101 H10F 109.9 . . ?
O100 C101 H10G 109.9 . . ?
C100 C101 H10G 109.9 . . ?
H10F C101 H10G 108.3 . . ?
O100 C102 C103 108.39(11) . . ?
O100 C102 H10D 110.0 . . ?
C103 C102 H10D 110.0 . . ?
O100 C102 H10E 110.0 . . ?
C103 C102 H10E 110.0 . . ?
H10D C102 H10E 108.4 . . ?
C102 C103 H10A 109.5 . . ?
C102 C103 H10B 109.5 . . ?
H10A C103 H10B 109.5 . . ?
C102 C103 H10C 109.5 . . ?
H10A C103 H10C 109.5 . . ?
H10B C103 H10C 109.5 . . ?
N2 Co1 N1 87.72(4) . . ?
N2 Co1 N3 89.76(4) . . ?
N1 Co1 N3 171.41(4) . . ?
N2 Co1 N4 170.70(4) . . ?
N1 Co1 N4 92.25(4) . . ?
N3 Co1 N4 88.91(4) . . ?
N2 Co1 Co2 85.44(3) . . ?
N1 Co1 Co2 87.36(3) . . ?
N3 Co1 Co2 84.26(3) . . ?
N4 Co1 Co2 85.27(3) . . ?
N2 Co1 Cl1 95.51(3) . . ?
N1 Co1 Cl1 94.04(3) . . ?
N3 Co1 Cl1 94.38(3) . . ?
N4 Co1 Cl1 93.77(3) . . ?
Co2 Co1 Cl1 178.340(12) . . ?
N6 Co2 N7 90.44(4) . . ?
N6 Co2 N8 178.95(5) . . ?
N7 Co2 N8 90.61(4) . . ?
N6 Co2 N5 89.36(4) . . ?
N7 Co2 N5 179.64(5) . . ?
N8 Co2 N5 89.59(4) . . ?
N6 Co2 Co3 90.15(3) . . ?
N7 Co2 Co3 90.85(3) . . ?
N8 Co2 Co3 89.71(3) . . ?
N5 Co2 Co3 88.85(3) . . ?
N6 Co2 Co1 90.26(3) . . ?
N7 Co2 Co1 91.45(3) . . ?
N8 Co2 Co1 89.84(3) . . ?
N5 Co2 Co1 88.85(3) . . ?
Co3 Co2 Co1 177.666(10) . . ?
N11 Co3 N12 87.45(4) . . ?
N11 Co3 N9 170.76(4) . . ?
N12 Co3 N9 91.23(4) . . ?
N11 Co3 N10 89.93(4) . . ?
N12 Co3 N10 171.12(4) . . ?
N9 Co3 N10 90.00(4) . . ?
N11 Co3 Co2 84.13(3) . . ?
N12 Co3 Co2 86.49(3) . . ?
N9 Co3 Co2 86.66(3) . . ?
N10 Co3 Co2 84.81(3) . . ?
N11 Co3 Cl2 94.50(3) . . ?
N12 Co3 Cl2 96.01(3) . . ?
N9 Co3 Cl2 94.73(3) . . ?
N10 Co3 Cl2 92.64(3) . . ?
Co2 Co3 Cl2 177.100(11) . . ?
C1 N1 C5 118.49(11) . . ?
C1 N1 Co1 121.81(9) . . ?
C5 N1 Co1 119.57(8) . . ?
C31 N2 C35 118.73(11) . . ?
C31 N2 Co1 119.89(9) . . ?
C35 N2 Co1 121.25(8) . . ?
C21 N3 C25 118.66(11) . . ?
C21 N3 Co1 119.10(9) . . ?
C25 N3 Co1 122.24(8) . . ?
C11 N4 C15 118.48(11) . . ?
C11 N4 Co1 120.48(9) . . ?
C15 N4 Co1 120.87(8) . . ?
C5 N5 C6 122.57(11) . . ?
C5 N5 Co2 120.05(8) . . ?
C6 N5 Co2 116.96(8) . . ?
C35 N6 C36 124.20(10) . . ?
C35 N6 Co2 117.52(8) . . ?
C36 N6 Co2 118.22(8) . . ?
C26 N7 C25 125.24(11) . . ?
C26 N7 Co2 117.02(8) . . ?
C25 N7 Co2 117.66(8) . . ?
C16 N8 C15 123.72(10) . . ?
C16 N8 Co2 119.00(8) . . ?
C15 N8 Co2 117.14(8) . . ?
C10 N9 C6 118.43(11) . . ?
C10 N9 Co3 121.36(9) . . ?
C6 N9 Co3 119.88(8) . . ?
C40 N10 C36 118.59(11) . . ?
C40 N10 Co3 120.85(9) . . ?
C36 N10 Co3 120.55(8) . . ?
C30 N11 C26 119.10(11) . . ?
C30 N11 Co3 118.82(8) . . ?
C26 N11 Co3 121.98(8) . . ?
C20 N12 C16 118.95(10) . . ?
C20 N12 Co3 120.63(8) . . ?
C16 N12 Co3 120.30(8) . . ?
C101 O100 C102 111.88(10) . . ?

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
N1 C1 C2 C3 3.5(2) . . . . ?
C1 C2 C3 C4 -1.1(2) . . . . ?
C2 C3 C4 C5 -2.4(2) . . . . ?
C3 C4 C5 N1 3.75(19) . . . . ?
C3 C4 C5 N5 -179.32(12) . . . . ?
N9 C6 C7 C8 1.35(19) . . . . ?
N5 C6 C7 C8 174.69(12) . . . . ?
C6 C7 C8 C9 0.8(2) . . . . ?
C7 C8 C9 C10 -2.1(2) . . . . ?
C8 C9 C10 N9 1.3(2) . . . . ?
N4 C11 C12 C13 2.1(2) . . . . ?
C11 C12 C13 C14 0.0(2) . . . . ?
C12 C13 C14 C15 -1.85(19) . . . . ?
C13 C14 C15 N4 1.78(18) . . . . ?
C13 C14 C15 N8 176.48(12) . . . . ?
N12 C16 C17 C18 2.02(19) . . . . ?
N8 C16 C17 C18 178.52(12) . . . . ?
C16 C17 C18 C19 -2.2(2) . . . . ?
C17 C18 C19 C20 0.1(2) . . . . ?
C18 C19 C20 N12 2.5(2) . . . . ?
N3 C21 C22 C23 2.0(2) . . . . ?
C21 C22 C23 C24 2.0(2) . . . . ?
C22 C23 C24 C25 -3.3(2) . . . . ?
C23 C24 C25 N3 0.72(19) . . . . ?
C23 C24 C25 N7 176.66(12) . . . . ?
N7 C26 C27 C28 169.70(12) . . . . ?
N11 C26 C27 C28 -4.59(18) . . . . ?
C26 C27 C28 C29 -0.35(19) . . . . ?
C27 C28 C29 C30 2.8(2) . . . . ?
C28 C29 C30 N11 -0.4(2) . . . . ?
N2 C31 C32 C33 1.5(2) . . . . ?
C31 C32 C33 C34 0.16(19) . . . . ?
C32 C33 C34 C35 -1.64(19) . . . . ?
C33 C34 C35 N6 176.54(12) . . . . ?
C33 C34 C35 N2 1.60(18) . . . . ?
N10 C36 C37 C38 -2.23(19) . . . . ?
N6 C36 C37 C38 172.81(12) . . . . ?
C36 C37 C38 C39 -1.2(2) . . . . ?
C37 C38 C39 C40 1.7(2) . . . . ?
C38 C39 C40 N10 1.2(2) . . . . ?
C2 C1 N1 C5 -2.16(19) . . . . ?
C2 C1 N1 Co1 173.74(10) . . . . ?
N5 C5 N1 C1 -178.66(11) . . . . ?
C4 C5 N1 C1 -1.49(17) . . . . ?
N5 C5 N1 Co1 5.34(14) . . . . ?
C4 C5 N1 Co1 -177.49(9) . . . . ?
C32 C31 N2 C35 -1.54(18) . . . . ?
C32 C31 N2 Co1 -177.39(10) . . . . ?
N6 C35 N2 C31 -175.41(11) . . . . ?
C34 C35 N2 C31 -0.03(17) . . . . ?
N6 C35 N2 Co1 0.38(14) . . . . ?
C34 C35 N2 Co1 175.77(9) . . . . ?
C22 C21 N3 C25 -4.57(19) . . . . ?
C22 C21 N3 Co1 174.85(10) . . . . ?
N7 C25 N3 C21 -173.23(11) . . . . ?
C24 C25 N3 C21 3.11(17) . . . . ?
N7 C25 N3 Co1 7.37(14) . . . . ?
C24 C25 N3 Co1 -176.29(9) . . . . ?
C12 C11 N4 C15 -2.23(19) . . . . ?
C12 C11 N4 Co1 -177.47(10) . . . . ?
N8 C15 N4 C11 -174.94(11) . . . . ?
C14 C15 N4 C11 0.22(17) . . . . ?
N8 C15 N4 Co1 0.28(14) . . . . ?
C14 C15 N4 Co1 175.44(9) . . . . ?
N1 C5 N5 C6 -153.16(11) . . . . ?
C4 C5 N5 C6 29.80(19) . . . . ?
N1 C5 N5 Co2 19.20(14) . . . . ?
C4 C5 N5 Co2 -157.84(10) . . . . ?
N9 C6 N5 C5 -157.77(11) . . . . ?
C7 C6 N5 C5 28.61(18) . . . . ?
N9 C6 N5 Co2 29.66(14) . . . . ?
C7 C6 N5 Co2 -143.97(10) . . . . ?
N2 C35 N6 C36 -157.48(11) . . . . ?
C34 C35 N6 C36 27.37(18) . . . . ?
N2 C35 N6 Co2 25.30(13) . . . . ?
C34 C35 N6 Co2 -149.85(10) . . . . ?
N10 C36 N6 C35 -157.14(11) . . . . ?
C37 C36 N6 C35 27.60(19) . . . . ?
N10 C36 N6 Co2 20.06(14) . . . . ?
C37 C36 N6 Co2 -155.20(10) . . . . ?
N11 C26 N7 C25 -163.06(11) . . . . ?
C27 C26 N7 C25 22.43(19) . . . . ?
N11 C26 N7 Co2 20.24(13) . . . . ?
C27 C26 N7 Co2 -154.27(10) . . . . ?
N3 C25 N7 C26 -157.93(11) . . . . ?
C24 C25 N7 C26 25.96(19) . . . . ?
N3 C25 N7 Co2 18.76(13) . . . . ?
C24 C25 N7 Co2 -157.36(10) . . . . ?
N12 C16 N8 C15 -157.73(11) . . . . ?
C17 C16 N8 C15 25.64(19) . . . . ?
N12 C16 N8 Co2 17.97(14) . . . . ?
C17 C16 N8 Co2 -158.66(10) . . . . ?
N4 C15 N8 C16 -157.20(11) . . . . ?
C14 C15 N8 C16 27.87(18) . . . . ?
N4 C15 N8 Co2 27.02(13) . . . . ?
C14 C15 N8 Co2 -147.90(10) . . . . ?
C9 C10 N9 C6 0.83(19) . . . . ?
C9 C10 N9 Co3 -172.65(10) . . . . ?
N5 C6 N9 C10 -176.04(11) . . . . ?
C7 C6 N9 C10 -2.16(17) . . . . ?
N5 C6 N9 Co3 -2.46(14) . . . . ?
C7 C6 N9 Co3 171.42(9) . . . . ?
C39 C40 N10 C36 -4.68(19) . . . . ?
C39 C40 N10 Co3 176.26(10) . . . . ?
N6 C36 N10 C40 -170.44(11) . . . . ?
C37 C36 N10 C40 5.07(17) . . . . ?
N6 C36 N10 Co3 8.63(14) . . . . ?
C37 C36 N10 Co3 -175.86(9) . . . . ?
C29 C30 N11 C26 -4.55(19) . . . . ?
C29 C30 N11 Co3 179.01(10) . . . . ?
N7 C26 N11 C30 -167.99(11) . . . . ?
C27 C26 N11 C30 6.93(17) . . . . ?
N7 C26 N11 Co3 8.34(14) . . . . ?
C27 C26 N11 Co3 -176.75(9) . . . . ?
C19 C20 N12 C16 -2.75(19) . . . . ?
C19 C20 N12 Co3 173.31(10) . . . . ?
N8 C16 N12 C20 -176.37(11) . . . . ?
C17 C16 N12 C20 0.43(18) . . . . ?
N8 C16 N12 Co3 7.55(14) . . . . ?
C17 C16 N12 Co3 -175.64(9) . . . . ?
C100 C101 O100 C102 170.14(12) . . . . ?
C103 C102 O100 C101 -176.55(11) . . . . ?

_refine_diff_density_max         0.469
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.062


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: DMF, ether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_1-2CH2CL2-85K
_database_code_depnum_ccdc_archive 'CCDC 1865579'
_audit_update_record             
;
2018-09-03 deposited with the CCDC.
2018-11-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C40 H32 Co3 F2 N12, 2(C H2 Cl2)'
_chemical_formula_sum            'C42 H36 Cl4 Co3 F2 N12'
_chemical_formula_weight         1065.42

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'
Cl Cl 0.1484 0.1585 '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'
F F 0.0171 0.0103 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

_cell_length_a                   20.362(5)
_cell_length_b                   13.838(3)
_cell_length_c                   17.100(7)
_cell_angle_alpha                90
_cell_angle_beta                 118.721(8)
_cell_angle_gamma                90
_cell_volume                     4225(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    85(2)
_cell_measurement_reflns_used    9883
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      26.32

_exptl_crystal_description       block
_exptl_crystal_colour            'dark reddish-brown'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_F_000             2156
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    1.476
_shelx_estimated_absorpt_T_min   0.855
_shelx_estimated_absorpt_T_max   0.866
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.688
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   '(SADABS; Bruker, 2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      85(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            39436
_diffrn_reflns_av_unetI/netI     0.0155
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.955
_diffrn_reflns_theta_max         26.379
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4321
_reflns_number_gt                3871
_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       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_structure_solution    'SHELXS2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_publication_material  'SHELXL-2016/4 (Sheldrick, 2016)'
_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)+(0.0287P)²+8.1978P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4321
_refine_ls_number_parameters     287
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0248
_refine_ls_wR_factor_ref         0.0649
_refine_ls_wR_factor_gt          0.0626
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_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
C1 C 0.64025(9) 0.94604(12) 0.27269(11) 0.0136(3) Uani 1 1 d . . . . .
H1 H 0.621365 1.004339 0.283617 0.016 Uiso 1 1 calc R U . . .
C1S C 0.40937(11) 0.20584(13) 0.16662(13) 0.0209(4) Uani 1 1 d . . . . .
H1SA H 0.435688 0.262891 0.203254 0.025 Uiso 1 1 calc R U . . .
H1SB H 0.436237 0.147207 0.199694 0.025 Uiso 1 1 calc R U . . .
C2 C 0.71025(10) 0.94745(13) 0.27865(12) 0.0163(4) Uani 1 1 d . . . . .
H2 H 0.737916 1.005869 0.290395 0.020 Uiso 1 1 calc R U . . .
C3 C 0.73917(9) 0.86078(13) 0.26696(12) 0.0165(4) Uani 1 1 d . . . . .
H3 H 0.787993 0.858800 0.272879 0.020 Uiso 1 1 calc R U . . .
C4 C 0.69672(9) 0.77811(13) 0.24682(11) 0.0143(3) Uani 1 1 d . . . . .
H4 H 0.716819 0.718436 0.240605 0.017 Uiso 1 1 calc R U . . .
C5 C 0.62295(9) 0.78162(11) 0.23529(11) 0.0104(3) Uani 1 1 d . . . . .
C6 C 0.57929(9) 0.62694(12) 0.16548(11) 0.0114(3) Uani 1 1 d . . . . .
C7 C 0.61120(9) 0.62835(13) 0.10771(11) 0.0154(4) Uani 1 1 d . . . . .
H7 H 0.632414 0.686401 0.100132 0.019 Uiso 1 1 calc R U . . .
C8 C 0.61161(10) 0.54623(14) 0.06265(12) 0.0183(4) Uani 1 1 d . . . . .
H8 H 0.633820 0.546945 0.024882 0.022 Uiso 1 1 calc R U . . .
C9 C 0.57912(10) 0.46202(13) 0.07296(12) 0.0186(4) Uani 1 1 d . . . . .
H9 H 0.579856 0.404028 0.043656 0.022 Uiso 1 1 calc R U . . .
C10 C 0.54587(9) 0.46470(12) 0.12664(11) 0.0151(3) Uani 1 1 d . . . . .
H10 H 0.522043 0.407927 0.131894 0.018 Uiso 1 1 calc R U . . .
C11 C 0.44966(9) 0.94519(12) 0.07237(11) 0.0125(3) Uani 1 1 d . . . . .
H11 H 0.474188 1.001682 0.104869 0.015 Uiso 1 1 calc R U . . .
C12 C 0.58416(9) 0.94852(13) 0.51969(12) 0.0155(4) Uani 1 1 d . . . . .
H12 H 0.584070 1.006163 0.549817 0.019 Uiso 1 1 calc R U . . .
C13 C 0.61840(10) 0.86462(13) 0.56694(12) 0.0159(4) Uani 1 1 d . . . . .
H13 H 0.641502 0.864013 0.630199 0.019 Uiso 1 1 calc R U . . .
C14 C 0.61851(10) 0.78281(12) 0.52140(11) 0.0134(3) Uani 1 1 d . . . . .
H14 H 0.641687 0.725552 0.553471 0.016 Uiso 1 1 calc R U . . .
C15 C 0.58422(9) 0.78309(11) 0.42662(11) 0.0104(3) Uani 1 1 d . . . . .
C16 C 0.62664(9) 0.62834(11) 0.40198(11) 0.0103(3) Uani 1 1 d . . . . .
C17 C 0.70122(9) 0.62996(12) 0.47288(11) 0.0126(3) Uani 1 1 d . . . . .
H17 H 0.719426 0.685683 0.509603 0.015 Uiso 1 1 calc R U . . .
C18 C 0.74739(9) 0.55169(13) 0.48896(11) 0.0145(3) Uani 1 1 d . . . . .
H18 H 0.797400 0.553357 0.536493 0.017 Uiso 1 1 calc R U . . .
C19 C 0.72063(9) 0.46960(13) 0.43523(12) 0.0150(3) Uani 1 1 d . . . . .
H19 H 0.751798 0.414859 0.444988 0.018 Uiso 1 1 calc R U . . .
C20 C 0.64749(9) 0.47061(12) 0.36755(11) 0.0129(3) Uani 1 1 d . . . . .
H20 H 0.628955 0.415264 0.330380 0.016 Uiso 1 1 calc R U . . .
Cl1 Cl 0.31589(3) 0.20327(4) 0.14907(4) 0.03435(14) Uani 1 1 d . . . . .
Cl2 Cl 0.41071(4) 0.21114(4) 0.06405(5) 0.04670(17) Uani 1 1 d . . . . .
Co1 Co 0.500000 0.87337(2) 0.250000 0.00794(8) Uani 1 2 d S T P . .
Co2 Co 0.500000 0.70524(2) 0.250000 0.00786(8) Uani 1 2 d S T P . .
Co3 Co 0.500000 0.53790(2) 0.250000 0.00886(8) Uani 1 2 d S T P . .
F1 F 0.500000 1.01869(9) 0.250000 0.0135(3) Uani 1 2 d S T P . .
F2 F 0.500000 0.39298(10) 0.250000 0.0165(3) Uani 1 2 d S T P . .
N1 N 0.59721(8) 0.86596(10) 0.25210(9) 0.0105(3) Uani 1 1 d . . . . .
N2 N 0.44973(7) 0.86570(10) 0.11879(9) 0.0103(3) Uani 1 1 d . . . . .
N3 N 0.57508(8) 0.70465(9) 0.21261(9) 0.0104(3) Uani 1 1 d . . . . .
N4 N 0.57769(8) 0.70484(9) 0.37365(9) 0.0101(3) Uani 1 1 d . . . . .
N5 N 0.54561(7) 0.54468(10) 0.17228(9) 0.0113(3) Uani 1 1 d . . . . .
N6 N 0.60079(8) 0.54653(10) 0.35144(9) 0.0102(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.350(2) . ?
C1 C2 1.379(2) . ?
C1 H1 0.9500 . ?
C1S Cl2 1.769(2) . ?
C1S Cl1 1.779(2) . ?
C1S H1SA 0.9900 . ?
C1S H1SB 0.9900 . ?
C2 C3 1.392(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.374(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.419(2) . ?
C4 H4 0.9500 . ?
C5 N1 1.365(2) . ?
C5 N3 1.368(2) . ?
C6 N5 1.362(2) . ?
C6 N3 1.371(2) . ?
C6 C7 1.420(2) . ?
C7 C8 1.375(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.392(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.378(3) . ?
C9 H9 0.9500 . ?
C10 N5 1.356(2) . ?
C10 H10 0.9500 . ?
C11 N2 1.356(2) . ?
C11 C12 1.383(2) 2_655 ?
C11 H11 0.9500 . ?
C12 C13 1.395(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.375(2) . ?
C13 H13 0.9500 . ?
C14 C15 1.424(2) . ?
C14 H14 0.9500 . ?
C15 N2 1.368(2) 2_655 ?
C15 N4 1.377(2) . ?
C16 N6 1.367(2) . ?
C16 N4 1.373(2) . ?
C16 C17 1.417(2) . ?
C17 C18 1.373(2) . ?
C17 H17 0.9500 . ?
C18 C19 1.397(2) . ?
C18 H18 0.9500 . ?
C19 C20 1.379(2) . ?
C19 H19 0.9500 . ?
C20 N6 1.354(2) . ?
C20 H20 0.9500 . ?
Co1 N1 1.9649(14) 2_655 ?
Co1 N1 1.9649(14) . ?
Co1 N2 1.9711(16) 2_655 ?
Co1 N2 1.9712(16) . ?
Co1 F1 2.0109(14) . ?
Co1 Co2 2.3265(6) . ?
Co2 N3 1.9198(14) 2_655 ?
Co2 N3 1.9198(14) . ?
Co2 N4 1.9387(15) 2_655 ?
Co2 N4 1.9387(15) . ?
Co2 Co3 2.3156(6) . ?
Co3 N6 1.9527(14) 2_655 ?
Co3 N6 1.9528(14) . ?
Co3 N5 1.9554(15) 2_655 ?
Co3 N5 1.9554(15) . ?
Co3 F2 2.0054(14) . ?

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
N1 C1 C2 123.30(16) . . ?
N1 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
Cl2 C1S Cl1 111.02(11) . . ?
Cl2 C1S H1SA 109.4 . . ?
Cl1 C1S H1SA 109.4 . . ?
Cl2 C1S H1SB 109.4 . . ?
Cl1 C1S H1SB 109.4 . . ?
H1SA C1S H1SB 108.0 . . ?
C1 C2 C3 118.07(16) . . ?
C1 C2 H2 121.0 . . ?
C3 C2 H2 121.0 . . ?
C4 C3 C2 119.63(16) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C3 C4 C5 120.19(16) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
N1 C5 N3 115.59(14) . . ?
N1 C5 C4 119.20(15) . . ?
N3 C5 C4 125.11(15) . . ?
N5 C6 N3 115.41(14) . . ?
N5 C6 C7 119.23(15) . . ?
N3 C6 C7 125.24(15) . . ?
C8 C7 C6 120.43(16) . . ?
C8 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
C7 C8 C9 119.31(16) . . ?
C7 C8 H8 120.3 . . ?
C9 C8 H8 120.3 . . ?
C10 C9 C8 118.50(16) . . ?
C10 C9 H9 120.8 . . ?
C8 C9 H9 120.8 . . ?
N5 C10 C9 122.98(17) . . ?
N5 C10 H10 118.5 . . ?
C9 C10 H10 118.5 . . ?
N2 C11 C12 123.58(16) . 2_655 ?
N2 C11 H11 118.2 . . ?
C12 C11 H11 118.2 2_655 . ?
C11 C12 C13 117.93(16) 2_655 . ?
C11 C12 H12 121.0 2_655 . ?
C13 C12 H12 121.0 . . ?
C14 C13 C12 119.59(16) . . ?
C14 C13 H13 120.2 . . ?
C12 C13 H13 120.2 . . ?
C13 C14 C15 120.61(16) . . ?
C13 C14 H14 119.7 . . ?
C15 C14 H14 119.7 . . ?
N2 C15 N4 114.91(14) 2_655 . ?
N2 C15 C14 119.08(14) 2_655 . ?
N4 C15 C14 125.90(15) . . ?
N6 C16 N4 114.95(14) . . ?
N6 C16 C17 118.88(14) . . ?
N4 C16 C17 125.99(15) . . ?
C18 C17 C16 120.55(16) . . ?
C18 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
C17 C18 C19 119.79(16) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 H18 120.1 . . ?
C20 C19 C18 117.81(16) . . ?
C20 C19 H19 121.1 . . ?
C18 C19 H19 121.1 . . ?
N6 C20 C19 123.27(16) . . ?
N6 C20 H20 118.4 . . ?
C19 C20 H20 118.4 . . ?
N1 Co1 N1 174.02(8) 2_655 . ?
N1 Co1 N2 89.17(6) 2_655 2_655 ?
N1 Co1 N2 90.50(6) . 2_655 ?
N1 Co1 N2 90.51(6) 2_655 . ?
N1 Co1 N2 89.17(6) . . ?
N2 Co1 N2 173.82(8) 2_655 . ?
N1 Co1 F1 92.99(4) 2_655 . ?
N1 Co1 F1 92.99(4) . . ?
N2 Co1 F1 93.09(4) 2_655 . ?
N2 Co1 F1 93.09(4) . . ?
N1 Co1 Co2 87.01(4) 2_655 . ?
N1 Co1 Co2 87.01(4) . . ?
N2 Co1 Co2 86.91(4) 2_655 . ?
N2 Co1 Co2 86.91(4) . . ?
F1 Co1 Co2 180.0 . . ?
N3 Co2 N3 179.51(8) 2_655 . ?
N3 Co2 N4 90.01(6) 2_655 2_655 ?
N3 Co2 N4 89.99(6) . 2_655 ?
N3 Co2 N4 89.99(6) 2_655 . ?
N3 Co2 N4 90.01(6) . . ?
N4 Co2 N4 179.67(8) 2_655 . ?
N3 Co2 Co3 89.75(4) 2_655 . ?
N3 Co2 Co3 89.75(4) . . ?
N4 Co2 Co3 89.83(4) 2_655 . ?
N4 Co2 Co3 89.83(4) . . ?
N3 Co2 Co1 90.25(4) 2_655 . ?
N3 Co2 Co1 90.25(4) . . ?
N4 Co2 Co1 90.17(4) 2_655 . ?
N4 Co2 Co1 90.17(4) . . ?
Co3 Co2 Co1 180.0 . . ?
N6 Co3 N6 172.99(8) 2_655 . ?
N6 Co3 N5 87.77(6) 2_655 2_655 ?
N6 Co3 N5 91.89(6) . 2_655 ?
N6 Co3 N5 91.89(6) 2_655 . ?
N6 Co3 N5 87.77(6) . . ?
N5 Co3 N5 174.50(8) 2_655 . ?
N6 Co3 F2 93.51(4) 2_655 . ?
N6 Co3 F2 93.51(4) . . ?
N5 Co3 F2 92.75(4) 2_655 . ?
N5 Co3 F2 92.75(4) . . ?
N6 Co3 Co2 86.49(4) 2_655 . ?
N6 Co3 Co2 86.49(4) . . ?
N5 Co3 Co2 87.25(4) 2_655 . ?
N5 Co3 Co2 87.25(4) . . ?
F2 Co3 Co2 180.0 . . ?
C1 N1 C5 119.32(14) . . ?
C1 N1 Co1 118.93(11) . . ?
C5 N1 Co1 121.74(11) . . ?
C11 N2 C15 119.17(14) . 2_655 ?
C11 N2 Co1 118.45(11) . . ?
C15 N2 Co1 122.37(11) 2_655 . ?
C5 N3 C6 122.69(14) . . ?
C5 N3 Co2 118.37(11) . . ?
C6 N3 Co2 118.94(11) . . ?
C16 N4 C15 123.38(14) . . ?
C16 N4 Co2 117.43(11) . . ?
C15 N4 Co2 119.04(11) . . ?
C10 N5 C6 119.45(15) . . ?
C10 N5 Co3 119.12(12) . . ?
C6 N5 Co3 121.40(11) . . ?
C20 N6 C16 119.65(14) . . ?
C20 N6 Co3 117.97(11) . . ?
C16 N6 Co3 122.23(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
N1 C1 C2 C3 -3.2(3) . . . . ?
C1 C2 C3 C4 2.4(3) . . . . ?
C2 C3 C4 C5 1.9(3) . . . . ?
C3 C4 C5 N1 -5.7(2) . . . . ?
C3 C4 C5 N3 177.95(16) . . . . ?
N5 C6 C7 C8 -3.4(2) . . . . ?
N3 C6 C7 C8 -179.15(16) . . . . ?
C6 C7 C8 C9 1.2(3) . . . . ?
C7 C8 C9 C10 1.6(3) . . . . ?
C8 C9 C10 N5 -2.3(3) . . . . ?
C11 C12 C13 C14 1.0(2) 2_655 . . . ?
C12 C13 C14 C15 0.2(3) . . . . ?
C13 C14 C15 N2 -0.8(2) . . . 2_655 ?
C13 C14 C15 N4 -176.75(16) . . . . ?
N6 C16 C17 C18 1.8(2) . . . . ?
N4 C16 C17 C18 -173.05(15) . . . . ?
C16 C17 C18 C19 -0.2(2) . . . . ?
C17 C18 C19 C20 -0.5(2) . . . . ?
C18 C19 C20 N6 -0.5(2) . . . . ?
C2 C1 N1 C5 -0.6(2) . . . . ?
C2 C1 N1 Co1 177.90(13) . . . . ?
N3 C5 N1 C1 -178.30(14) . . . . ?
C4 C5 N1 C1 5.0(2) . . . . ?
N3 C5 N1 Co1 3.20(19) . . . . ?
C4 C5 N1 Co1 -173.47(12) . . . . ?
C12 C11 N2 C15 1.0(2) 2_655 . . 2_655 ?
C12 C11 N2 Co1 -179.59(13) 2_655 . . . ?
N1 C5 N3 C6 157.19(15) . . . . ?
C4 C5 N3 C6 -26.4(2) . . . . ?
N1 C5 N3 Co2 -23.69(18) . . . . ?
C4 C5 N3 Co2 152.75(14) . . . . ?
N5 C6 N3 C5 159.88(15) . . . . ?
C7 C6 N3 C5 -24.2(2) . . . . ?
N5 C6 N3 Co2 -19.23(19) . . . . ?
C7 C6 N3 Co2 156.72(13) . . . . ?
N6 C16 N4 C15 162.36(14) . . . . ?
C17 C16 N4 C15 -22.6(2) . . . . ?
N6 C16 N4 Co2 -22.04(17) . . . . ?
C17 C16 N4 Co2 153.01(13) . . . . ?
N2 C15 N4 C16 156.78(14) 2_655 . . . ?
C14 C15 N4 C16 -27.1(2) . . . . ?
N2 C15 N4 Co2 -18.75(18) 2_655 . . . ?
C14 C15 N4 Co2 157.38(13) . . . . ?
C9 C10 N5 C6 0.2(2) . . . . ?
C9 C10 N5 Co3 -177.60(13) . . . . ?
N3 C6 N5 C10 178.85(14) . . . . ?
C7 C6 N5 C10 2.6(2) . . . . ?
N3 C6 N5 Co3 -3.43(19) . . . . ?
C7 C6 N5 Co3 -179.63(12) . . . . ?
C19 C20 N6 C16 2.1(2) . . . . ?
C19 C20 N6 Co3 177.73(13) . . . . ?
N4 C16 N6 C20 172.70(14) . . . . ?
C17 C16 N6 C20 -2.7(2) . . . . ?
N4 C16 N6 Co3 -2.70(18) . . . . ?
C17 C16 N6 Co3 -178.13(11) . . . . ?

_refine_diff_density_max         0.671
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.059


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dichloromethane'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_2-Et2O-85K
_database_code_depnum_ccdc_archive 'CCDC 1865583'
_audit_update_record             
;
2018-09-03 deposited with the CCDC.
2018-11-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C40 H32 Cl2 Co3 N12, C4 H10 O'
_chemical_formula_sum            'C44 H42 Cl2 Co3 N12 O'
_chemical_formula_weight         1002.58

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'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   15.8035(8)
_cell_length_b                   15.6410(8)
_cell_length_c                   16.9161(8)
_cell_angle_alpha                90
_cell_angle_beta                 98.981(2)
_cell_angle_gamma                90
_cell_volume                     4130.1(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    85(2)
_cell_measurement_reflns_used    9788
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      27.11

_exptl_crystal_description       block
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_F_000             2052
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.61
_exptl_crystal_size_min          0.58
_exptl_absorpt_coefficient_mu    1.374
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5238
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   '(SADABS; Bruker, 2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      85(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            77046
_diffrn_reflns_av_unetI/netI     0.0130
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.783
_diffrn_reflns_theta_max         27.145
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             9131
_reflns_number_gt                8599
_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       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_structure_solution    'SHELXS2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_publication_material  'SHELXL-2016/4 (Sheldrick, 2016)'
_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)+(0.0225P)²+3.5084P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9131
_refine_ls_number_parameters     561
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0219
_refine_ls_wR_factor_ref         0.0550
_refine_ls_wR_factor_gt          0.0539
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.002
_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
C1 C 0.72931(9) -0.15588(9) 0.42508(8) 0.0111(3) Uani 1 1 d . . . . .
H1 H 0.678056 -0.148419 0.447091 0.013 Uiso 1 1 calc R U . . .
C2 C 0.79340(9) -0.20528(9) 0.46672(8) 0.0129(3) Uani 1 1 d . . . . .
H2 H 0.785780 -0.232910 0.515125 0.015 Uiso 1 1 calc R U . . .
C3 C 0.86996(9) -0.21362(9) 0.43577(8) 0.0124(3) Uani 1 1 d . . . . .
H3 H 0.915557 -0.247080 0.463062 0.015 Uiso 1 1 calc R U . . .
C4 C 0.87866(9) -0.17296(9) 0.36547(8) 0.0106(3) Uani 1 1 d . . . . .
H4 H 0.931075 -0.177056 0.344821 0.013 Uiso 1 1 calc R U . . .
C5 C 0.80997(8) -0.12507(8) 0.32374(8) 0.0081(2) Uani 1 1 d . . . . .
C6 C 0.86738(8) -0.09876(8) 0.20191(7) 0.0079(2) Uani 1 1 d . . . . .
C7 C 0.89915(9) -0.18168(9) 0.19043(8) 0.0107(3) Uani 1 1 d . . . . .
H7 H 0.884558 -0.228010 0.222025 0.013 Uiso 1 1 calc R U . . .
C8 C 0.95125(9) -0.19531(9) 0.13344(8) 0.0123(3) Uani 1 1 d . . . . .
H8 H 0.974412 -0.250474 0.127029 0.015 Uiso 1 1 calc R U . . .
C9 C 0.96975(9) -0.12760(9) 0.08524(8) 0.0123(3) Uani 1 1 d . . . . .
H9 H 1.005508 -0.135622 0.045615 0.015 Uiso 1 1 calc R U . . .
C10 C 0.93475(8) -0.04882(9) 0.09670(8) 0.0101(3) Uani 1 1 d . . . . .
H10 H 0.945167 -0.003228 0.062381 0.012 Uiso 1 1 calc R U . . .
C11 C 0.61612(9) 0.06418(9) 0.43567(8) 0.0112(3) Uani 1 1 d . . . . .
H11 H 0.560570 0.039511 0.425249 0.013 Uiso 1 1 calc R U . . .
C12 C 0.63446(9) 0.11850(9) 0.50009(8) 0.0141(3) Uani 1 1 d . . . . .
H12 H 0.593286 0.129749 0.534113 0.017 Uiso 1 1 calc R U . . .
C13 C 0.71507(9) 0.15648(9) 0.51396(8) 0.0138(3) Uani 1 1 d . . . . .
H13 H 0.730539 0.192800 0.558903 0.017 Uiso 1 1 calc R U . . .
C14 C 0.77237(9) 0.14089(9) 0.46180(8) 0.0119(3) Uani 1 1 d . . . . .
H14 H 0.826341 0.168956 0.469311 0.014 Uiso 1 1 calc R U . . .
C15 C 0.75114(8) 0.08347(8) 0.39737(8) 0.0086(2) Uani 1 1 d . . . . .
C16 C 0.88830(8) 0.07504(8) 0.34960(8) 0.0082(2) Uani 1 1 d . . . . .
C17 C 0.94433(9) 0.07424(9) 0.42358(8) 0.0115(3) Uani 1 1 d . . . . .
H17 H 0.921676 0.076833 0.472345 0.014 Uiso 1 1 calc R U . . .
C18 C 1.03149(9) 0.06971(9) 0.42502(8) 0.0131(3) Uani 1 1 d . . . . .
H18 H 1.069084 0.069755 0.474667 0.016 Uiso 1 1 calc R U . . .
C19 C 1.06447(9) 0.06504(9) 0.35332(9) 0.0138(3) Uani 1 1 d . . . . .
H19 H 1.124254 0.058963 0.353135 0.017 Uiso 1 1 calc R U . . .
C20 C 1.00791(8) 0.06949(9) 0.28297(8) 0.0114(3) Uani 1 1 d . . . . .
H20 H 1.030140 0.067022 0.233979 0.014 Uiso 1 1 calc R U . . .
C21 C 0.47676(9) 0.02248(9) 0.22465(8) 0.0116(3) Uani 1 1 d . . . . .
H21 H 0.456738 -0.028833 0.245425 0.014 Uiso 1 1 calc R U . . .
C22 C 0.41802(9) 0.07530(9) 0.18016(8) 0.0133(3) Uani 1 1 d . . . . .
H22 H 0.358769 0.061442 0.171583 0.016 Uiso 1 1 calc R U . . .
C23 C 0.44745(9) 0.14968(9) 0.14793(8) 0.0121(3) Uani 1 1 d . . . . .
H23 H 0.408317 0.187377 0.117027 0.015 Uiso 1 1 calc R U . . .
C24 C 0.53377(9) 0.16794(9) 0.16134(8) 0.0107(3) Uani 1 1 d . . . . .
H24 H 0.554637 0.217678 0.138533 0.013 Uiso 1 1 calc R U . . .
C25 C 0.59119(8) 0.11264(8) 0.20903(8) 0.0083(2) Uani 1 1 d . . . . .
C26 C 0.71870(8) 0.19976(8) 0.22065(7) 0.0084(2) Uani 1 1 d . . . . .
C27 C 0.68360(9) 0.27946(9) 0.23804(8) 0.0113(3) Uani 1 1 d . . . . .
H27 H 0.625537 0.282916 0.246109 0.014 Uiso 1 1 calc R U . . .
C28 C 0.73339(9) 0.35206(9) 0.24331(8) 0.0136(3) Uani 1 1 d . . . . .
H28 H 0.709729 0.405890 0.253982 0.016 Uiso 1 1 calc R U . . .
C29 C 0.81900(9) 0.34572(9) 0.23281(8) 0.0142(3) Uani 1 1 d . . . . .
H29 H 0.855014 0.394676 0.237645 0.017 Uiso 1 1 calc R U . . .
C30 C 0.85010(9) 0.26675(9) 0.21524(8) 0.0114(3) Uani 1 1 d . . . . .
H30 H 0.908653 0.262326 0.209019 0.014 Uiso 1 1 calc R U . . .
C31 C 0.57384(8) -0.19335(9) 0.20742(8) 0.0110(3) Uani 1 1 d . . . . .
H31 H 0.557531 -0.210954 0.256641 0.013 Uiso 1 1 calc R U . . .
C32 C 0.55047(9) -0.24401(9) 0.14121(9) 0.0137(3) Uani 1 1 d . . . . .
H32 H 0.516151 -0.293465 0.143943 0.016 Uiso 1 1 calc R U . . .
C33 C 0.57857(9) -0.22086(9) 0.06949(8) 0.0138(3) Uani 1 1 d . . . . .
H33 H 0.564601 -0.255099 0.022887 0.017 Uiso 1 1 calc R U . . .
C34 C 0.62659(9) -0.14791(9) 0.06775(8) 0.0122(3) Uani 1 1 d . . . . .
H34 H 0.647655 -0.132598 0.020069 0.015 Uiso 1 1 calc R U . . .
C35 C 0.64498(8) -0.09528(8) 0.13643(8) 0.0090(2) Uani 1 1 d . . . . .
C36 C 0.69300(8) 0.02918(8) 0.07343(8) 0.0086(2) Uani 1 1 d . . . . .
C37 C 0.62506(9) 0.03504(9) 0.00863(8) 0.0127(3) Uani 1 1 d . . . . .
H37 H 0.576372 -0.000924 0.006994 0.015 Uiso 1 1 calc R U . . .
C38 C 0.62916(9) 0.09262(9) -0.05208(8) 0.0146(3) Uani 1 1 d . . . . .
H38 H 0.583198 0.097201 -0.095349 0.018 Uiso 1 1 calc R U . . .
C39 C 0.70139(9) 0.14412(9) -0.04947(8) 0.0145(3) Uani 1 1 d . . . . .
H39 H 0.706534 0.183052 -0.091564 0.017 Uiso 1 1 calc R U . . .
C40 C 0.76524(9) 0.13717(9) 0.01575(8) 0.0118(3) Uani 1 1 d . . . . .
H40 H 0.813962 0.173188 0.018008 0.014 Uiso 1 1 calc R U . . .
C100 C 0.32093(10) 0.05974(10) 0.37937(9) 0.0193(3) Uani 1 1 d . . . . .
H41A H 0.277856 0.025800 0.401228 0.029 Uiso 1 1 calc R U . . .
H41B H 0.352116 0.095558 0.421750 0.029 Uiso 1 1 calc R U . . .
H41C H 0.361196 0.021400 0.358436 0.029 Uiso 1 1 calc R U . . .
C101 C 0.27710(9) 0.11604(9) 0.31252(9) 0.0155(3) Uani 1 1 d . . . . .
H42A H 0.234789 0.153590 0.332717 0.019 Uiso 1 1 calc R U . . .
H42B H 0.319866 0.152548 0.291778 0.019 Uiso 1 1 calc R U . . .
C102 C 0.19613(9) 0.11086(9) 0.18267(8) 0.0143(3) Uani 1 1 d . . . . .
H43A H 0.237764 0.152396 0.166970 0.017 Uiso 1 1 calc R U . . .
H43B H 0.146372 0.142957 0.196298 0.017 Uiso 1 1 calc R U . . .
C103 C 0.16732(10) 0.04999(10) 0.11439(9) 0.0204(3) Uani 1 1 d . . . . .
H44A H 0.217202 0.020083 0.099931 0.031 Uiso 1 1 calc R U . . .
H44B H 0.138802 0.082201 0.068074 0.031 Uiso 1 1 calc R U . . .
H44C H 0.127260 0.008228 0.130875 0.031 Uiso 1 1 calc R U . . .
CL1 Cl 0.53102(2) -0.11207(2) 0.36994(2) 0.01228(7) Uani 1 1 d . . . . .
CL2 Cl 0.95772(2) 0.15632(2) 0.10998(2) 0.01133(7) Uani 1 1 d . . . . .
CO1 Co 0.64080(2) -0.04326(2) 0.30103(2) 0.00665(4) Uani 1 1 d . . . . .
CO2 Co 0.74637(2) 0.02238(2) 0.24004(2) 0.00599(4) Uani 1 1 d . . . . .
CO3 Co 0.84925(2) 0.08454(2) 0.17437(2) 0.00629(4) Uani 1 1 d . . . . .
N1 N 0.73533(7) -0.11726(7) 0.35434(7) 0.0084(2) Uani 1 1 d . . . . .
N2 N 0.67297(7) 0.04389(7) 0.38620(7) 0.0088(2) Uani 1 1 d . . . . .
N3 N 0.56154(7) 0.03985(7) 0.24031(7) 0.0089(2) Uani 1 1 d . . . . .
N4 N 0.61892(7) -0.11958(7) 0.20643(7) 0.0086(2) Uani 1 1 d . . . . .
N5 N 0.81401(7) -0.07891(7) 0.25565(6) 0.0078(2) Uani 1 1 d . . . . .
N6 N 0.80133(7) 0.06671(7) 0.33997(6) 0.0079(2) Uani 1 1 d . . . . .
N7 N 0.67806(7) 0.12276(7) 0.22244(6) 0.0083(2) Uani 1 1 d . . . . .
N8 N 0.69141(7) -0.02147(7) 0.13934(7) 0.0083(2) Uani 1 1 d . . . . .
N9 N 0.88614(7) -0.03292(7) 0.15444(6) 0.0081(2) Uani 1 1 d . . . . .
N10 N 0.92205(7) 0.07723(7) 0.27987(7) 0.0082(2) Uani 1 1 d . . . . .
N11 N 0.80126(7) 0.19508(7) 0.20641(6) 0.0087(2) Uani 1 1 d . . . . .
N12 N 0.76230(7) 0.08183(7) 0.07673(6) 0.0086(2) Uani 1 1 d . . . . .
O100 O 0.23508(6) 0.06234(6) 0.25022(6) 0.01294(19) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.3571(17) . ?
C1 C2 1.3770(19) . ?
C1 H1 0.9500 . ?
C2 C3 1.397(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.3742(19) . ?
C3 H3 0.9500 . ?
C4 C5 1.4137(18) . ?
C4 H4 0.9500 . ?
C5 N1 1.3655(17) . ?
C5 N5 1.3694(17) . ?
C6 N9 1.3665(17) . ?
C6 N5 1.3688(17) . ?
C6 C7 1.4151(18) . ?
C7 C8 1.3786(19) . ?
C7 H7 0.9500 . ?
C8 C9 1.395(2) . ?
C8 H8 0.9500 . ?
C9 C10 1.3767(19) . ?
C9 H9 0.9500 . ?
C10 N9 1.3566(17) . ?
C10 H10 0.9500 . ?
C11 N2 1.3576(17) . ?
C11 C12 1.377(2) . ?
C11 H11 0.9500 . ?
C12 C13 1.392(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.381(2) . ?
C13 H13 0.9500 . ?
C14 C15 1.4116(18) . ?
C14 H14 0.9500 . ?
C15 N2 1.3684(17) . ?
C15 N6 1.3716(17) . ?
C16 N6 1.3648(17) . ?
C16 N10 1.3688(17) . ?
C16 C17 1.4157(18) . ?
C17 C18 1.3758(19) . ?
C17 H17 0.9500 . ?
C18 C19 1.395(2) . ?
C18 H18 0.9500 . ?
C19 C20 1.3741(19) . ?
C19 H19 0.9500 . ?
C20 N10 1.3551(17) . ?
C20 H20 0.9500 . ?
C21 N3 1.3522(17) . ?
C21 C22 1.376(2) . ?
C21 H21 0.9500 . ?
C22 C23 1.395(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.3775(19) . ?
C23 H23 0.9500 . ?
C24 C25 1.4120(18) . ?
C24 H24 0.9500 . ?
C25 N7 1.3653(17) . ?
C25 N3 1.3687(17) . ?
C26 N11 1.3652(17) . ?
C26 N7 1.3675(17) . ?
C26 C27 1.4139(18) . ?
C27 C28 1.376(2) . ?
C27 H27 0.9500 . ?
C28 C29 1.395(2) . ?
C28 H28 0.9500 . ?
C29 C30 1.379(2) . ?
C29 H29 0.9500 . ?
C30 N11 1.3560(17) . ?
C30 H30 0.9500 . ?
C31 N4 1.3575(17) . ?
C31 C32 1.375(2) . ?
C31 H31 0.9500 . ?
C32 C33 1.403(2) . ?
C32 H32 0.9500 . ?
C33 C34 1.373(2) . ?
C33 H33 0.9500 . ?
C34 C35 1.4164(18) . ?
C34 H34 0.9500 . ?
C35 N8 1.3647(17) . ?
C35 N4 1.3670(17) . ?
C36 N12 1.3644(17) . ?
C36 N8 1.3712(17) . ?
C36 C37 1.4125(18) . ?
C37 C38 1.375(2) . ?
C37 H37 0.9500 . ?
C38 C39 1.392(2) . ?
C38 H38 0.9500 . ?
C39 C40 1.3784(19) . ?
C39 H39 0.9500 . ?
C40 N12 1.3529(17) . ?
C40 H40 0.9500 . ?
C100 C101 1.513(2) . ?
C100 H41A 0.9800 . ?
C100 H41B 0.9800 . ?
C100 H41C 0.9800 . ?
C101 O100 1.4278(17) . ?
C101 H42A 0.9900 . ?
C101 H42B 0.9900 . ?
C102 O100 1.4286(17) . ?
C102 C103 1.511(2) . ?
C102 H43A 0.9900 . ?
C102 H43B 0.9900 . ?
C103 H44A 0.9800 . ?
C103 H44B 0.9800 . ?
C103 H44C 0.9800 . ?
CL1 CO1 2.4816(4) . ?
CL2 CO3 2.4430(3) . ?
CO1 N3 1.9779(11) . ?
CO1 N4 1.9831(11) . ?
CO1 N1 1.9910(11) . ?
CO1 N2 1.9908(11) . ?
CO1 CO2 2.3323(2) . ?
CO2 N7 1.9023(11) . ?
CO2 N5 1.9063(11) . ?
CO2 N6 1.9064(11) . ?
CO2 N8 1.9143(11) . ?
CO2 CO3 2.3209(2) . ?
CO3 N10 1.9699(11) . ?
CO3 N9 1.9723(11) . ?
CO3 N12 1.9772(11) . ?
CO3 N11 1.9966(11) . ?

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
N1 C1 C2 123.61(13) . . ?
N1 C1 H1 118.2 . . ?
C2 C1 H1 118.2 . . ?
C1 C2 C3 118.12(12) . . ?
C1 C2 H2 120.9 . . ?
C3 C2 H2 120.9 . . ?
C4 C3 C2 119.37(13) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C3 C4 C5 120.30(13) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
N1 C5 N5 115.34(11) . . ?
N1 C5 C4 119.97(12) . . ?
N5 C5 C4 124.50(12) . . ?
N9 C6 N5 115.59(11) . . ?
N9 C6 C7 119.73(12) . . ?
N5 C6 C7 124.59(12) . . ?
C8 C7 C6 120.08(12) . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C7 C8 C9 119.59(13) . . ?
C7 C8 H8 120.2 . . ?
C9 C8 H8 120.2 . . ?
C10 C9 C8 118.14(12) . . ?
C10 C9 H9 120.9 . . ?
C8 C9 H9 120.9 . . ?
N9 C10 C9 123.41(12) . . ?
N9 C10 H10 118.3 . . ?
C9 C10 H10 118.3 . . ?
N2 C11 C12 123.68(13) . . ?
N2 C11 H11 118.2 . . ?
C12 C11 H11 118.2 . . ?
C11 C12 C13 118.09(13) . . ?
C11 C12 H12 121.0 . . ?
C13 C12 H12 121.0 . . ?
C14 C13 C12 119.41(13) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C13 C14 C15 120.34(13) . . ?
C13 C14 H14 119.8 . . ?
C15 C14 H14 119.8 . . ?
N2 C15 N6 115.15(11) . . ?
N2 C15 C14 119.68(12) . . ?
N6 C15 C14 125.05(12) . . ?
N6 C16 N10 114.85(11) . . ?
N6 C16 C17 125.72(12) . . ?
N10 C16 C17 119.20(12) . . ?
C18 C17 C16 120.16(13) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
C17 C18 C19 119.76(12) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 H18 120.1 . . ?
C20 C19 C18 118.01(13) . . ?
C20 C19 H19 121.0 . . ?
C18 C19 H19 121.0 . . ?
N10 C20 C19 123.37(13) . . ?
N10 C20 H20 118.3 . . ?
C19 C20 H20 118.3 . . ?
N3 C21 C22 123.36(13) . . ?
N3 C21 H21 118.3 . . ?
C22 C21 H21 118.3 . . ?
C21 C22 C23 118.49(12) . . ?
C21 C22 H22 120.8 . . ?
C23 C22 H22 120.8 . . ?
C24 C23 C22 119.38(13) . . ?
C24 C23 H23 120.3 . . ?
C22 C23 H23 120.3 . . ?
C23 C24 C25 119.91(13) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
N7 C25 N3 115.35(11) . . ?
N7 C25 C24 124.32(12) . . ?
N3 C25 C24 120.15(12) . . ?
N11 C26 N7 114.94(11) . . ?
N11 C26 C27 120.06(12) . . ?
N7 C26 C27 124.82(12) . . ?
C28 C27 C26 120.12(12) . . ?
C28 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
C27 C28 C29 119.28(13) . . ?
C27 C28 H28 120.4 . . ?
C29 C28 H28 120.4 . . ?
C30 C29 C28 118.45(13) . . ?
C30 C29 H29 120.8 . . ?
C28 C29 H29 120.8 . . ?
N11 C30 C29 123.25(13) . . ?
N11 C30 H30 118.4 . . ?
C29 C30 H30 118.4 . . ?
N4 C31 C32 123.68(13) . . ?
N4 C31 H31 118.2 . . ?
C32 C31 H31 118.2 . . ?
C31 C32 C33 118.35(13) . . ?
C31 C32 H32 120.8 . . ?
C33 C32 H32 120.8 . . ?
C34 C33 C32 118.91(13) . . ?
C34 C33 H33 120.5 . . ?
C32 C33 H33 120.5 . . ?
C33 C34 C35 120.57(13) . . ?
C33 C34 H34 119.7 . . ?
C35 C34 H34 119.7 . . ?
N8 C35 N4 115.91(11) . . ?
N8 C35 C34 124.16(12) . . ?
N4 C35 C34 119.87(12) . . ?
N12 C36 N8 115.59(11) . . ?
N12 C36 C37 120.05(12) . . ?
N8 C36 C37 124.08(12) . . ?
C38 C37 C36 120.22(13) . . ?
C38 C37 H37 119.9 . . ?
C36 C37 H37 119.9 . . ?
C37 C38 C39 119.30(13) . . ?
C37 C38 H38 120.4 . . ?
C39 C38 H38 120.4 . . ?
C40 C39 C38 118.29(13) . . ?
C40 C39 H39 120.9 . . ?
C38 C39 H39 120.9 . . ?
N12 C40 C39 123.55(13) . . ?
N12 C40 H40 118.2 . . ?
C39 C40 H40 118.2 . . ?
C101 C100 H41A 109.5 . . ?
C101 C100 H41B 109.5 . . ?
H41A C100 H41B 109.5 . . ?
C101 C100 H41C 109.5 . . ?
H41A C100 H41C 109.5 . . ?
H41B C100 H41C 109.5 . . ?
O100 C101 C100 108.37(12) . . ?
O100 C101 H42A 110.0 . . ?
C100 C101 H42A 110.0 . . ?
O100 C101 H42B 110.0 . . ?
C100 C101 H42B 110.0 . . ?
H42A C101 H42B 108.4 . . ?
O100 C102 C103 108.51(12) . . ?
O100 C102 H43A 110.0 . . ?
C103 C102 H43A 110.0 . . ?
O100 C102 H43B 110.0 . . ?
C103 C102 H43B 110.0 . . ?
H43A C102 H43B 108.4 . . ?
C102 C103 H44A 109.5 . . ?
C102 C103 H44B 109.5 . . ?
H44A C103 H44B 109.5 . . ?
C102 C103 H44C 109.5 . . ?
H44A C103 H44C 109.5 . . ?
H44B C103 H44C 109.5 . . ?
N3 CO1 N4 87.71(5) . . ?
N3 CO1 N1 170.69(5) . . ?
N4 CO1 N1 92.26(4) . . ?
N3 CO1 N2 89.73(5) . . ?
N4 CO1 N2 171.40(5) . . ?
N1 CO1 N2 88.94(5) . . ?
N3 CO1 CO2 85.39(3) . . ?
N4 CO1 CO2 87.40(3) . . ?
N1 CO1 CO2 85.31(3) . . ?
N2 CO1 CO2 84.22(3) . . ?
N3 CO1 CL1 95.54(3) . . ?
N4 CO1 CL1 94.09(3) . . ?
N1 CO1 CL1 93.75(3) . . ?
N2 CO1 CL1 94.32(3) . . ?
CO2 CO1 CL1 178.267(12) . . ?
N7 CO2 N5 178.91(5) . . ?
N7 CO2 N6 90.43(5) . . ?
N5 CO2 N6 90.65(5) . . ?
N7 CO2 N8 89.37(5) . . ?
N5 CO2 N8 89.55(5) . . ?
N6 CO2 N8 179.62(5) . . ?
N7 CO2 CO3 90.13(3) . . ?
N5 CO2 CO3 89.71(3) . . ?
N6 CO2 CO3 90.91(3) . . ?
N8 CO2 CO3 88.78(3) . . ?
N7 CO2 CO1 90.28(3) . . ?
N5 CO2 CO1 89.84(3) . . ?
N6 CO2 CO1 91.50(3) . . ?
N8 CO2 CO1 88.82(3) . . ?
CO3 CO2 CO1 177.557(10) . . ?
N10 CO3 N9 87.38(4) . . ?
N10 CO3 N12 170.74(5) . . ?
N9 CO3 N12 91.30(4) . . ?
N10 CO3 N11 89.84(4) . . ?
N9 CO3 N11 171.08(5) . . ?
N12 CO3 N11 90.08(4) . . ?
N10 CO3 CO2 84.02(3) . . ?
N9 CO3 CO2 86.53(3) . . ?
N12 CO3 CO2 86.75(3) . . ?
N11 CO3 CO2 84.75(3) . . ?
N10 CO3 CL2 94.55(3) . . ?
N9 CO3 CL2 96.04(3) . . ?
N12 CO3 CL2 94.70(3) . . ?
N11 CO3 CL2 92.63(3) . . ?
CO2 CO3 CL2 177.013(12) . . ?
C1 N1 C5 118.56(11) . . ?
C1 N1 CO1 120.47(9) . . ?
C5 N1 CO1 120.79(9) . . ?
C11 N2 C15 118.62(11) . . ?
C11 N2 CO1 119.17(9) . . ?
C15 N2 CO1 122.20(9) . . ?
C21 N3 C25 118.68(11) . . ?
C21 N3 CO1 119.83(9) . . ?
C25 N3 CO1 121.35(9) . . ?
C31 N4 C35 118.47(11) . . ?
C31 N4 CO1 121.83(9) . . ?
C35 N4 CO1 119.57(9) . . ?
C6 N5 C5 123.61(11) . . ?
C6 N5 CO2 119.13(9) . . ?
C5 N5 CO2 117.13(9) . . ?
C16 N6 C15 125.46(11) . . ?
C16 N6 CO2 116.84(9) . . ?
C15 N6 CO2 117.62(9) . . ?
C25 N7 C26 124.19(11) . . ?
C25 N7 CO2 117.50(9) . . ?
C26 N7 CO2 118.25(9) . . ?
C35 N8 C36 122.50(11) . . ?
C35 N8 CO2 120.13(9) . . ?
C36 N8 CO2 116.95(9) . . ?
C10 N9 C6 118.95(11) . . ?
C10 N9 CO3 120.63(9) . . ?
C6 N9 CO3 120.30(9) . . ?
C20 N10 C16 119.14(11) . . ?
C20 N10 CO3 118.68(9) . . ?
C16 N10 CO3 122.08(9) . . ?
C30 N11 C26 118.65(11) . . ?
C30 N11 CO3 120.79(9) . . ?
C26 N11 CO3 120.56(9) . . ?
C40 N12 C36 118.55(11) . . ?
C40 N12 CO3 121.40(9) . . ?
C36 N12 CO3 119.73(9) . . ?
C101 O100 C102 111.75(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
N1 C1 C2 C3 2.3(2) . . . . ?
C1 C2 C3 C4 -0.2(2) . . . . ?
C2 C3 C4 C5 -1.7(2) . . . . ?
C3 C4 C5 N1 1.69(19) . . . . ?
C3 C4 C5 N5 176.51(12) . . . . ?
N9 C6 C7 C8 2.24(19) . . . . ?
N5 C6 C7 C8 178.64(12) . . . . ?
C6 C7 C8 C9 -2.4(2) . . . . ?
C7 C8 C9 C10 0.0(2) . . . . ?
C8 C9 C10 N9 2.7(2) . . . . ?
N2 C11 C12 C13 1.8(2) . . . . ?
C11 C12 C13 C14 2.1(2) . . . . ?
C12 C13 C14 C15 -3.3(2) . . . . ?
C13 C14 C15 N2 0.7(2) . . . . ?
C13 C14 C15 N6 176.56(13) . . . . ?
N6 C16 C17 C18 169.76(13) . . . . ?
N10 C16 C17 C18 -4.5(2) . . . . ?
C16 C17 C18 C19 -0.6(2) . . . . ?
C17 C18 C19 C20 3.2(2) . . . . ?
C18 C19 C20 N10 -0.7(2) . . . . ?
N3 C21 C22 C23 1.5(2) . . . . ?
C21 C22 C23 C24 0.1(2) . . . . ?
C22 C23 C24 C25 -1.6(2) . . . . ?
C23 C24 C25 N7 176.50(12) . . . . ?
C23 C24 C25 N3 1.62(19) . . . . ?
N11 C26 C27 C28 -2.17(19) . . . . ?
N7 C26 C27 C28 172.67(12) . . . . ?
C26 C27 C28 C29 -1.2(2) . . . . ?
C27 C28 C29 C30 1.8(2) . . . . ?
C28 C29 C30 N11 1.1(2) . . . . ?
N4 C31 C32 C33 3.6(2) . . . . ?
C31 C32 C33 C34 -1.3(2) . . . . ?
C32 C33 C34 C35 -2.2(2) . . . . ?
C33 C34 C35 N8 -179.32(13) . . . . ?
C33 C34 C35 N4 3.7(2) . . . . ?
N12 C36 C37 C38 1.2(2) . . . . ?
N8 C36 C37 C38 174.73(13) . . . . ?
C36 C37 C38 C39 0.9(2) . . . . ?
C37 C38 C39 C40 -2.1(2) . . . . ?
C38 C39 C40 N12 1.3(2) . . . . ?
C2 C1 N1 C5 -2.4(2) . . . . ?
C2 C1 N1 CO1 -177.53(10) . . . . ?
N5 C5 N1 C1 -174.97(11) . . . . ?
C4 C5 N1 C1 0.31(18) . . . . ?
N5 C5 N1 CO1 0.19(15) . . . . ?
C4 C5 N1 CO1 175.47(9) . . . . ?
C12 C11 N2 C15 -4.3(2) . . . . ?
C12 C11 N2 CO1 174.81(11) . . . . ?
N6 C15 N2 C11 -173.23(11) . . . . ?
C14 C15 N2 C11 3.00(18) . . . . ?
N6 C15 N2 CO1 7.64(15) . . . . ?
C14 C15 N2 CO1 -176.13(9) . . . . ?
C22 C21 N3 C25 -1.5(2) . . . . ?
C22 C21 N3 CO1 -177.34(11) . . . . ?
N7 C25 N3 C21 -175.41(12) . . . . ?
C24 C25 N3 C21 -0.09(18) . . . . ?
N7 C25 N3 CO1 0.36(15) . . . . ?
C24 C25 N3 CO1 175.68(9) . . . . ?
C32 C31 N4 C35 -2.07(19) . . . . ?
C32 C31 N4 CO1 173.78(10) . . . . ?
N8 C35 N4 C31 -178.81(11) . . . . ?
C34 C35 N4 C31 -1.58(18) . . . . ?
N8 C35 N4 CO1 5.25(15) . . . . ?
C34 C35 N4 CO1 -177.52(9) . . . . ?
N9 C6 N5 C5 -157.79(12) . . . . ?
C7 C6 N5 C5 25.68(19) . . . . ?
N9 C6 N5 CO2 17.92(14) . . . . ?
C7 C6 N5 CO2 -158.62(10) . . . . ?
N1 C5 N5 C6 -157.10(12) . . . . ?
C4 C5 N5 C6 27.86(19) . . . . ?
N1 C5 N5 CO2 27.12(14) . . . . ?
C4 C5 N5 CO2 -147.92(11) . . . . ?
N10 C16 N6 C15 -163.25(12) . . . . ?
C17 C16 N6 C15 22.3(2) . . . . ?
N10 C16 N6 CO2 20.20(15) . . . . ?
C17 C16 N6 CO2 -154.26(11) . . . . ?
N2 C15 N6 C16 -158.04(12) . . . . ?
C14 C15 N6 C16 26.0(2) . . . . ?
N2 C15 N6 CO2 18.49(15) . . . . ?
C14 C15 N6 CO2 -157.51(11) . . . . ?
N3 C25 N7 C26 -157.56(12) . . . . ?
C24 C25 N7 C26 27.3(2) . . . . ?
N3 C25 N7 CO2 25.32(14) . . . . ?
C24 C25 N7 CO2 -149.78(11) . . . . ?
N11 C26 N7 C25 -157.19(12) . . . . ?
C27 C26 N7 C25 27.7(2) . . . . ?
N11 C26 N7 CO2 19.91(14) . . . . ?
C27 C26 N7 CO2 -155.17(10) . . . . ?
N4 C35 N8 C36 -153.10(12) . . . . ?
C34 C35 N8 C36 29.81(19) . . . . ?
N4 C35 N8 CO2 19.28(15) . . . . ?
C34 C35 N8 CO2 -157.82(10) . . . . ?
N12 C36 N8 C35 -157.68(12) . . . . ?
C37 C36 N8 C35 28.6(2) . . . . ?
N12 C36 N8 CO2 29.72(14) . . . . ?
C37 C36 N8 CO2 -144.05(11) . . . . ?
C9 C10 N9 C6 -2.92(19) . . . . ?
C9 C10 N9 CO3 173.17(10) . . . . ?
N5 C6 N9 C10 -176.35(11) . . . . ?
C7 C6 N9 C10 0.37(18) . . . . ?
N5 C6 N9 CO3 7.54(15) . . . . ?
C7 C6 N9 CO3 -175.74(9) . . . . ?
C19 C20 N10 C16 -4.4(2) . . . . ?
C19 C20 N10 CO3 179.11(11) . . . . ?
N6 C16 N10 C20 -167.95(12) . . . . ?
C17 C16 N10 C20 6.90(18) . . . . ?
N6 C16 N10 CO3 8.40(15) . . . . ?
C17 C16 N10 CO3 -176.75(9) . . . . ?
C29 C30 N11 C26 -4.42(19) . . . . ?
C29 C30 N11 CO3 176.21(10) . . . . ?
N7 C26 N11 C30 -170.45(11) . . . . ?
C27 C26 N11 C30 4.88(18) . . . . ?
N7 C26 N11 CO3 8.92(15) . . . . ?
C27 C26 N11 CO3 -175.75(9) . . . . ?
C39 C40 N12 C36 0.8(2) . . . . ?
C39 C40 N12 CO3 -172.67(11) . . . . ?
N8 C36 N12 C40 -176.06(12) . . . . ?
C37 C36 N12 C40 -2.02(18) . . . . ?
N8 C36 N12 CO3 -2.50(15) . . . . ?
C37 C36 N12 CO3 171.54(10) . . . . ?
C100 C101 O100 C102 -176.64(11) . . . . ?
C103 C102 O100 C101 169.88(12) . . . . ?

_refine_diff_density_max         0.361
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.059


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: DMF, ether'
####################################################################### 
# 
# 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_4-CLCH22-120K
_database_code_depnum_ccdc_archive 'CCDC 1865587'
_audit_update_record             
;
2018-09-03 deposited with the CCDC.
2018-11-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C40 H32 Co3 I2 N12, C2 H4 Cl2'
_chemical_formula_sum            'C42 H36 Cl2 Co3 I2 N12'
_chemical_formula_weight         1210.32

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'
Cl Cl 0.1484 0.1585 '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'
I I -0.4742 1.8119 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/n'
_space_group_name_Hall           '-P 2yac'

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

_cell_length_a                   13.0708(7)
_cell_length_b                   11.5118(6)
_cell_length_c                   14.2242(8)
_cell_angle_alpha                90
_cell_angle_beta                 94.580(2)
_cell_angle_gamma                90
_cell_volume                     2133.5(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9891
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      27.49

_exptl_crystal_description       needle
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.884
_exptl_crystal_F_000             1186
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.049
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.013
_exptl_absorpt_coefficient_mu    2.774
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6550
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS (Bruker, 2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            46630
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.769
_diffrn_reflns_theta_max         27.520
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4914
_reflns_number_gt                4218
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2014)'
_computing_publication_material  'SHELXL-2016/4 (Sheldrick, 2016)'
_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)+(0.0179P)²+4.1520P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_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_number_reflns         4914
_refine_ls_number_parameters     321
_refine_ls_number_restraints     56
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0226
_refine_ls_wR_factor_ref         0.0534
_refine_ls_wR_factor_gt          0.0505
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.004
_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
C1 C 0.93278(18) 0.0739(2) 0.11803(17) 0.0151(5) Uani 1 1 d . . . . .
H1 H 1.002404 0.097820 0.118780 0.018 Uiso 1 1 calc R U . . .
C2 C 0.90979(19) -0.0400(2) 0.09676(18) 0.0188(5) Uani 1 1 d . . . . .
H2 H 0.961700 -0.092281 0.080315 0.023 Uiso 1 1 calc R U . . .
C3 C 0.8089(2) -0.0771(2) 0.09983(19) 0.0214(5) Uani 1 1 d . . . . .
H3 H 0.790969 -0.155827 0.086858 0.026 Uiso 1 1 calc R U . . .
C4 C 0.73535(18) 0.0018(2) 0.12194(18) 0.0171(5) Uani 1 1 d . . . . .
H4 H 0.666337 -0.022685 0.125391 0.021 Uiso 1 1 calc R U . . .
C5 C 0.76232(17) 0.11869(19) 0.13945(15) 0.0107(4) Uani 1 1 d . . . . .
C6 C 0.43483(17) 0.2807(2) 0.17726(17) 0.0142(5) Uani 1 1 d . . . . .
H6 H 0.396032 0.325605 0.217741 0.017 Uiso 1 1 calc R U . . .
C7 C 0.38654(19) 0.2402(2) 0.09458(18) 0.0198(5) Uani 1 1 d . . . . .
H7 H 0.316006 0.256010 0.078324 0.024 Uiso 1 1 calc R U . . .
C8 C 0.4439(2) 0.1752(2) 0.03518(18) 0.0217(5) Uani 1 1 d . . . . .
H8 H 0.412004 0.143778 -0.021569 0.026 Uiso 1 1 calc R U . . .
C9 C 0.54625(19) 0.1563(2) 0.05835(17) 0.0178(5) Uani 1 1 d . . . . .
H9 H 0.585831 0.113229 0.017331 0.021 Uiso 1 1 calc R U . . .
C10 C 0.59240(17) 0.20147(19) 0.14368(16) 0.0112(4) Uani 1 1 d . . . . .
C11 C 0.96645(17) 0.5617(2) 0.17507(16) 0.0138(5) Uani 1 1 d . . . . .
H11 H 0.994609 0.540112 0.118053 0.017 Uiso 1 1 calc R U . . .
C12 C 0.9807(2) 0.6740(2) 0.20678(18) 0.0184(5) Uani 1 1 d . . . . .
H12 H 1.019175 0.727685 0.173128 0.022 Uiso 1 1 calc R U . . .
C13 C 0.9380(2) 0.7072(2) 0.28863(18) 0.0203(5) Uani 1 1 d . . . . .
H13 H 0.947802 0.783802 0.312527 0.024 Uiso 1 1 calc R U . . .
C14 C 0.88115(19) 0.6281(2) 0.33499(17) 0.0166(5) Uani 1 1 d . . . . .
H14 H 0.850457 0.650266 0.390614 0.020 Uiso 1 1 calc R U . . .
C15 C 0.86863(16) 0.51420(19) 0.29969(15) 0.0103(4) Uani 1 1 d . . . . .
C16 C 0.83126(18) 0.3447(2) -0.02685(16) 0.0137(5) Uani 1 1 d . . . . .
H16 H 0.891970 0.301898 -0.035370 0.016 Uiso 1 1 calc R U . . .
C17 C 0.76959(19) 0.3762(2) -0.10549(17) 0.0177(5) Uani 1 1 d . . . . .
H17 H 0.787882 0.356223 -0.166742 0.021 Uiso 1 1 calc R U . . .
C18 C 0.68012(19) 0.4378(2) -0.09394(17) 0.0173(5) Uani 1 1 d . . . . .
H18 H 0.636612 0.461480 -0.147182 0.021 Uiso 1 1 calc R U . . .
C19 C 0.65556(18) 0.4639(2) -0.00415(16) 0.0150(5) Uani 1 1 d . . . . .
H19 H 0.594889 0.506530 0.004862 0.018 Uiso 1 1 calc R U . . .
C20 C 0.71983(17) 0.42773(19) 0.07442(16) 0.0103(4) Uani 1 1 d . . . . .
Co1 Co 0.89929(2) 0.31736(3) 0.17321(2) 0.00822(7) Uani 1 1 d . . . . .
Co2 Co 0.750000 0.31834(4) 0.250000 0.00851(9) Uani 1 2 d S T P . .
I1 I 1.08706(2) 0.31947(2) 0.07852(2) 0.01633(5) Uani 1 1 d . . . . .
N1 N 0.86187(14) 0.15411(16) 0.13797(13) 0.0102(4) Uani 1 1 d . . . . .
N2 N 0.53487(14) 0.26010(16) 0.20428(13) 0.0104(4) Uani 1 1 d . . . . .
N3 N 0.91453(14) 0.48061(16) 0.22075(13) 0.0098(4) Uani 1 1 d . . . . .
N4 N 0.80987(14) 0.37154(16) 0.06212(13) 0.0102(4) Uani 1 1 d . . . . .
N5 N 0.69536(14) 0.20067(16) 0.16776(13) 0.0103(4) Uani 1 1 d . . . . .
N6 N 0.69499(14) 0.43363(16) 0.16593(13) 0.0104(4) Uani 1 1 d . . . . .
Cl1 Cl 0.1679(8) -0.0903(9) 0.3292(6) 0.083(4) Uani 0.232(2) 1 d D U P A -1
C21 C 0.2591(12) 0.0018(14) 0.3317(10) 0.052(3) Uani 0.232(2) 1 d D U P A -1
H21A H 0.237186 0.072527 0.364192 0.062 Uiso 0.232(2) 1 calc R U P A -1
H21B H 0.318676 -0.030928 0.370171 0.062 Uiso 0.232(2) 1 calc R U P A -1
C22 C 0.2934(13) 0.0364(11) 0.2395(12) 0.042(3) Uani 0.232(2) 1 d D U P A -1
H22A H 0.334177 0.108802 0.247026 0.050 Uiso 0.232(2) 1 calc R U P A -1
H22B H 0.232742 0.052476 0.195237 0.050 Uiso 0.232(2) 1 calc R U P A -1
Cl2 Cl 0.3690(6) -0.0737(9) 0.1916(7) 0.068(3) Uani 0.232(2) 1 d D U P A -1
Cl3 Cl 0.2856(9) -0.0790(12) 0.3662(9) 0.075(5) Uani 0.268(2) 1 d D U P A -2
C23 C 0.2891(15) 0.0384(11) 0.2840(11) 0.026(4) Uiso 0.268(2) 1 d D U P A -2
H23A H 0.294084 0.113253 0.318266 0.031 Uiso 0.268(2) 1 calc R U P A -2
H23B H 0.350026 0.030623 0.247364 0.031 Uiso 0.268(2) 1 calc R U P A -2
C24 C 0.1950(16) 0.0363(12) 0.2197(12) 0.030(4) Uiso 0.268(2) 1 d D U P A -2
H24A H 0.188099 0.110743 0.184864 0.036 Uiso 0.268(2) 1 calc R U P A -2
H24B H 0.134453 0.027405 0.256665 0.036 Uiso 0.268(2) 1 calc R U P A -2
Cl4 Cl 0.1992(6) -0.0814(7) 0.1376(7) 0.0269(13) Uani 0.268(2) 1 d D . 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
C1 N1 1.354(3) . ?
C1 C2 1.374(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.390(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.377(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.408(3) . ?
C4 H4 0.9500 . ?
C5 N1 1.365(3) . ?
C5 N5 1.369(3) . ?
C6 N2 1.354(3) . ?
C6 C7 1.371(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.392(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.369(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.411(3) . ?
C9 H9 0.9500 . ?
C10 N5 1.362(3) . ?
C10 N2 1.366(3) . ?
C11 N3 1.351(3) . ?
C11 C12 1.377(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.385(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.376(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.409(3) . ?
C14 H14 0.9500 . ?
C15 N6 1.362(3) 2_655 ?
C15 N3 1.370(3) . ?
C16 N4 1.353(3) . ?
C16 C17 1.374(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.388(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.375(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.406(3) . ?
C19 H19 0.9500 . ?
C20 N4 1.366(3) . ?
C20 N6 1.368(3) . ?
Co1 N4 1.9892(18) . ?
Co1 N2 1.9931(19) 2_655 ?
Co1 N1 1.9958(19) . ?
Co1 N3 2.0017(19) . ?
Co1 Co2 2.3111(3) . ?
Co1 I1 2.8925(4) . ?
Co2 N6 1.8898(19) . ?
Co2 N6 1.8898(19) 2_655 ?
Co2 N5 1.8921(19) . ?
Co2 N5 1.8921(19) 2_655 ?
Cl1 C21 1.594(15) . ?
C21 C22 1.474(14) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 Cl2 1.776(13) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
Cl3 C23 1.790(11) . ?
C23 C24 1.473(12) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 Cl4 1.792(11) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?

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
N1 C1 C2 123.8(2) . . ?
N1 C1 H1 118.1 . . ?
C2 C1 H1 118.1 . . ?
C1 C2 C3 118.6(2) . . ?
C1 C2 H2 120.7 . . ?
C3 C2 H2 120.7 . . ?
C4 C3 C2 119.0(2) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C3 C4 C5 120.1(2) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
N1 C5 N5 115.53(19) . . ?
N1 C5 C4 120.5(2) . . ?
N5 C5 C4 123.6(2) . . ?
N2 C6 C7 123.5(2) . . ?
N2 C6 H6 118.3 . . ?
C7 C6 H6 118.3 . . ?
C6 C7 C8 118.0(2) . . ?
C6 C7 H7 121.0 . . ?
C8 C7 H7 121.0 . . ?
C9 C8 C7 120.2(2) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C8 C9 C10 119.4(2) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
N5 C10 N2 115.29(19) . . ?
N5 C10 C9 124.0(2) . . ?
N2 C10 C9 120.4(2) . . ?
N3 C11 C12 123.5(2) . . ?
N3 C11 H11 118.3 . . ?
C12 C11 H11 118.3 . . ?
C11 C12 C13 118.8(2) . . ?
C11 C12 H12 120.6 . . ?
C13 C12 H12 120.6 . . ?
C14 C13 C12 119.3(2) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C13 C14 C15 119.8(2) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
N6 C15 N3 114.94(19) 2_655 . ?
N6 C15 C14 124.2(2) 2_655 . ?
N3 C15 C14 120.6(2) . . ?
N4 C16 C17 123.3(2) . . ?
N4 C16 H16 118.3 . . ?
C17 C16 H16 118.3 . . ?
C16 C17 C18 118.9(2) . . ?
C16 C17 H17 120.5 . . ?
C18 C17 H17 120.5 . . ?
C19 C18 C17 118.9(2) . . ?
C19 C18 H18 120.6 . . ?
C17 C18 H18 120.6 . . ?
C18 C19 C20 120.3(2) . . ?
C18 C19 H19 119.8 . . ?
C20 C19 H19 119.8 . . ?
N4 C20 N6 114.68(19) . . ?
N4 C20 C19 120.3(2) . . ?
N6 C20 C19 124.7(2) . . ?
N4 Co1 N2 169.59(8) . 2_655 ?
N4 Co1 N1 88.80(8) . . ?
N2 Co1 N1 89.33(8) 2_655 . ?
N4 Co1 N3 90.59(7) . . ?
N2 Co1 N3 89.47(7) 2_655 . ?
N1 Co1 N3 169.95(8) . . ?
N4 Co1 Co2 84.79(5) . . ?
N2 Co1 Co2 84.86(5) 2_655 . ?
N1 Co1 Co2 85.64(6) . . ?
N3 Co1 Co2 84.31(5) . . ?
N4 Co1 I1 95.39(5) . . ?
N2 Co1 I1 94.98(5) 2_655 . ?
N1 Co1 I1 95.22(5) . . ?
N3 Co1 I1 94.83(5) . . ?
Co2 Co1 I1 179.118(16) . . ?
N6 Co2 N6 90.77(11) . 2_655 ?
N6 Co2 N5 90.34(8) . . ?
N6 Co2 N5 178.85(8) 2_655 . ?
N6 Co2 N5 178.85(8) . 2_655 ?
N6 Co2 N5 90.33(8) 2_655 2_655 ?
N5 Co2 N5 88.56(11) . 2_655 ?
N6 Co2 Co1 90.55(6) . 2_655 ?
N6 Co2 Co1 89.84(6) 2_655 2_655 ?
N5 Co2 Co1 89.85(6) . 2_655 ?
N5 Co2 Co1 89.75(6) 2_655 2_655 ?
N6 Co2 Co1 89.84(6) . . ?
N6 Co2 Co1 90.55(6) 2_655 . ?
N5 Co2 Co1 89.75(6) . . ?
N5 Co2 Co1 89.85(6) 2_655 . ?
Co1 Co2 Co1 179.44(2) 2_655 . ?
C1 N1 C5 117.95(19) . . ?
C1 N1 Co1 122.44(16) . . ?
C5 N1 Co1 119.48(15) . . ?
C6 N2 C10 118.36(19) . . ?
C6 N2 Co1 122.00(16) . 2_655 ?
C10 N2 Co1 119.60(15) . 2_655 ?
C11 N3 C15 117.96(19) . . ?
C11 N3 Co1 121.77(15) . . ?
C15 N3 Co1 120.23(15) . . ?
C16 N4 C20 118.17(19) . . ?
C16 N4 Co1 121.27(15) . . ?
C20 N4 Co1 120.28(15) . . ?
C10 N5 C5 124.93(19) . . ?
C10 N5 Co2 117.85(15) . . ?
C5 N5 Co2 117.18(15) . . ?
C15 N6 C20 124.99(19) 2_655 . ?
C15 N6 Co2 117.60(15) 2_655 . ?
C20 N6 Co2 117.39(15) . . ?
C22 C21 Cl1 116.1(11) . . ?
C22 C21 H21A 108.3 . . ?
Cl1 C21 H21A 108.2 . . ?
C22 C21 H21B 108.2 . . ?
Cl1 C21 H21B 108.2 . . ?
H21A C21 H21B 107.4 . . ?
C21 C22 Cl2 111.5(10) . . ?
C21 C22 H22A 109.3 . . ?
Cl2 C22 H22A 109.3 . . ?
C21 C22 H22B 109.3 . . ?
Cl2 C22 H22B 109.3 . . ?
H22A C22 H22B 108.0 . . ?
C24 C23 Cl3 109.3(10) . . ?
C24 C23 H23A 109.8 . . ?
Cl3 C23 H23A 109.8 . . ?
C24 C23 H23B 109.8 . . ?
Cl3 C23 H23B 109.8 . . ?
H23A C23 H23B 108.3 . . ?
C23 C24 Cl4 110.4(10) . . ?
C23 C24 H24A 109.6 . . ?
Cl4 C24 H24A 109.6 . . ?
C23 C24 H24B 109.6 . . ?
Cl4 C24 H24B 109.6 . . ?
H24A C24 H24B 108.1 . . ?

_refine_diff_density_max         0.534
_refine_diff_density_min         -0.590
_refine_diff_density_rms         0.084


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dichloroethane'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_3-Et2O-298K
_database_code_depnum_ccdc_archive 'CCDC 1865585'
_audit_update_record             
;
2018-09-03 deposited with the CCDC.
2018-11-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C40 H32 Br2 Co3 N12, C4 H10 O'
_chemical_formula_sum            'C44 H42 Br2 Co3 N12 O'
_chemical_formula_weight         1091.50

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   16.1426(14)
_cell_length_b                   15.8923(14)
_cell_length_c                   17.1821(15)
_cell_angle_alpha                90
_cell_angle_beta                 99.607(4)
_cell_angle_gamma                90
_cell_volume                     4346.1(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9205
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      28.50

_exptl_crystal_description       block
_exptl_crystal_colour            'light brown'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_F_000             2196
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.87
_exptl_crystal_size_mid          0.78
_exptl_crystal_size_min          0.44
_exptl_absorpt_coefficient_mu    3.022
_shelx_estimated_absorpt_T_min   0.179
_shelx_estimated_absorpt_T_max   0.350
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6968
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   'SADABS (Bruker, 2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            154061
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.757
_diffrn_reflns_theta_max         28.724
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             11240
_reflns_number_gt                8787
_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       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_structure_solution    'SHELXS2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_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)+(0.0752P)²+8.8092P] 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_number_reflns         11240
_refine_ls_number_parameters     561
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0431
_refine_ls_wR_factor_ref         0.1427
_refine_ls_wR_factor_gt          0.1293
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_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
C1 C 0.4789(2) 0.4759(2) 0.7254(2) 0.0396(8) Uani 1 1 d . . . . .
H1 H 0.459056 0.524497 0.746230 0.048 Uiso 1 1 calc R U . . .
C1S C 0.1681(4) 0.4533(4) 0.6151(4) 0.0841(19) Uani 1 1 d . . . . .
H1SA H 0.131106 0.494502 0.631561 0.126 Uiso 1 1 calc R U . . .
H1SB H 0.139126 0.422961 0.570442 0.126 Uiso 1 1 calc R U . . .
H1SC H 0.216269 0.481026 0.600804 0.126 Uiso 1 1 calc R U . . .
C2 C 0.4223(2) 0.4242(3) 0.6806(3) 0.0459(9) Uani 1 1 d . . . . .
H2 H 0.365244 0.436929 0.672252 0.055 Uiso 1 1 calc R U . . .
C2S C 0.1959(3) 0.3937(3) 0.6810(3) 0.0530(11) Uani 1 1 d . . . . .
H2SA H 0.147921 0.363312 0.694059 0.064 Uiso 1 1 calc R U . . .
H2SB H 0.235115 0.353214 0.665633 0.064 Uiso 1 1 calc R U . . .
C3 C 0.4511(2) 0.3528(3) 0.6480(2) 0.0428(9) Uani 1 1 d . . . . .
H3 H 0.413754 0.316744 0.617231 0.051 Uiso 1 1 calc R U . . .
C3S C 0.2729(3) 0.3881(3) 0.8101(3) 0.0536(11) Uani 1 1 d . . . . .
H3SA H 0.313582 0.351100 0.792038 0.064 Uiso 1 1 calc R U . . .
H3SB H 0.230462 0.353697 0.828491 0.064 Uiso 1 1 calc R U . . .
C4 C 0.5361(2) 0.3357(2) 0.6615(2) 0.0356(7) Uani 1 1 d . . . . .
H4 H 0.556308 0.288297 0.638997 0.043 Uiso 1 1 calc R U . . .
C4S C 0.3154(4) 0.4426(4) 0.8755(3) 0.0727(15) Uani 1 1 d . . . . .
H4SA H 0.359113 0.474349 0.857516 0.109 Uiso 1 1 calc R U . . .
H4SB H 0.339191 0.408032 0.919366 0.109 Uiso 1 1 calc R U . . .
H4SC H 0.275089 0.480440 0.891615 0.109 Uiso 1 1 calc R U . . .
C5 C 0.5921(2) 0.38939(19) 0.70912(19) 0.0266(6) Uani 1 1 d . . . . .
C6 C 0.7165(2) 0.30454(18) 0.72168(18) 0.0263(6) Uani 1 1 d . . . . .
C7 C 0.6839(3) 0.2265(2) 0.7404(2) 0.0389(8) Uani 1 1 d . . . . .
H7 H 0.628598 0.223322 0.748991 0.047 Uiso 1 1 calc R U . . .
C8 C 0.7315(3) 0.1557(2) 0.7460(3) 0.0471(10) Uani 1 1 d . . . . .
H8 H 0.708487 0.104017 0.756197 0.057 Uiso 1 1 calc R U . . .
C9 C 0.8154(3) 0.1613(2) 0.7364(3) 0.0505(10) Uani 1 1 d . . . . .
H9 H 0.850205 0.114296 0.742682 0.061 Uiso 1 1 calc R U . . .
C10 C 0.8451(3) 0.2388(2) 0.7172(2) 0.0391(8) Uani 1 1 d . . . . .
H10 H 0.901057 0.242878 0.710736 0.047 Uiso 1 1 calc R U . . .
C11 C 0.5771(2) 0.6938(2) 0.7104(2) 0.0387(8) Uani 1 1 d . . . . .
H11 H 0.561796 0.710353 0.757888 0.046 Uiso 1 1 calc R U . . .
C12 C 0.5551(3) 0.7445(2) 0.6461(3) 0.0471(10) Uani 1 1 d . . . . .
H12 H 0.523006 0.792593 0.649302 0.056 Uiso 1 1 calc R U . . .
C13 C 0.5817(3) 0.7229(2) 0.5760(3) 0.0473(10) Uani 1 1 d . . . . .
H13 H 0.568616 0.756856 0.531526 0.057 Uiso 1 1 calc R U . . .
C14 C 0.6275(3) 0.6507(2) 0.5735(2) 0.0387(8) Uani 1 1 d . . . . .
H14 H 0.647657 0.636491 0.527574 0.046 Uiso 1 1 calc R U . . .
C15 C 0.64445(19) 0.59759(19) 0.64011(19) 0.0267(6) Uani 1 1 d . . . . .
C16 C 0.6882(2) 0.47453(19) 0.57669(18) 0.0267(6) Uani 1 1 d . . . . .
C17 C 0.6204(2) 0.4707(2) 0.5136(2) 0.0397(8) Uani 1 1 d . . . . .
H17 H 0.575088 0.507070 0.512575 0.048 Uiso 1 1 calc R U . . .
C18 C 0.6205(3) 0.4136(3) 0.4538(2) 0.0477(10) Uani 1 1 d . . . . .
H18 H 0.574892 0.409716 0.412963 0.057 Uiso 1 1 calc R U . . .
C19 C 0.6897(3) 0.3619(3) 0.4553(2) 0.0498(10) Uani 1 1 d . . . . .
H19 H 0.692511 0.324195 0.414375 0.060 Uiso 1 1 calc R U . . .
C20 C 0.7545(3) 0.3672(2) 0.5185(2) 0.0390(8) Uani 1 1 d . . . . .
H20 H 0.800427 0.331598 0.519667 0.047 Uiso 1 1 calc R U . . .
C21 C 0.7355(3) 0.6531(2) 0.9269(2) 0.0392(8) Uani 1 1 d . . . . .
H21 H 0.687000 0.646650 0.948874 0.047 Uiso 1 1 calc R U . . .
C22 C 0.7996(3) 0.7002(3) 0.9670(2) 0.0460(9) Uani 1 1 d . . . . .
H22 H 0.794133 0.726417 1.014313 0.055 Uiso 1 1 calc R U . . .
C23 C 0.8726(3) 0.7079(2) 0.9359(2) 0.0427(9) Uani 1 1 d . . . . .
H23 H 0.917203 0.739285 0.962302 0.051 Uiso 1 1 calc R U . . .
C24 C 0.8792(2) 0.6690(2) 0.8655(2) 0.0341(7) Uani 1 1 d . . . . .
H24 H 0.928851 0.672787 0.844907 0.041 Uiso 1 1 calc R U . . .
C25 C 0.8104(2) 0.62327(18) 0.82488(18) 0.0247(6) Uani 1 1 d . . . . .
C26 C 0.86265(19) 0.59915(19) 0.70370(18) 0.0239(6) Uani 1 1 d . . . . .
C27 C 0.8933(2) 0.6805(2) 0.6923(2) 0.0342(7) Uani 1 1 d . . . . .
H27 H 0.879855 0.724913 0.723176 0.041 Uiso 1 1 calc R U . . .
C28 C 0.9425(3) 0.6944(2) 0.6365(2) 0.0421(9) Uani 1 1 d . . . . .
H28 H 0.964569 0.747666 0.630822 0.050 Uiso 1 1 calc R U . . .
C29 C 0.9595(3) 0.6291(3) 0.5880(2) 0.0427(9) Uani 1 1 d . . . . .
H29 H 0.993232 0.637550 0.549828 0.051 Uiso 1 1 calc R U . . .
C30 C 0.9250(2) 0.5516(2) 0.5981(2) 0.0357(7) Uani 1 1 d . . . . .
H30 H 0.933762 0.508321 0.563949 0.043 Uiso 1 1 calc R U . . .
C31 C 0.6245(3) 0.4316(2) 0.9370(2) 0.0436(9) Uani 1 1 d . . . . .
H31 H 0.570687 0.454254 0.928527 0.052 Uiso 1 1 calc R U . . .
C32 C 0.6463(3) 0.3777(3) 0.9997(3) 0.0527(11) Uani 1 1 d . . . . .
H32 H 0.608848 0.365986 1.033984 0.063 Uiso 1 1 calc R U . . .
C33 C 0.7244(3) 0.3417(3) 1.0104(2) 0.0502(11) Uani 1 1 d . . . . .
H33 H 0.741180 0.306379 1.053288 0.060 Uiso 1 1 calc R U . . .
C34 C 0.7781(3) 0.3578(2) 0.9579(2) 0.0411(8) Uani 1 1 d . . . . .
H34 H 0.829894 0.330902 0.963477 0.049 Uiso 1 1 calc R U . . .
C35 C 0.7543(2) 0.41534(19) 0.89534(18) 0.0277(6) Uani 1 1 d . . . . .
C36 C 0.8865(2) 0.42713(19) 0.84698(19) 0.0270(6) Uani 1 1 d . . . . .
C37 C 0.9428(2) 0.4291(2) 0.9195(2) 0.0398(8) Uani 1 1 d . . . . .
H37 H 0.922296 0.427167 0.966950 0.048 Uiso 1 1 calc R U . . .
C38 C 1.0279(3) 0.4339(3) 0.9198(3) 0.0482(10) Uani 1 1 d . . . . .
H38 H 1.064922 0.434563 0.967476 0.058 Uiso 1 1 calc R U . . .
C39 C 1.0584(2) 0.4376(3) 0.8495(3) 0.0501(10) Uani 1 1 d . . . . .
H39 H 1.115659 0.443545 0.848934 0.060 Uiso 1 1 calc R U . . .
C40 C 1.0020(2) 0.4323(2) 0.7805(2) 0.0386(8) Uani 1 1 d . . . . .
H40 H 1.022449 0.434036 0.732988 0.046 Uiso 1 1 calc R U . . .
N1 N 0.56230(17) 0.45980(17) 0.74105(17) 0.0296(6) Uani 1 1 d . . . . .
N2 N 0.61994(17) 0.62059(16) 0.70881(17) 0.0280(5) Uani 1 1 d . . . . .
N3 N 0.73876(17) 0.61527(16) 0.85639(16) 0.0275(5) Uani 1 1 d . . . . .
N4 N 0.67748(18) 0.45331(17) 0.88687(16) 0.0295(6) Uani 1 1 d . . . . .
N5 N 0.67695(16) 0.37997(15) 0.72244(16) 0.0248(5) Uani 1 1 d . . . . .
N6 N 0.68896(16) 0.52407(16) 0.64212(15) 0.0251(5) Uani 1 1 d . . . . .
N7 N 0.81176(16) 0.57909(15) 0.75694(15) 0.0243(5) Uani 1 1 d . . . . .
N8 N 0.80125(17) 0.43410(16) 0.83820(15) 0.0256(5) Uani 1 1 d . . . . .
N9 N 0.79751(17) 0.30860(16) 0.70750(16) 0.0272(5) Uani 1 1 d . . . . .
N10 N 0.75446(17) 0.42183(16) 0.57891(15) 0.0268(5) Uani 1 1 d . . . . .
N11 N 0.87908(16) 0.53505(17) 0.65539(15) 0.0259(5) Uani 1 1 d . . . . .
N12 N 0.91810(17) 0.42468(16) 0.77814(16) 0.0275(5) Uani 1 1 d . . . . .
O1S O 0.23521(18) 0.44047(18) 0.74748(18) 0.0475(7) Uani 1 1 d . . . . .
Co1 Co 0.64139(3) 0.54327(3) 0.80402(3) 0.02726(11) Uani 1 1 d . . . . .
Co2 Co 0.74469(2) 0.47935(2) 0.74047(2) 0.02083(10) Uani 1 1 d . . . . .
Co3 Co 0.84359(3) 0.41781(2) 0.67458(2) 0.02385(10) Uani 1 1 d . . . . .
Br1 Br 0.52883(3) 0.61314(3) 0.87853(3) 0.05208(13) Uani 1 1 d . . . . .
Br2 Br 0.95304(3) 0.34126(3) 0.60372(3) 0.05410(13) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.353(4) . ?
C1 C2 1.366(6) . ?
C1 H1 0.9300 . ?
C1S C2S 1.487(8) . ?
C1S H1SA 0.9600 . ?
C1S H1SB 0.9600 . ?
C1S H1SC 0.9600 . ?
C2 C3 1.381(6) . ?
C2 H2 0.9300 . ?
C2S O1S 1.420(5) . ?
C2S H2SA 0.9700 . ?
C2S H2SB 0.9700 . ?
C3 C4 1.379(5) . ?
C3 H3 0.9300 . ?
C3S O1S 1.414(5) . ?
C3S C4S 1.492(7) . ?
C3S H3SA 0.9700 . ?
C3S H3SB 0.9700 . ?
C4 C5 1.403(5) . ?
C4 H4 0.9300 . ?
C4S H4SA 0.9600 . ?
C4S H4SB 0.9600 . ?
C4S H4SC 0.9600 . ?
C5 N5 1.359(4) . ?
C5 N1 1.368(4) . ?
C6 N5 1.360(4) . ?
C6 N9 1.371(4) . ?
C6 C7 1.405(4) . ?
C7 C8 1.358(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.393(6) . ?
C8 H8 0.9300 . ?
C9 C10 1.382(6) . ?
C9 H9 0.9300 . ?
C10 N9 1.344(4) . ?
C10 H10 0.9300 . ?
C11 N2 1.356(4) . ?
C11 C12 1.365(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.388(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.371(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.411(5) . ?
C14 H14 0.9300 . ?
C15 N2 1.356(4) . ?
C15 N6 1.369(4) . ?
C16 N10 1.354(4) . ?
C16 N6 1.371(4) . ?
C16 C17 1.408(5) . ?
C17 C18 1.371(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.384(6) . ?
C18 H18 0.9300 . ?
C19 C20 1.379(6) . ?
C19 H19 0.9300 . ?
C20 N10 1.353(4) . ?
C20 H20 0.9300 . ?
C21 N3 1.361(4) . ?
C21 C22 1.367(6) . ?
C21 H21 0.9300 . ?
C22 C23 1.378(6) . ?
C22 H22 0.9300 . ?
C23 C24 1.379(5) . ?
C23 H23 0.9300 . ?
C24 C25 1.411(5) . ?
C24 H24 0.9300 . ?
C25 N3 1.362(4) . ?
C25 N7 1.366(4) . ?
C26 N7 1.365(4) . ?
C26 N11 1.368(4) . ?
C26 C27 1.409(4) . ?
C27 C28 1.362(5) . ?
C27 H27 0.9300 . ?
C28 C29 1.386(6) . ?
C28 H28 0.9300 . ?
C29 C30 1.376(5) . ?
C29 H29 0.9300 . ?
C30 N11 1.353(4) . ?
C30 H30 0.9300 . ?
C31 N4 1.355(4) . ?
C31 C32 1.375(6) . ?
C31 H31 0.9300 . ?
C32 C33 1.368(7) . ?
C32 H32 0.9300 . ?
C33 C34 1.376(6) . ?
C33 H33 0.9300 . ?
C34 C35 1.414(5) . ?
C34 H34 0.9300 . ?
C35 N4 1.365(4) . ?
C35 N8 1.370(4) . ?
C36 N8 1.363(4) . ?
C36 N12 1.365(4) . ?
C36 C37 1.415(5) . ?
C37 C38 1.374(6) . ?
C37 H37 0.9300 . ?
C38 C39 1.380(7) . ?
C38 H38 0.9300 . ?
C39 C40 1.372(6) . ?
C39 H39 0.9300 . ?
C40 N12 1.354(4) . ?
C40 H40 0.9300 . ?
N1 Co1 2.025(3) . ?
N2 Co1 2.029(3) . ?
N3 Co1 2.029(3) . ?
N4 Co1 2.033(3) . ?
N5 Co2 1.916(2) . ?
N6 Co2 1.914(3) . ?
N7 Co2 1.914(2) . ?
N8 Co2 1.913(3) . ?
N9 Co3 2.007(3) . ?
N10 Co3 1.997(3) . ?
N11 Co3 1.993(3) . ?
N12 Co3 1.977(3) . ?
Co1 Co2 2.3691(6) . ?
Co1 Br1 2.6363(6) . ?
Co2 Co3 2.3218(5) . ?
Co3 Br2 2.6081(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 123.2(4) . . ?
N1 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
C2S C1S H1SA 109.5 . . ?
C2S C1S H1SB 109.5 . . ?
H1SA C1S H1SB 109.5 . . ?
C2S C1S H1SC 109.5 . . ?
H1SA C1S H1SC 109.5 . . ?
H1SB C1S H1SC 109.5 . . ?
C1 C2 C3 118.9(3) . . ?
C1 C2 H2 120.5 . . ?
C3 C2 H2 120.5 . . ?
O1S C2S C1S 108.4(4) . . ?
O1S C2S H2SA 110.0 . . ?
C1S C2S H2SA 110.0 . . ?
O1S C2S H2SB 110.0 . . ?
C1S C2S H2SB 110.0 . . ?
H2SA C2S H2SB 108.4 . . ?
C4 C3 C2 119.1(4) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
O1S C3S C4S 108.4(4) . . ?
O1S C3S H3SA 110.0 . . ?
C4S C3S H3SA 110.0 . . ?
O1S C3S H3SB 110.0 . . ?
C4S C3S H3SB 110.0 . . ?
H3SA C3S H3SB 108.4 . . ?
C3 C4 C5 120.3(4) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C3S C4S H4SA 109.5 . . ?
C3S C4S H4SB 109.5 . . ?
H4SA C4S H4SB 109.5 . . ?
C3S C4S H4SC 109.5 . . ?
H4SA C4S H4SC 109.5 . . ?
H4SB C4S H4SC 109.5 . . ?
N5 C5 N1 115.7(3) . . ?
N5 C5 C4 124.4(3) . . ?
N1 C5 C4 119.7(3) . . ?
N5 C6 N9 115.1(3) . . ?
N5 C6 C7 125.5(3) . . ?
N9 C6 C7 119.2(3) . . ?
C8 C7 C6 121.2(4) . . ?
C8 C7 H7 119.4 . . ?
C6 C7 H7 119.4 . . ?
C7 C8 C9 119.3(4) . . ?
C7 C8 H8 120.4 . . ?
C9 C8 H8 120.4 . . ?
C10 C9 C8 117.9(4) . . ?
C10 C9 H9 121.0 . . ?
C8 C9 H9 121.0 . . ?
N9 C10 C9 123.4(4) . . ?
N9 C10 H10 118.3 . . ?
C9 C10 H10 118.3 . . ?
N2 C11 C12 123.8(4) . . ?
N2 C11 H11 118.1 . . ?
C12 C11 H11 118.1 . . ?
C11 C12 C13 118.7(3) . . ?
C11 C12 H12 120.7 . . ?
C13 C12 H12 120.7 . . ?
C14 C13 C12 118.7(4) . . ?
C14 C13 H13 120.6 . . ?
C12 C13 H13 120.6 . . ?
C13 C14 C15 120.5(4) . . ?
C13 C14 H14 119.7 . . ?
C15 C14 H14 119.7 . . ?
N2 C15 N6 115.9(3) . . ?
N2 C15 C14 120.0(3) . . ?
N6 C15 C14 124.1(3) . . ?
N10 C16 N6 115.7(3) . . ?
N10 C16 C17 120.3(3) . . ?
N6 C16 C17 123.7(3) . . ?
C18 C17 C16 120.5(4) . . ?
C18 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
C17 C18 C19 118.7(4) . . ?
C17 C18 H18 120.6 . . ?
C19 C18 H18 120.6 . . ?
C20 C19 C18 118.8(4) . . ?
C20 C19 H19 120.6 . . ?
C18 C19 H19 120.6 . . ?
N10 C20 C19 123.1(4) . . ?
N10 C20 H20 118.4 . . ?
C19 C20 H20 118.4 . . ?
N3 C21 C22 123.5(3) . . ?
N3 C21 H21 118.2 . . ?
C22 C21 H21 118.2 . . ?
C21 C22 C23 118.5(3) . . ?
C21 C22 H22 120.8 . . ?
C23 C22 H22 120.8 . . ?
C22 C23 C24 119.9(3) . . ?
C22 C23 H23 120.1 . . ?
C24 C23 H23 120.1 . . ?
C23 C24 C25 119.6(3) . . ?
C23 C24 H24 120.2 . . ?
C25 C24 H24 120.2 . . ?
N3 C25 N7 115.3(3) . . ?
N3 C25 C24 120.2(3) . . ?
N7 C25 C24 124.3(3) . . ?
N7 C26 N11 115.6(3) . . ?
N7 C26 C27 124.8(3) . . ?
N11 C26 C27 119.4(3) . . ?
C28 C27 C26 120.4(3) . . ?
C28 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
C27 C28 C29 119.9(3) . . ?
C27 C28 H28 120.0 . . ?
C29 C28 H28 120.0 . . ?
C30 C29 C28 118.0(3) . . ?
C30 C29 H29 121.0 . . ?
C28 C29 H29 121.0 . . ?
N11 C30 C29 123.2(3) . . ?
N11 C30 H30 118.4 . . ?
C29 C30 H30 118.4 . . ?
N4 C31 C32 123.5(4) . . ?
N4 C31 H31 118.3 . . ?
C32 C31 H31 118.3 . . ?
C33 C32 C31 118.3(4) . . ?
C33 C32 H32 120.8 . . ?
C31 C32 H32 120.8 . . ?
C32 C33 C34 120.1(4) . . ?
C32 C33 H33 119.9 . . ?
C34 C33 H33 119.9 . . ?
C33 C34 C35 119.9(4) . . ?
C33 C34 H34 120.1 . . ?
C35 C34 H34 120.1 . . ?
N4 C35 N8 115.4(3) . . ?
N4 C35 C34 119.6(3) . . ?
N8 C35 C34 125.0(3) . . ?
N8 C36 N12 115.0(3) . . ?
N8 C36 C37 125.7(3) . . ?
N12 C36 C37 119.1(3) . . ?
C38 C37 C36 119.9(4) . . ?
C38 C37 H37 120.0 . . ?
C36 C37 H37 120.0 . . ?
C37 C38 C39 120.1(4) . . ?
C37 C38 H38 119.9 . . ?
C39 C38 H38 119.9 . . ?
C40 C39 C38 118.1(4) . . ?
C40 C39 H39 120.9 . . ?
C38 C39 H39 120.9 . . ?
N12 C40 C39 123.2(4) . . ?
N12 C40 H40 118.4 . . ?
C39 C40 H40 118.4 . . ?
C1 N1 C5 118.7(3) . . ?
C1 N1 Co1 120.0(2) . . ?
C5 N1 Co1 121.2(2) . . ?
C15 N2 C11 118.2(3) . . ?
C15 N2 Co1 120.2(2) . . ?
C11 N2 Co1 121.5(2) . . ?
C21 N3 C25 118.3(3) . . ?
C21 N3 Co1 120.1(2) . . ?
C25 N3 Co1 121.5(2) . . ?
C31 N4 C35 118.5(3) . . ?
C31 N4 Co1 119.1(3) . . ?
C35 N4 Co1 122.3(2) . . ?
C5 N5 C6 123.9(3) . . ?
C5 N5 Co2 117.9(2) . . ?
C6 N5 Co2 118.2(2) . . ?
C15 N6 C16 122.5(3) . . ?
C15 N6 Co2 120.4(2) . . ?
C16 N6 Co2 116.7(2) . . ?
C26 N7 C25 123.4(3) . . ?
C26 N7 Co2 118.9(2) . . ?
C25 N7 Co2 117.6(2) . . ?
C36 N8 C35 124.9(3) . . ?
C36 N8 Co2 116.9(2) . . ?
C35 N8 Co2 118.1(2) . . ?
C10 N9 C6 118.8(3) . . ?
C10 N9 Co3 121.2(2) . . ?
C6 N9 Co3 120.0(2) . . ?
C20 N10 C16 118.5(3) . . ?
C20 N10 Co3 121.2(2) . . ?
C16 N10 Co3 120.0(2) . . ?
C30 N11 C26 118.8(3) . . ?
C30 N11 Co3 120.6(2) . . ?
C26 N11 Co3 120.4(2) . . ?
C40 N12 C36 119.3(3) . . ?
C40 N12 Co3 119.1(2) . . ?
C36 N12 Co3 121.5(2) . . ?
C3S O1S C2S 112.4(3) . . ?
N1 Co1 N3 168.27(11) . . ?
N1 Co1 N2 87.61(11) . . ?
N3 Co1 N2 91.80(11) . . ?
N1 Co1 N4 89.70(11) . . ?
N3 Co1 N4 88.61(11) . . ?
N2 Co1 N4 168.76(11) . . ?
N1 Co1 Co2 84.39(8) . . ?
N3 Co1 Co2 83.88(7) . . ?
N2 Co1 Co2 85.79(8) . . ?
N4 Co1 Co2 83.09(8) . . ?
N1 Co1 Br1 96.39(8) . . ?
N3 Co1 Br1 95.33(8) . . ?
N2 Co1 Br1 95.61(8) . . ?
N4 Co1 Br1 95.53(8) . . ?
Co2 Co1 Br1 178.42(2) . . ?
N7 Co2 N8 90.35(11) . . ?
N7 Co2 N6 89.65(11) . . ?
N8 Co2 N6 179.39(11) . . ?
N7 Co2 N5 179.17(12) . . ?
N8 Co2 N5 90.46(11) . . ?
N6 Co2 N5 89.53(11) . . ?
N7 Co2 Co3 90.16(8) . . ?
N8 Co2 Co3 90.19(8) . . ?
N6 Co2 Co3 89.20(8) . . ?
N5 Co2 Co3 89.68(8) . . ?
N7 Co2 Co1 90.06(8) . . ?
N8 Co2 Co1 91.50(8) . . ?
N6 Co2 Co1 89.11(8) . . ?
N5 Co2 Co1 90.08(8) . . ?
Co3 Co2 Co1 178.29(2) . . ?
N12 Co3 N11 87.07(11) . . ?
N12 Co3 N10 170.24(11) . . ?
N11 Co3 N10 91.23(11) . . ?
N12 Co3 N9 89.57(11) . . ?
N11 Co3 N9 170.29(11) . . ?
N10 Co3 N9 90.55(11) . . ?
N12 Co3 Co2 84.40(8) . . ?
N11 Co3 Co2 85.81(8) . . ?
N10 Co3 Co2 85.89(8) . . ?
N9 Co3 Co2 84.80(8) . . ?
N12 Co3 Br2 95.06(8) . . ?
N11 Co3 Br2 97.07(8) . . ?
N10 Co3 Br2 94.69(8) . . ?
N9 Co3 Br2 92.29(8) . . ?
Co2 Co3 Br2 177.04(2) . . ?

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
N1 C1 C2 C3 -1.4(6) . . . . ?
C1 C2 C3 C4 0.0(6) . . . . ?
C2 C3 C4 C5 1.2(5) . . . . ?
C3 C4 C5 N5 -176.5(3) . . . . ?
C3 C4 C5 N1 -1.1(5) . . . . ?
N5 C6 C7 C8 -173.0(4) . . . . ?
N9 C6 C7 C8 1.3(5) . . . . ?
C6 C7 C8 C9 2.7(6) . . . . ?
C7 C8 C9 C10 -3.4(7) . . . . ?
C8 C9 C10 N9 0.0(7) . . . . ?
N2 C11 C12 C13 -3.6(6) . . . . ?
C11 C12 C13 C14 1.3(6) . . . . ?
C12 C13 C14 C15 2.5(6) . . . . ?
C13 C14 C15 N2 -4.2(5) . . . . ?
C13 C14 C15 N6 179.3(3) . . . . ?
N10 C16 C17 C18 0.0(5) . . . . ?
N6 C16 C17 C18 -173.5(3) . . . . ?
C16 C17 C18 C19 -2.1(6) . . . . ?
C17 C18 C19 C20 2.6(6) . . . . ?
C18 C19 C20 N10 -1.2(6) . . . . ?
N3 C21 C22 C23 -1.9(6) . . . . ?
C21 C22 C23 C24 0.4(6) . . . . ?
C22 C23 C24 C25 1.6(6) . . . . ?
C23 C24 C25 N3 -2.3(5) . . . . ?
C23 C24 C25 N7 -176.7(3) . . . . ?
N7 C26 C27 C28 -178.7(3) . . . . ?
N11 C26 C27 C28 -3.4(5) . . . . ?
C26 C27 C28 C29 2.9(6) . . . . ?
C27 C28 C29 C30 0.4(6) . . . . ?
C28 C29 C30 N11 -3.4(6) . . . . ?
N4 C31 C32 C33 -2.5(7) . . . . ?
C31 C32 C33 C34 -1.9(7) . . . . ?
C32 C33 C34 C35 3.6(6) . . . . ?
C33 C34 C35 N4 -1.2(5) . . . . ?
C33 C34 C35 N8 -177.7(4) . . . . ?
N8 C36 C37 C38 -170.4(3) . . . . ?
N12 C36 C37 C38 4.1(5) . . . . ?
C36 C37 C38 C39 0.7(6) . . . . ?
C37 C38 C39 C40 -3.1(6) . . . . ?
C38 C39 C40 N12 0.9(6) . . . . ?
C2 C1 N1 C5 1.5(5) . . . . ?
C2 C1 N1 Co1 177.2(3) . . . . ?
N5 C5 N1 C1 175.5(3) . . . . ?
C4 C5 N1 C1 -0.2(5) . . . . ?
N5 C5 N1 Co1 -0.1(4) . . . . ?
C4 C5 N1 Co1 -175.9(2) . . . . ?
N6 C15 N2 C11 178.7(3) . . . . ?
C14 C15 N2 C11 2.0(5) . . . . ?
N6 C15 N2 Co1 -4.8(4) . . . . ?
C14 C15 N2 Co1 178.4(3) . . . . ?
C12 C11 N2 C15 1.9(5) . . . . ?
C12 C11 N2 Co1 -174.5(3) . . . . ?
C22 C21 N3 C25 1.3(5) . . . . ?
C22 C21 N3 Co1 177.7(3) . . . . ?
N7 C25 N3 C21 175.7(3) . . . . ?
C24 C25 N3 C21 0.8(4) . . . . ?
N7 C25 N3 Co1 -0.7(4) . . . . ?
C24 C25 N3 Co1 -175.6(2) . . . . ?
C32 C31 N4 C35 4.9(6) . . . . ?
C32 C31 N4 Co1 -173.4(3) . . . . ?
N8 C35 N4 C31 173.9(3) . . . . ?
C34 C35 N4 C31 -3.0(5) . . . . ?
N8 C35 N4 Co1 -7.8(4) . . . . ?
C34 C35 N4 Co1 175.3(3) . . . . ?
N1 C5 N5 C6 155.4(3) . . . . ?
C4 C5 N5 C6 -29.1(5) . . . . ?
N1 C5 N5 Co2 -26.4(4) . . . . ?
C4 C5 N5 Co2 149.1(3) . . . . ?
N9 C6 N5 C5 157.2(3) . . . . ?
C7 C6 N5 C5 -28.4(5) . . . . ?
N9 C6 N5 Co2 -21.0(4) . . . . ?
C7 C6 N5 Co2 153.4(3) . . . . ?
N2 C15 N6 C16 152.0(3) . . . . ?
C14 C15 N6 C16 -31.4(5) . . . . ?
N2 C15 N6 Co2 -20.5(4) . . . . ?
C14 C15 N6 Co2 156.1(3) . . . . ?
N10 C16 N6 C15 158.0(3) . . . . ?
C17 C16 N6 C15 -28.3(5) . . . . ?
N10 C16 N6 Co2 -29.3(3) . . . . ?
C17 C16 N6 Co2 144.5(3) . . . . ?
N11 C26 N7 C25 157.6(3) . . . . ?
C27 C26 N7 C25 -26.9(5) . . . . ?
N11 C26 N7 Co2 -17.5(4) . . . . ?
C27 C26 N7 Co2 158.0(3) . . . . ?
N3 C25 N7 C26 157.7(3) . . . . ?
C24 C25 N7 C26 -27.6(5) . . . . ?
N3 C25 N7 Co2 -27.1(3) . . . . ?
C24 C25 N7 Co2 147.6(3) . . . . ?
N12 C36 N8 C35 161.5(3) . . . . ?
C37 C36 N8 C35 -23.8(5) . . . . ?
N12 C36 N8 Co2 -22.1(3) . . . . ?
C37 C36 N8 Co2 152.6(3) . . . . ?
N4 C35 N8 C36 157.5(3) . . . . ?
C34 C35 N8 C36 -25.8(5) . . . . ?
N4 C35 N8 Co2 -18.9(4) . . . . ?
C34 C35 N8 Co2 157.8(3) . . . . ?
C9 C10 N9 C6 4.0(6) . . . . ?
C9 C10 N9 Co3 -177.0(3) . . . . ?
N5 C6 N9 C10 170.3(3) . . . . ?
C7 C6 N9 C10 -4.5(5) . . . . ?
N5 C6 N9 Co3 -8.7(4) . . . . ?
C7 C6 N9 Co3 176.5(3) . . . . ?
C19 C20 N10 C16 -0.9(5) . . . . ?
C19 C20 N10 Co3 173.0(3) . . . . ?
N6 C16 N10 C20 175.5(3) . . . . ?
C17 C16 N10 C20 1.5(5) . . . . ?
N6 C16 N10 Co3 1.5(4) . . . . ?
C17 C16 N10 Co3 -172.5(3) . . . . ?
C29 C30 N11 C26 3.0(5) . . . . ?
C29 C30 N11 Co3 -172.3(3) . . . . ?
N7 C26 N11 C30 176.2(3) . . . . ?
C27 C26 N11 C30 0.5(5) . . . . ?
N7 C26 N11 Co3 -8.6(4) . . . . ?
C27 C26 N11 Co3 175.7(2) . . . . ?
C39 C40 N12 C36 3.9(5) . . . . ?
C39 C40 N12 Co3 179.9(3) . . . . ?
N8 C36 N12 C40 168.8(3) . . . . ?
C37 C36 N12 C40 -6.3(4) . . . . ?
N8 C36 N12 Co3 -7.1(4) . . . . ?
C37 C36 N12 Co3 177.8(2) . . . . ?
C4S C3S O1S C2S 177.7(4) . . . . ?
C1S C2S O1S C3S -172.7(4) . . . . ?

_refine_diff_density_max         0.788
_refine_diff_density_min         -1.812
_refine_diff_density_rms         0.104


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: DMF, ether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_3-Et2O-120K
_database_code_depnum_ccdc_archive 'CCDC 1865584'
_audit_update_record             
;
2018-09-03 deposited with the CCDC.
2018-11-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C40 H32 Br2 Co3 N12, C4 H10 O'
_chemical_formula_sum            'C44 H42 Br2 Co3 N12 O'
_chemical_formula_weight         1091.50

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'
Br Br -0.2901 2.4595 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   16.0223(3)
_cell_length_b                   15.7356(3)
_cell_length_c                   17.0502(3)
_cell_angle_alpha                90
_cell_angle_beta                 100.446(1)
_cell_angle_gamma                90
_cell_volume                     4227.46(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9501
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      36.18

_exptl_crystal_description       block
_exptl_crystal_colour            'light brown'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_F_000             2196
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    3.106
_shelx_estimated_absorpt_T_min   0.436
_shelx_estimated_absorpt_T_max   0.575
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6104
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_process_details   '(SADABS; Bruker, 2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            108719
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.829
_diffrn_reflns_theta_max         36.287
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             20351
_reflns_number_gt                16481
_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       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_structure_solution    'SHELXS2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_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)+(0.0312P)²+2.7928P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         20351
_refine_ls_number_parameters     559
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0291
_refine_ls_wR_factor_ref         0.0727
_refine_ls_wR_factor_gt          0.0685
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_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
C100 C 0.17951(11) 0.44226(11) 0.12181(9) 0.0257(3) Uani 1 1 d . . . . .
H1S1 H 0.151605 0.406436 0.077746 0.039 Uiso 1 1 calc R U . . .
H1S2 H 0.136925 0.477309 0.141180 0.039 Uiso 1 1 calc R U . . .
H1S3 H 0.221136 0.479114 0.103082 0.039 Uiso 1 1 calc R U . . .
C101 C 0.22393(10) 0.38673(9) 0.18867(9) 0.0191(3) Uani 1 1 d . . . . .
H2S1 H 0.182380 0.349027 0.207785 0.023 Uiso 1 1 calc R U . . .
H2S2 H 0.266881 0.350838 0.169556 0.023 Uiso 1 1 calc R U . . .
C102 C 0.30396(9) 0.39278(9) 0.31927(9) 0.0189(3) Uani 1 1 d . . . . .
H3S1 H 0.353526 0.361809 0.306354 0.023 Uiso 1 1 calc R U . . .
H3S2 H 0.263748 0.350699 0.334365 0.023 Uiso 1 1 calc R U . . .
C103 C 0.33221(12) 0.45316(12) 0.38729(10) 0.0300(4) Uani 1 1 d . . . . .
H4S1 H 0.359961 0.421212 0.434165 0.045 Uiso 1 1 calc R U . . .
H4S2 H 0.372290 0.494349 0.372048 0.045 Uiso 1 1 calc R U . . .
H4S3 H 0.282789 0.483273 0.399973 0.045 Uiso 1 1 calc R U . . .
O100 O 0.26382(6) 0.44028(6) 0.25173(6) 0.01660(18) Uani 1 1 d . . . . .
C1 C -0.02122(8) -0.02536(8) 0.22584(8) 0.0142(2) Uani 1 1 d . . . . .
H1 H -0.041111 0.024950 0.247161 0.017 Uiso 1 1 calc R U . . .
C2 C -0.07977(8) -0.07788(9) 0.18044(8) 0.0163(2) Uani 1 1 d . . . . .
H2 H -0.138654 -0.065041 0.172144 0.020 Uiso 1 1 calc R U . . .
C3 C -0.05043(8) -0.15033(9) 0.14699(8) 0.0150(2) Uani 1 1 d . . . . .
H3 H -0.089213 -0.187606 0.115149 0.018 Uiso 1 1 calc R U . . .
C4 C 0.03538(8) -0.16741(8) 0.16052(8) 0.0130(2) Uani 1 1 d . . . . .
H4 H 0.056059 -0.216004 0.137071 0.016 Uiso 1 1 calc R U . . .
C5 C 0.09261(8) -0.11262(7) 0.20928(7) 0.01000(19) Uani 1 1 d . . . . .
C6 C 0.21905(8) -0.19813(7) 0.22117(7) 0.01042(19) Uani 1 1 d . . . . .
C7 C 0.18551(9) -0.27748(8) 0.23883(8) 0.0147(2) Uani 1 1 d . . . . .
H7 H 0.128227 -0.281381 0.246080 0.018 Uiso 1 1 calc R U . . .
C8 C 0.23556(10) -0.34908(8) 0.24555(9) 0.0177(2) Uani 1 1 d . . . . .
H8 H 0.212747 -0.402780 0.255961 0.021 Uiso 1 1 calc R U . . .
C9 C 0.32033(10) -0.34192(8) 0.23689(9) 0.0183(2) Uani 1 1 d . . . . .
H9 H 0.356844 -0.389953 0.243578 0.022 Uiso 1 1 calc R U . . .
C10 C 0.34968(9) -0.26335(8) 0.21838(8) 0.0144(2) Uani 1 1 d . . . . .
H10 H 0.407475 -0.258421 0.213038 0.017 Uiso 1 1 calc R U . . .
C11 C 0.12561(9) -0.07043(8) 0.43606(8) 0.0145(2) Uani 1 1 d . . . . .
H11 H 0.069671 -0.047929 0.425662 0.017 Uiso 1 1 calc R U . . .
C12 C 0.14741(10) -0.12397(9) 0.50046(8) 0.0180(2) Uani 1 1 d . . . . .
H12 H 0.108347 -0.136424 0.534658 0.022 Uiso 1 1 calc R U . . .
C13 C 0.22848(10) -0.15930(8) 0.51389(8) 0.0173(2) Uani 1 1 d . . . . .
H13 H 0.246444 -0.194663 0.558950 0.021 Uiso 1 1 calc R U . . .
C14 C 0.28244(9) -0.14260(8) 0.46139(8) 0.0147(2) Uani 1 1 d . . . . .
H14 H 0.336405 -0.169402 0.468370 0.018 Uiso 1 1 calc R U . . .
C15 C 0.25783(8) -0.08580(7) 0.39727(7) 0.01041(19) Uani 1 1 d . . . . .
C16 C 0.39097(8) -0.07417(7) 0.34870(7) 0.01008(19) Uani 1 1 d . . . . .
C17 C 0.44913(9) -0.07262(8) 0.42187(8) 0.0144(2) Uani 1 1 d . . . . .
H17 H 0.428916 -0.076071 0.470821 0.017 Uiso 1 1 calc R U . . .
C18 C 0.53494(9) -0.06612(9) 0.42232(8) 0.0165(2) Uani 1 1 d . . . . .
H18 H 0.573866 -0.065475 0.471494 0.020 Uiso 1 1 calc R U . . .
C19 C 0.56463(8) -0.06049(9) 0.35039(9) 0.0169(2) Uani 1 1 d . . . . .
H19 H 0.623328 -0.053354 0.349511 0.020 Uiso 1 1 calc R U . . .
C20 C 0.50590(8) -0.06563(8) 0.28080(8) 0.0136(2) Uani 1 1 d . . . . .
H20 H 0.525663 -0.062315 0.231616 0.016 Uiso 1 1 calc R U . . .
C21 C 0.23307(9) 0.15122(8) 0.42818(8) 0.0137(2) Uani 1 1 d . . . . .
H21 H 0.183482 0.142340 0.450347 0.016 Uiso 1 1 calc R U . . .
C22 C 0.29657(9) 0.20123(9) 0.46978(8) 0.0165(2) Uani 1 1 d . . . . .
H22 H 0.290049 0.228109 0.518197 0.020 Uiso 1 1 calc R U . . .
C23 C 0.37078(9) 0.21126(9) 0.43874(8) 0.0155(2) Uani 1 1 d . . . . .
H23 H 0.415933 0.245138 0.466073 0.019 Uiso 1 1 calc R U . . .
C24 C 0.37819(8) 0.17177(8) 0.36826(7) 0.0127(2) Uani 1 1 d . . . . .
H24 H 0.429254 0.176912 0.347717 0.015 Uiso 1 1 calc R U . . .
C25 C 0.30993(8) 0.12362(7) 0.32649(7) 0.00940(18) Uani 1 1 d . . . . .
C26 C 0.36317(7) 0.09990(7) 0.20475(7) 0.00947(18) Uani 1 1 d . . . . .
C27 C 0.39402(8) 0.18273(8) 0.19460(8) 0.0132(2) Uani 1 1 d . . . . .
H27 H 0.379729 0.228192 0.226359 0.016 Uiso 1 1 calc R U . . .
C28 C 0.44457(9) 0.19763(8) 0.13898(8) 0.0154(2) Uani 1 1 d . . . . .
H28 H 0.467236 0.252692 0.133706 0.018 Uiso 1 1 calc R U . . .
C29 C 0.46233(9) 0.13113(9) 0.09025(8) 0.0156(2) Uani 1 1 d . . . . .
H29 H 0.497582 0.139758 0.051764 0.019 Uiso 1 1 calc R U . . .
C30 C 0.42723(8) 0.05262(8) 0.09963(7) 0.0131(2) Uani 1 1 d . . . . .
H30 H 0.436486 0.008172 0.064485 0.016 Uiso 1 1 calc R U . . .
C31 C 0.07503(8) 0.19216(8) 0.21305(8) 0.0134(2) Uani 1 1 d . . . . .
H31 H 0.059879 0.208465 0.262257 0.016 Uiso 1 1 calc R U . . .
C32 C 0.05144(9) 0.24457(8) 0.14809(8) 0.0166(2) Uani 1 1 d . . . . .
H32 H 0.018125 0.293869 0.151711 0.020 Uiso 1 1 calc R U . . .
C33 C 0.07769(9) 0.22344(8) 0.07676(8) 0.0172(2) Uani 1 1 d . . . . .
H33 H 0.063299 0.258707 0.031084 0.021 Uiso 1 1 calc R U . . .
C34 C 0.12479(9) 0.15066(8) 0.07372(8) 0.0151(2) Uani 1 1 d . . . . .
H34 H 0.145022 0.136786 0.026271 0.018 Uiso 1 1 calc R U . . .
C35 C 0.14323(8) 0.09638(8) 0.14091(7) 0.01042(19) Uani 1 1 d . . . . .
C36 C 0.18778(8) -0.02606(7) 0.07580(7) 0.01041(19) Uani 1 1 d . . . . .
C37 C 0.11867(9) -0.02971(9) 0.01147(8) 0.0154(2) Uani 1 1 d . . . . .
H37 H 0.071796 0.007527 0.010350 0.018 Uiso 1 1 calc R U . . .
C38 C 0.11871(9) -0.08690(9) -0.04969(8) 0.0175(2) Uani 1 1 d . . . . .
H38 H 0.071745 -0.090159 -0.092502 0.021 Uiso 1 1 calc R U . . .
C39 C 0.18873(10) -0.13991(9) -0.04779(8) 0.0178(2) Uani 1 1 d . . . . .
H39 H 0.191054 -0.179154 -0.089677 0.021 Uiso 1 1 calc R U . . .
C40 C 0.25463(9) -0.13393(8) 0.01650(7) 0.0141(2) Uani 1 1 d . . . . .
H40 H 0.302202 -0.170260 0.017754 0.017 Uiso 1 1 calc R U . . .
Br1 Br 0.02742(2) 0.11031(2) 0.37964(2) 0.01659(3) Uani 1 1 d . . . . .
Br2 Br 0.45581(2) -0.15919(2) 0.10331(2) 0.01649(3) Uani 1 1 d . . . . .
Co1 Co 0.14320(2) 0.04018(2) 0.30328(2) 0.00838(3) Uani 1 1 d . . . . .
Co2 Co 0.24629(2) -0.02216(2) 0.24158(2) 0.00774(3) Uani 1 1 d . . . . .
Co3 Co 0.34510(2) -0.08236(2) 0.17458(2) 0.00800(3) Uani 1 1 d . . . . .
N1 N 0.06314(7) -0.04161(7) 0.24167(6) 0.01058(17) Uani 1 1 d . . . . .
N2 N 0.17930(7) -0.04802(6) 0.38673(6) 0.01057(17) Uani 1 1 d . . . . .
N3 N 0.23738(7) 0.11388(6) 0.35721(6) 0.00997(17) Uani 1 1 d . . . . .
N4 N 0.11868(7) 0.11858(6) 0.21074(6) 0.01042(17) Uani 1 1 d . . . . .
N5 N 0.17869(7) -0.12200(6) 0.22280(6) 0.00972(17) Uani 1 1 d . . . . .
N6 N 0.30477(7) -0.06728(7) 0.33994(6) 0.00980(17) Uani 1 1 d . . . . .
N7 N 0.31235(7) 0.07876(6) 0.25812(6) 0.00937(16) Uani 1 1 d . . . . .
N8 N 0.18870(7) 0.02296(6) 0.14234(6) 0.01000(17) Uani 1 1 d . . . . .
N9 N 0.42150(7) -0.07516(6) 0.27859(6) 0.01003(17) Uani 1 1 d . . . . .
N10 N 0.38028(6) 0.03544(6) 0.15621(6) 0.00954(16) Uani 1 1 d . . . . .
N11 N 0.25527(7) -0.07915(7) 0.07793(6) 0.01046(17) Uani 1 1 d . . . . .
N12 N 0.30041(7) -0.19286(6) 0.20741(6) 0.01018(17) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C100 C101 1.508(2) . ?
C100 H1S1 0.9800 . ?
C100 H1S2 0.9800 . ?
C100 H1S3 0.9800 . ?
C101 O100 1.4232(17) . ?
C101 H2S1 0.9900 . ?
C101 H2S2 0.9900 . ?
C102 O100 1.4248(17) . ?
C102 C103 1.504(2) . ?
C102 H3S1 0.9900 . ?
C102 H3S2 0.9900 . ?
C103 H4S1 0.9800 . ?
C103 H4S2 0.9800 . ?
C103 H4S3 0.9800 . ?
C1 N1 1.3538(16) . ?
C1 C2 1.3781(19) . ?
C1 H1 0.9500 . ?
C2 C3 1.394(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.3786(19) . ?
C3 H3 0.9500 . ?
C4 C5 1.4138(17) . ?
C4 H4 0.9500 . ?
C5 N5 1.3645(16) . ?
C5 N1 1.3678(16) . ?
C6 N5 1.3640(15) . ?
C6 N12 1.3683(16) . ?
C6 C7 1.4133(17) . ?
C7 C8 1.3757(19) . ?
C7 H7 0.9500 . ?
C8 C9 1.397(2) . ?
C8 H8 0.9500 . ?
C9 C10 1.3795(19) . ?
C9 H9 0.9500 . ?
C10 N12 1.3545(16) . ?
C10 H10 0.9500 . ?
C11 N2 1.3543(16) . ?
C11 C12 1.3778(19) . ?
C11 H11 0.9500 . ?
C12 C13 1.393(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.3777(19) . ?
C13 H13 0.9500 . ?
C14 C15 1.4118(17) . ?
C14 H14 0.9500 . ?
C15 N6 1.3685(15) . ?
C15 N2 1.3736(16) . ?
C16 N6 1.3663(16) . ?
C16 N9 1.3712(16) . ?
C16 C17 1.4156(17) . ?
C17 C18 1.3772(19) . ?
C17 H17 0.9500 . ?
C18 C19 1.396(2) . ?
C18 H18 0.9500 . ?
C19 C20 1.3766(19) . ?
C19 H19 0.9500 . ?
C20 N9 1.3544(16) . ?
C20 H20 0.9500 . ?
C21 N3 1.3580(16) . ?
C21 C22 1.3769(19) . ?
C21 H21 0.9500 . ?
C22 C23 1.395(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.3769(18) . ?
C23 H23 0.9500 . ?
C24 C25 1.4124(17) . ?
C24 H24 0.9500 . ?
C25 N3 1.3675(15) . ?
C25 N7 1.3694(15) . ?
C26 N7 1.3676(15) . ?
C26 N10 1.3679(15) . ?
C26 C27 1.4156(17) . ?
C27 C28 1.3742(18) . ?
C27 H27 0.9500 . ?
C28 C29 1.3972(19) . ?
C28 H28 0.9500 . ?
C29 C30 1.3786(18) . ?
C29 H29 0.9500 . ?
C30 N10 1.3538(16) . ?
C30 H30 0.9500 . ?
C31 N4 1.3570(16) . ?
C31 C32 1.3775(18) . ?
C31 H31 0.9500 . ?
C32 C33 1.397(2) . ?
C32 H32 0.9500 . ?
C33 C34 1.3777(19) . ?
C33 H33 0.9500 . ?
C34 C35 1.4164(17) . ?
C34 H34 0.9500 . ?
C35 N8 1.3637(15) . ?
C35 N4 1.3654(16) . ?
C36 N11 1.3617(16) . ?
C36 N8 1.3699(16) . ?
C36 C37 1.4113(18) . ?
C37 C38 1.3776(19) . ?
C37 H37 0.9500 . ?
C38 C39 1.394(2) . ?
C38 H38 0.9500 . ?
C39 C40 1.3804(19) . ?
C39 H39 0.9500 . ?
C40 N11 1.3550(16) . ?
C40 H40 0.9500 . ?
Br1 Co1 2.6890(2) . ?
Br2 Co3 2.6205(2) . ?
Co1 N1 1.9790(11) . ?
Co1 N4 1.9852(11) . ?
Co1 N3 1.9912(11) . ?
Co1 N2 1.9967(10) . ?
Co1 Co2 2.3295(2) . ?
Co2 N7 1.9010(10) . ?
Co2 N5 1.9021(10) . ?
Co2 N6 1.9039(10) . ?
Co2 N8 1.9111(10) . ?
Co2 Co3 2.3162(2) . ?
Co3 N9 1.9670(10) . ?
Co3 N10 1.9789(10) . ?
Co3 N11 1.9823(11) . ?
Co3 N12 1.9986(10) . ?

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
C101 C100 H1S1 109.5 . . ?
C101 C100 H1S2 109.5 . . ?
H1S1 C100 H1S2 109.5 . . ?
C101 C100 H1S3 109.5 . . ?
H1S1 C100 H1S3 109.5 . . ?
H1S2 C100 H1S3 109.5 . . ?
O100 C101 C100 108.28(12) . . ?
O100 C101 H2S1 110.0 . . ?
C100 C101 H2S1 110.0 . . ?
O100 C101 H2S2 110.0 . . ?
C100 C101 H2S2 110.0 . . ?
H2S1 C101 H2S2 108.4 . . ?
O100 C102 C103 108.69(12) . . ?
O100 C102 H3S1 110.0 . . ?
C103 C102 H3S1 110.0 . . ?
O100 C102 H3S2 110.0 . . ?
C103 C102 H3S2 110.0 . . ?
H3S1 C102 H3S2 108.3 . . ?
C102 C103 H4S1 109.5 . . ?
C102 C103 H4S2 109.5 . . ?
H4S1 C103 H4S2 109.5 . . ?
C102 C103 H4S3 109.5 . . ?
H4S1 C103 H4S3 109.5 . . ?
H4S2 C103 H4S3 109.5 . . ?
C101 O100 C102 112.04(11) . . ?
N1 C1 C2 123.51(12) . . ?
N1 C1 H1 118.2 . . ?
C2 C1 H1 118.2 . . ?
C1 C2 C3 118.33(12) . . ?
C1 C2 H2 120.8 . . ?
C3 C2 H2 120.8 . . ?
C4 C3 C2 119.40(12) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C3 C4 C5 120.03(12) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
N5 C5 N1 115.62(10) . . ?
N5 C5 C4 124.15(11) . . ?
N1 C5 C4 120.07(11) . . ?
N5 C6 N12 114.85(10) . . ?
N5 C6 C7 124.86(11) . . ?
N12 C6 C7 120.07(11) . . ?
C8 C7 C6 120.20(12) . . ?
C8 C7 H7 119.9 . . ?
C6 C7 H7 119.9 . . ?
C7 C8 C9 119.23(12) . . ?
C7 C8 H8 120.4 . . ?
C9 C8 H8 120.4 . . ?
C10 C9 C8 118.34(12) . . ?
C10 C9 H9 120.8 . . ?
C8 C9 H9 120.8 . . ?
N12 C10 C9 123.45(13) . . ?
N12 C10 H10 118.3 . . ?
C9 C10 H10 118.3 . . ?
N2 C11 C12 123.80(13) . . ?
N2 C11 H11 118.1 . . ?
C12 C11 H11 118.1 . . ?
C11 C12 C13 117.98(12) . . ?
C11 C12 H12 121.0 . . ?
C13 C12 H12 121.0 . . ?
C14 C13 C12 119.55(12) . . ?
C14 C13 H13 120.2 . . ?
C12 C13 H13 120.2 . . ?
C13 C14 C15 120.26(12) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
N6 C15 N2 115.05(10) . . ?
N6 C15 C14 125.13(11) . . ?
N2 C15 C14 119.73(11) . . ?
N6 C16 N9 114.76(10) . . ?
N6 C16 C17 125.86(11) . . ?
N9 C16 C17 119.12(11) . . ?
C18 C17 C16 120.21(12) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
C17 C18 C19 119.90(12) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?
C20 C19 C18 117.70(12) . . ?
C20 C19 H19 121.2 . . ?
C18 C19 H19 121.2 . . ?
N9 C20 C19 123.61(12) . . ?
N9 C20 H20 118.2 . . ?
C19 C20 H20 118.2 . . ?
N3 C21 C22 123.65(12) . . ?
N3 C21 H21 118.2 . . ?
C22 C21 H21 118.2 . . ?
C21 C22 C23 118.04(12) . . ?
C21 C22 H22 121.0 . . ?
C23 C22 H22 121.0 . . ?
C24 C23 C22 119.62(12) . . ?
C24 C23 H23 120.2 . . ?
C22 C23 H23 120.2 . . ?
C23 C24 C25 120.05(12) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
N3 C25 N7 115.19(10) . . ?
N3 C25 C24 120.09(11) . . ?
N7 C25 C24 124.54(11) . . ?
N7 C26 N10 115.53(10) . . ?
N7 C26 C27 124.65(11) . . ?
N10 C26 C27 119.73(11) . . ?
C28 C27 C26 120.27(12) . . ?
C28 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
C27 C28 C29 119.44(12) . . ?
C27 C28 H28 120.3 . . ?
C29 C28 H28 120.3 . . ?
C30 C29 C28 118.09(12) . . ?
C30 C29 H29 121.0 . . ?
C28 C29 H29 121.0 . . ?
N10 C30 C29 123.55(12) . . ?
N10 C30 H30 118.2 . . ?
C29 C30 H30 118.2 . . ?
N4 C31 C32 123.72(12) . . ?
N4 C31 H31 118.1 . . ?
C32 C31 H31 118.1 . . ?
C31 C32 C33 118.39(12) . . ?
C31 C32 H32 120.8 . . ?
C33 C32 H32 120.8 . . ?
C34 C33 C32 118.94(12) . . ?
C34 C33 H33 120.5 . . ?
C32 C33 H33 120.5 . . ?
C33 C34 C35 120.42(12) . . ?
C33 C34 H34 119.8 . . ?
C35 C34 H34 119.8 . . ?
N8 C35 N4 116.01(10) . . ?
N8 C35 C34 123.91(11) . . ?
N4 C35 C34 120.01(11) . . ?
N11 C36 N8 115.73(11) . . ?
N11 C36 C37 120.21(11) . . ?
N8 C36 C37 123.76(11) . . ?
C38 C37 C36 120.45(13) . . ?
C38 C37 H37 119.8 . . ?
C36 C37 H37 119.8 . . ?
C37 C38 C39 118.96(12) . . ?
C37 C38 H38 120.5 . . ?
C39 C38 H38 120.5 . . ?
C40 C39 C38 118.31(12) . . ?
C40 C39 H39 120.8 . . ?
C38 C39 H39 120.8 . . ?
N11 C40 C39 123.69(13) . . ?
N11 C40 H40 118.2 . . ?
C39 C40 H40 118.2 . . ?
N1 Co1 N4 88.08(4) . . ?
N1 Co1 N3 171.09(4) . . ?
N4 Co1 N3 91.68(4) . . ?
N1 Co1 N2 90.13(4) . . ?
N4 Co1 N2 171.24(4) . . ?
N3 Co1 N2 88.76(4) . . ?
N1 Co1 Co2 86.04(3) . . ?
N4 Co1 Co2 87.55(3) . . ?
N3 Co1 Co2 85.06(3) . . ?
N2 Co1 Co2 83.78(3) . . ?
N1 Co1 Br1 94.95(3) . . ?
N4 Co1 Br1 94.32(3) . . ?
N3 Co1 Br1 93.95(3) . . ?
N2 Co1 Br1 94.38(3) . . ?
Co2 Co1 Br1 177.919(9) . . ?
N7 Co2 N5 178.65(5) . . ?
N7 Co2 N6 90.51(4) . . ?
N5 Co2 N6 90.84(4) . . ?
N7 Co2 N8 89.28(4) . . ?
N5 Co2 N8 89.37(4) . . ?
N6 Co2 N8 179.36(4) . . ?
N7 Co2 Co3 90.16(3) . . ?
N5 Co2 Co3 89.91(3) . . ?
N6 Co2 Co3 90.61(3) . . ?
N8 Co2 Co3 88.78(3) . . ?
N7 Co2 Co1 90.15(3) . . ?
N5 Co2 Co1 89.72(3) . . ?
N6 Co2 Co1 92.02(3) . . ?
N8 Co2 Co1 88.59(3) . . ?
Co3 Co2 Co1 177.343(10) . . ?
N9 Co3 N10 86.57(4) . . ?
N9 Co3 N11 170.89(4) . . ?
N10 Co3 N11 91.68(4) . . ?
N9 Co3 N12 89.63(4) . . ?
N10 Co3 N12 170.42(4) . . ?
N11 Co3 N12 90.69(4) . . ?
N9 Co3 Co2 84.32(3) . . ?
N10 Co3 Co2 86.26(3) . . ?
N11 Co3 Co2 86.64(3) . . ?
N12 Co3 Co2 84.61(3) . . ?
N9 Co3 Br2 94.69(3) . . ?
N10 Co3 Br2 97.04(3) . . ?
N11 Co3 Br2 94.40(3) . . ?
N12 Co3 Br2 92.03(3) . . ?
Co2 Co3 Br2 176.500(9) . . ?
C1 N1 C5 118.62(11) . . ?
C1 N1 Co1 120.70(9) . . ?
C5 N1 Co1 120.50(8) . . ?
C11 N2 C15 118.42(11) . . ?
C11 N2 Co1 119.28(9) . . ?
C15 N2 Co1 122.29(8) . . ?
C21 N3 C25 118.48(11) . . ?
C21 N3 Co1 120.45(9) . . ?
C25 N3 Co1 120.93(8) . . ?
C31 N4 C35 118.37(11) . . ?
C31 N4 Co1 122.41(9) . . ?
C35 N4 Co1 119.16(8) . . ?
C6 N5 C5 124.06(10) . . ?
C6 N5 Co2 118.11(8) . . ?
C5 N5 Co2 117.80(8) . . ?
C16 N6 C15 125.50(10) . . ?
C16 N6 Co2 116.89(8) . . ?
C15 N6 Co2 117.52(8) . . ?
C26 N7 C25 123.59(10) . . ?
C26 N7 Co2 119.16(8) . . ?
C25 N7 Co2 117.13(8) . . ?
C35 N8 C36 122.46(10) . . ?
C35 N8 Co2 120.08(8) . . ?
C36 N8 Co2 117.07(8) . . ?
C20 N9 C16 119.12(11) . . ?
C20 N9 Co3 119.11(8) . . ?
C16 N9 Co3 121.64(8) . . ?
C30 N10 C26 118.77(10) . . ?
C30 N10 Co3 120.72(8) . . ?
C26 N10 Co3 120.31(8) . . ?
C40 N11 C36 118.35(11) . . ?
C40 N11 Co3 121.94(9) . . ?
C36 N11 Co3 119.42(8) . . ?
C10 N12 C6 118.43(11) . . ?
C10 N12 Co3 121.45(9) . . ?
C6 N12 Co3 120.10(8) . . ?

_refine_diff_density_max         0.718
_refine_diff_density_min         -1.041
_refine_diff_density_rms         0.094


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: DMF, ether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_4-Et2O-240K
_database_code_depnum_ccdc_archive 'CCDC 1865591'
_audit_update_record             
;
2018-09-03 deposited with the CCDC.
2018-11-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C40 H32 Co3 I2 N12, C4 H10 O'
_chemical_formula_sum            'C44 H42 Co3 I2 N12 O'
_chemical_formula_weight         1185.48

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

_cell_length_a                   37.3975(17)
_cell_length_b                   12.7054(5)
_cell_length_c                   18.9980(8)
_cell_angle_alpha                90
_cell_angle_beta                 91.748(2)
_cell_angle_gamma                90
_cell_volume                     9022.7(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    240(2)
_cell_measurement_reflns_used    9903
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      25.34

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.745
_exptl_crystal_F_000             4680
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    2.508
_shelx_estimated_absorpt_T_min   0.770
_shelx_estimated_absorpt_T_max   0.929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6529
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   '(SADABS; Bruker, 2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      240(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            50126
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.995
_diffrn_reflns_theta_max         25.360
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8265
_reflns_number_gt                7394
_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       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_structure_solution    'SHELXS2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_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)+(0.0199P)²+16.6082P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8265
_refine_ls_number_parameters     561
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0212
_refine_ls_wR_factor_ref         0.0506
_refine_ls_wR_factor_gt          0.0482
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.004
_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
C1 C 0.05785(7) 0.7708(2) 0.15746(13) 0.0396(6) Uani 1 1 d . . . . .
H1 H 0.059102 0.835952 0.134282 0.047 Uiso 1 1 calc R U . . .
C2 C 0.03757(7) 0.6929(2) 0.12654(14) 0.0464(7) Uani 1 1 d . . . . .
H2 H 0.024956 0.704678 0.083711 0.056 Uiso 1 1 calc R U . . .
C3 C 0.03613(7) 0.5965(2) 0.16002(14) 0.0424(6) Uani 1 1 d . . . . .
H3 H 0.022883 0.540957 0.139471 0.051 Uiso 1 1 calc R U . . .
C4 C 0.05408(6) 0.58207(19) 0.22330(13) 0.0354(6) Uani 1 1 d . . . . .
H4 H 0.052825 0.517075 0.246730 0.042 Uiso 1 1 calc R U . . .
C5 C 0.07430(6) 0.66463(17) 0.25286(11) 0.0263(5) Uani 1 1 d . . . . .
C6 C 0.08980(6) 0.58803(17) 0.36638(11) 0.0259(5) Uani 1 1 d . . . . .
C7 C 0.05575(7) 0.5591(2) 0.38828(14) 0.0427(6) Uani 1 1 d . . . . .
H7 H 0.035337 0.577709 0.360994 0.051 Uiso 1 1 calc R U . . .
C8 C 0.05220(8) 0.5034(3) 0.44966(15) 0.0535(8) Uani 1 1 d . . . . .
H8 H 0.029395 0.483569 0.464377 0.064 Uiso 1 1 calc R U . . .
C9 C 0.08220(8) 0.4767(2) 0.48952(14) 0.0490(7) Uani 1 1 d . . . . .
H9 H 0.080164 0.439682 0.532061 0.059 Uiso 1 1 calc R U . . .
C10 C 0.11504(7) 0.50501(19) 0.46599(12) 0.0342(5) Uani 1 1 d . . . . .
H10 H 0.135423 0.487616 0.493743 0.041 Uiso 1 1 calc R U . . .
C11 C 0.15967(7) 0.91810(18) 0.13551(13) 0.0366(6) Uani 1 1 d . . . . .
H11 H 0.150523 0.986732 0.139118 0.044 Uiso 1 1 calc R U . . .
C12 C 0.18424(8) 0.8990(2) 0.08546(14) 0.0462(7) Uani 1 1 d . . . . .
H12 H 0.191639 0.953071 0.055453 0.055 Uiso 1 1 calc R U . . .
C13 C 0.19807(8) 0.7984(2) 0.07970(13) 0.0418(6) Uani 1 1 d . . . . .
H13 H 0.214802 0.782941 0.045259 0.050 Uiso 1 1 calc R U . . .
C14 C 0.18700(7) 0.72150(18) 0.12506(12) 0.0334(5) Uani 1 1 d . . . . .
H14 H 0.196239 0.652912 0.121944 0.040 Uiso 1 1 calc R U . . .
C15 C 0.16184(6) 0.74566(16) 0.17606(11) 0.0239(5) Uani 1 1 d . . . . .
C16 C 0.15198(6) 0.57066(16) 0.22107(11) 0.0228(4) Uani 1 1 d . . . . .
C17 C 0.14436(7) 0.51695(18) 0.15752(12) 0.0325(5) Uani 1 1 d . . . . .
H17 H 0.143346 0.554081 0.114711 0.039 Uiso 1 1 calc R U . . .
C18 C 0.13844(7) 0.41084(19) 0.15812(13) 0.0409(6) Uani 1 1 d . . . . .
H18 H 0.133413 0.374863 0.115732 0.049 Uiso 1 1 calc R U . . .
C19 C 0.13986(7) 0.35637(18) 0.22133(13) 0.0395(6) Uani 1 1 d . . . . .
H19 H 0.134969 0.283841 0.222788 0.047 Uiso 1 1 calc R U . . .
C20 C 0.14856(6) 0.41095(17) 0.28165(12) 0.0303(5) Uani 1 1 d . . . . .
H20 H 0.149643 0.373934 0.324504 0.036 Uiso 1 1 calc R U . . .
C21 C 0.14830(7) 1.06977(18) 0.33496(13) 0.0350(6) Uani 1 1 d . . . . .
H21 H 0.127220 1.105343 0.320944 0.042 Uiso 1 1 calc R U . . .
C22 C 0.17363(8) 1.12363(18) 0.37399(13) 0.0409(6) Uani 1 1 d . . . . .
H22 H 0.170010 1.194457 0.386175 0.049 Uiso 1 1 calc R U . . .
C23 C 0.20467(7) 1.07184(19) 0.39518(13) 0.0389(6) Uani 1 1 d . . . . .
H23 H 0.222550 1.107305 0.421705 0.047 Uiso 1 1 calc R U . . .
C24 C 0.20910(6) 0.96823(18) 0.37710(12) 0.0308(5) Uani 1 1 d . . . . .
H24 H 0.230049 0.932135 0.391227 0.037 Uiso 1 1 calc R U . . .
C25 C 0.18206(6) 0.91617(16) 0.33722(10) 0.0230(4) Uani 1 1 d . . . . .
C26 C 0.21298(5) 0.75469(16) 0.31191(10) 0.0211(4) Uani 1 1 d . . . . .
C27 C 0.24286(6) 0.79620(18) 0.27779(11) 0.0286(5) Uani 1 1 d . . . . .
H27 H 0.243992 0.868596 0.267898 0.034 Uiso 1 1 calc R U . . .
C28 C 0.27019(6) 0.73132(19) 0.25906(12) 0.0336(5) Uani 1 1 d . . . . .
H28 H 0.289916 0.758423 0.235491 0.040 Uiso 1 1 calc R U . . .
C29 C 0.26840(6) 0.62469(19) 0.27536(12) 0.0321(5) Uani 1 1 d . . . . .
H29 H 0.286972 0.578764 0.263439 0.039 Uiso 1 1 calc R U . . .
C30 C 0.23910(6) 0.58804(17) 0.30908(11) 0.0264(5) Uani 1 1 d . . . . .
H30 H 0.237974 0.515788 0.319428 0.032 Uiso 1 1 calc R U . . .
C31 C 0.04669(7) 0.92176(19) 0.34976(14) 0.0385(6) Uani 1 1 d . . . . .
H31 H 0.037702 0.951558 0.307523 0.046 Uiso 1 1 calc R U . . .
C32 C 0.02493(7) 0.9212(2) 0.40670(16) 0.0482(7) Uani 1 1 d . . . . .
H32 H 0.001980 0.951304 0.403837 0.058 Uiso 1 1 calc R U . . .
C33 C 0.03772(7) 0.8750(2) 0.46832(15) 0.0485(7) Uani 1 1 d . . . . .
H33 H 0.023430 0.873035 0.508149 0.058 Uiso 1 1 calc R U . . .
C34 C 0.07142(7) 0.8320(2) 0.47104(13) 0.0384(6) Uani 1 1 d . . . . .
H34 H 0.080193 0.800118 0.512737 0.046 Uiso 1 1 calc R U . . .
C35 C 0.09280(6) 0.83573(16) 0.41152(11) 0.0258(5) Uani 1 1 d . . . . .
C36 C 0.14896(6) 0.77011(16) 0.46160(10) 0.0224(4) Uani 1 1 d . . . . .
C37 C 0.15115(7) 0.83219(18) 0.52322(11) 0.0319(5) Uani 1 1 d . . . . .
H37 H 0.133566 0.883154 0.531586 0.038 Uiso 1 1 calc R U . . .
C38 C 0.17892(7) 0.81792(19) 0.57061(12) 0.0386(6) Uani 1 1 d . . . . .
H38 H 0.180191 0.857828 0.612275 0.046 Uiso 1 1 calc R U . . .
C39 C 0.20519(7) 0.74445(19) 0.55709(12) 0.0381(6) Uani 1 1 d . . . . .
H39 H 0.225097 0.736413 0.588035 0.046 Uiso 1 1 calc R U . . .
C40 C 0.20158(6) 0.68377(17) 0.49776(11) 0.0290(5) Uani 1 1 d . . . . .
H40 H 0.219489 0.634116 0.488641 0.035 Uiso 1 1 calc R U . . .
C41 C -0.02138(18) 0.3036(4) 0.3693(3) 0.135(2) Uani 1 1 d . . . . .
H41A H -0.035631 0.243327 0.382456 0.202 Uiso 1 1 calc R U . . .
H41B H -0.031968 0.336073 0.327426 0.202 Uiso 1 1 calc R U . . .
H41C H -0.020674 0.354226 0.407543 0.202 Uiso 1 1 calc R U . . .
C42 C 0.01492(19) 0.2693(4) 0.3550(3) 0.124(2) Uani 1 1 d . . . . .
H42A H 0.014044 0.210980 0.321217 0.149 Uiso 1 1 calc R U . . .
H42B H 0.028180 0.327360 0.334135 0.149 Uiso 1 1 calc R U . . .
C43 C 0.06864(15) 0.2010(4) 0.4095(3) 0.1179(19) Uani 1 1 d . . . . .
H43A H 0.083095 0.259505 0.392495 0.141 Uiso 1 1 calc R U . . .
H43B H 0.068711 0.144835 0.374153 0.141 Uiso 1 1 calc R U . . .
C44 C 0.08422(15) 0.1612(4) 0.4776(3) 0.1220(19) Uani 1 1 d . . . . .
H44A H 0.091174 0.220263 0.507293 0.183 Uiso 1 1 calc R U . . .
H44B H 0.105078 0.118392 0.468608 0.183 Uiso 1 1 calc R U . . .
H44C H 0.066568 0.119007 0.501086 0.183 Uiso 1 1 calc R U . . .
N1 N 0.07628(5) 0.75935(15) 0.21966(9) 0.0291(4) Uani 1 1 d . . . . .
N2 N 0.14767(5) 0.84395(14) 0.18038(9) 0.0266(4) Uani 1 1 d . . . . .
N3 N 0.15200(5) 0.96772(13) 0.31544(9) 0.0261(4) Uani 1 1 d . . . . .
N4 N 0.08029(5) 0.88203(14) 0.35078(10) 0.0282(4) Uani 1 1 d . . . . .
N5 N 0.09604(5) 0.65421(13) 0.31183(9) 0.0239(4) Uani 1 1 d . . . . .
N6 N 0.15217(5) 0.67756(13) 0.22813(8) 0.0211(4) Uani 1 1 d . . . . .
N7 N 0.18247(5) 0.81051(13) 0.32331(9) 0.0211(4) Uani 1 1 d . . . . .
N8 N 0.12544(5) 0.78688(13) 0.40632(9) 0.0222(4) Uani 1 1 d . . . . .
N9 N 0.11961(5) 0.55691(13) 0.40467(9) 0.0237(4) Uani 1 1 d . . . . .
N10 N 0.15572(5) 0.51582(13) 0.28273(9) 0.0222(4) Uani 1 1 d . . . . .
N11 N 0.21157(4) 0.65010(13) 0.32843(8) 0.0206(4) Uani 1 1 d . . . . .
N12 N 0.17347(5) 0.69194(13) 0.45170(8) 0.0213(4) Uani 1 1 d . . . . .
O1 O 0.03312(9) 0.2354(2) 0.41945(16) 0.0962(9) Uani 1 1 d . . . . .
Co1 Co 0.11055(2) 0.88606(2) 0.25791(2) 0.02947(8) Uani 1 1 d . . . . .
Co2 Co 0.13893(2) 0.73348(2) 0.31703(2) 0.01902(7) Uani 1 1 d . . . . .
Co3 Co 0.16752(2) 0.59406(2) 0.37089(2) 0.01931(7) Uani 1 1 d . . . . .
I1 I 0.07879(2) 1.05395(2) 0.18993(2) 0.04712(6) Uani 1 1 d . . . . .
I2 I 0.20367(2) 0.42041(2) 0.43868(2) 0.03689(5) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.357(3) . ?
C1 C2 1.368(4) . ?
C1 H1 0.9400 . ?
C2 C3 1.382(4) . ?
C2 H2 0.9400 . ?
C3 C4 1.371(3) . ?
C3 H3 0.9400 . ?
C4 C5 1.401(3) . ?
C4 H4 0.9400 . ?
C5 N1 1.362(3) . ?
C5 N5 1.370(3) . ?
C6 N5 1.360(3) . ?
C6 N9 1.371(3) . ?
C6 C7 1.401(3) . ?
C7 C8 1.374(4) . ?
C7 H7 0.9400 . ?
C8 C9 1.377(4) . ?
C8 H8 0.9400 . ?
C9 C10 1.368(4) . ?
C9 H9 0.9400 . ?
C10 N9 1.354(3) . ?
C10 H10 0.9400 . ?
C11 N2 1.356(3) . ?
C11 C12 1.364(4) . ?
C11 H11 0.9400 . ?
C12 C13 1.384(4) . ?
C12 H12 0.9400 . ?
C13 C14 1.375(3) . ?
C13 H13 0.9400 . ?
C14 C15 1.405(3) . ?
C14 H14 0.9400 . ?
C15 N2 1.360(3) . ?
C15 N6 1.371(3) . ?
C16 N6 1.365(3) . ?
C16 N10 1.367(3) . ?
C16 C17 1.408(3) . ?
C17 C18 1.366(3) . ?
C17 H17 0.9400 . ?
C18 C19 1.386(4) . ?
C18 H18 0.9400 . ?
C19 C20 1.370(3) . ?
C19 H19 0.9400 . ?
C20 N10 1.359(3) . ?
C20 H20 0.9400 . ?
C21 N3 1.357(3) . ?
C21 C22 1.369(4) . ?
C21 H21 0.9400 . ?
C22 C23 1.383(4) . ?
C22 H22 0.9400 . ?
C23 C24 1.372(3) . ?
C23 H23 0.9400 . ?
C24 C25 1.409(3) . ?
C24 H24 0.9400 . ?
C25 N3 1.355(3) . ?
C25 N7 1.368(3) . ?
C26 N7 1.366(3) . ?
C26 N11 1.367(3) . ?
C26 C27 1.411(3) . ?
C27 C28 1.369(3) . ?
C27 H27 0.9400 . ?
C28 C29 1.392(3) . ?
C28 H28 0.9400 . ?
C29 C30 1.368(3) . ?
C29 H29 0.9400 . ?
C30 N11 1.356(3) . ?
C30 H30 0.9400 . ?
C31 N4 1.354(3) . ?
C31 C32 1.373(4) . ?
C31 H31 0.9400 . ?
C32 C33 1.382(4) . ?
C32 H32 0.9400 . ?
C33 C34 1.373(4) . ?
C33 H33 0.9400 . ?
C34 C35 1.406(3) . ?
C34 H34 0.9400 . ?
C35 N4 1.365(3) . ?
C35 N8 1.376(3) . ?
C36 N8 1.366(3) . ?
C36 N12 1.368(3) . ?
C36 C37 1.412(3) . ?
C37 C38 1.365(3) . ?
C37 H37 0.9400 . ?
C38 C39 1.385(3) . ?
C38 H38 0.9400 . ?
C39 C40 1.369(3) . ?
C39 H39 0.9400 . ?
C40 N12 1.351(3) . ?
C40 H40 0.9400 . ?
C41 C42 1.459(7) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C41 H41C 0.9700 . ?
C42 O1 1.448(6) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C43 O1 1.416(6) . ?
C43 C44 1.490(7) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C44 H44C 0.9700 . ?
N1 Co1 2.1692(19) . ?
N2 Co1 2.1232(19) . ?
N3 Co1 2.1380(18) . ?
N4 Co1 2.1254(19) . ?
N5 Co2 1.8941(17) . ?
N6 Co2 1.9116(17) . ?
N7 Co2 1.9005(17) . ?
N8 Co2 1.9090(17) . ?
N9 Co3 1.9787(18) . ?
N10 Co3 1.9856(17) . ?
N11 Co3 1.9881(17) . ?
N12 Co3 1.9830(16) . ?
Co1 Co2 2.4645(4) . ?
Co1 I1 2.7449(3) . ?
Co2 Co3 2.2937(4) . ?
Co3 I2 2.8719(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 123.8(2) . . ?
N1 C1 H1 118.1 . . ?
C2 C1 H1 118.1 . . ?
C1 C2 C3 118.2(2) . . ?
C1 C2 H2 120.9 . . ?
C3 C2 H2 120.9 . . ?
C4 C3 C2 119.8(2) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C3 C4 C5 119.7(2) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
N1 C5 N5 115.14(19) . . ?
N1 C5 C4 120.8(2) . . ?
N5 C5 C4 123.7(2) . . ?
N5 C6 N9 115.28(18) . . ?
N5 C6 C7 124.6(2) . . ?
N9 C6 C7 119.9(2) . . ?
C8 C7 C6 120.0(2) . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C7 C8 C9 119.7(2) . . ?
C7 C8 H8 120.1 . . ?
C9 C8 H8 120.1 . . ?
C10 C9 C8 118.7(2) . . ?
C10 C9 H9 120.7 . . ?
C8 C9 H9 120.7 . . ?
N9 C10 C9 123.2(2) . . ?
N9 C10 H10 118.4 . . ?
C9 C10 H10 118.4 . . ?
N2 C11 C12 123.9(2) . . ?
N2 C11 H11 118.1 . . ?
C12 C11 H11 118.1 . . ?
C11 C12 C13 118.7(2) . . ?
C11 C12 H12 120.6 . . ?
C13 C12 H12 120.6 . . ?
C14 C13 C12 119.1(2) . . ?
C14 C13 H13 120.5 . . ?
C12 C13 H13 120.5 . . ?
C13 C14 C15 119.8(2) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
N2 C15 N6 115.11(19) . . ?
N2 C15 C14 120.8(2) . . ?
N6 C15 C14 123.81(19) . . ?
N6 C16 N10 115.03(17) . . ?
N6 C16 C17 124.53(19) . . ?
N10 C16 C17 120.03(19) . . ?
C18 C17 C16 120.0(2) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C17 C18 C19 119.9(2) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 H18 120.1 . . ?
C20 C19 C18 118.3(2) . . ?
C20 C19 H19 120.9 . . ?
C18 C19 H19 120.9 . . ?
N10 C20 C19 123.4(2) . . ?
N10 C20 H20 118.3 . . ?
C19 C20 H20 118.3 . . ?
N3 C21 C22 123.4(2) . . ?
N3 C21 H21 118.3 . . ?
C22 C21 H21 118.3 . . ?
C21 C22 C23 118.7(2) . . ?
C21 C22 H22 120.6 . . ?
C23 C22 H22 120.6 . . ?
C24 C23 C22 119.4(2) . . ?
C24 C23 H23 120.3 . . ?
C22 C23 H23 120.3 . . ?
C23 C24 C25 119.7(2) . . ?
C23 C24 H24 120.2 . . ?
C25 C24 H24 120.2 . . ?
N3 C25 N7 115.42(18) . . ?
N3 C25 C24 120.81(19) . . ?
N7 C25 C24 123.5(2) . . ?
N7 C26 N11 115.46(18) . . ?
N7 C26 C27 123.75(19) . . ?
N11 C26 C27 120.37(19) . . ?
C28 C27 C26 120.2(2) . . ?
C28 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
C27 C28 C29 119.2(2) . . ?
C27 C28 H28 120.4 . . ?
C29 C28 H28 120.4 . . ?
C30 C29 C28 118.7(2) . . ?
C30 C29 H29 120.7 . . ?
C28 C29 H29 120.7 . . ?
N11 C30 C29 123.7(2) . . ?
N11 C30 H30 118.2 . . ?
C29 C30 H30 118.2 . . ?
N4 C31 C32 124.0(2) . . ?
N4 C31 H31 118.0 . . ?
C32 C31 H31 118.0 . . ?
C31 C32 C33 118.1(2) . . ?
C31 C32 H32 120.9 . . ?
C33 C32 H32 120.9 . . ?
C34 C33 C32 119.6(3) . . ?
C34 C33 H33 120.2 . . ?
C32 C33 H33 120.2 . . ?
C33 C34 C35 120.0(2) . . ?
C33 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
N4 C35 N8 114.55(19) . . ?
N4 C35 C34 120.4(2) . . ?
N8 C35 C34 124.8(2) . . ?
N8 C36 N12 115.20(17) . . ?
N8 C36 C37 124.76(19) . . ?
N12 C36 C37 119.83(18) . . ?
C38 C37 C36 119.8(2) . . ?
C38 C37 H37 120.1 . . ?
C36 C37 H37 120.1 . . ?
C37 C38 C39 119.8(2) . . ?
C37 C38 H38 120.1 . . ?
C39 C38 H38 120.1 . . ?
C40 C39 C38 118.7(2) . . ?
C40 C39 H39 120.7 . . ?
C38 C39 H39 120.7 . . ?
N12 C40 C39 123.0(2) . . ?
N12 C40 H40 118.5 . . ?
C39 C40 H40 118.5 . . ?
C42 C41 H41A 109.5 . . ?
C42 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C42 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O1 C42 C41 110.3(5) . . ?
O1 C42 H42A 109.6 . . ?
C41 C42 H42A 109.6 . . ?
O1 C42 H42B 109.6 . . ?
C41 C42 H42B 109.6 . . ?
H42A C42 H42B 108.1 . . ?
O1 C43 C44 109.4(4) . . ?
O1 C43 H43A 109.8 . . ?
C44 C43 H43A 109.8 . . ?
O1 C43 H43B 109.8 . . ?
C44 C43 H43B 109.8 . . ?
H43A C43 H43B 108.2 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C1 N1 C5 117.7(2) . . ?
C1 N1 Co1 119.44(16) . . ?
C5 N1 Co1 122.72(14) . . ?
C11 N2 C15 117.6(2) . . ?
C11 N2 Co1 119.80(15) . . ?
C15 N2 Co1 122.51(14) . . ?
C25 N3 C21 117.98(19) . . ?
C25 N3 Co1 120.23(13) . . ?
C21 N3 Co1 121.66(16) . . ?
C31 N4 C35 117.8(2) . . ?
C31 N4 Co1 119.77(16) . . ?
C35 N4 Co1 122.33(14) . . ?
C6 N5 C5 124.85(18) . . ?
C6 N5 Co2 116.98(14) . . ?
C5 N5 Co2 118.13(14) . . ?
C16 N6 C15 123.91(17) . . ?
C16 N6 Co2 117.13(14) . . ?
C15 N6 Co2 118.95(13) . . ?
C26 N7 C25 123.65(18) . . ?
C26 N7 Co2 116.16(13) . . ?
C25 N7 Co2 120.18(14) . . ?
C36 N8 C35 124.55(18) . . ?
C36 N8 Co2 116.51(14) . . ?
C35 N8 Co2 118.90(13) . . ?
C10 N9 C6 118.37(19) . . ?
C10 N9 Co3 122.32(15) . . ?
C6 N9 Co3 119.27(14) . . ?
C20 N10 C16 118.16(18) . . ?
C20 N10 Co3 122.84(15) . . ?
C16 N10 Co3 118.82(13) . . ?
C30 N11 C26 117.91(18) . . ?
C30 N11 Co3 123.15(14) . . ?
C26 N11 Co3 118.66(14) . . ?
C40 N12 C36 118.55(17) . . ?
C40 N12 Co3 121.32(14) . . ?
C36 N12 Co3 120.13(13) . . ?
C43 O1 C42 113.4(4) . . ?
N2 Co1 N4 161.04(7) . . ?
N2 Co1 N3 89.86(7) . . ?
N4 Co1 N3 89.05(7) . . ?
N2 Co1 N1 88.43(7) . . ?
N4 Co1 N1 86.34(7) . . ?
N3 Co1 N1 160.59(7) . . ?
N2 Co1 Co2 80.58(5) . . ?
N4 Co1 Co2 80.53(5) . . ?
N3 Co1 Co2 81.56(5) . . ?
N1 Co1 Co2 79.09(5) . . ?
N2 Co1 I1 98.75(5) . . ?
N4 Co1 I1 100.12(5) . . ?
N3 Co1 I1 99.21(5) . . ?
N1 Co1 I1 100.16(5) . . ?
Co2 Co1 I1 178.989(15) . . ?
N5 Co2 N7 178.74(7) . . ?
N5 Co2 N8 89.37(7) . . ?
N7 Co2 N8 90.59(7) . . ?
N5 Co2 N6 89.89(7) . . ?
N7 Co2 N6 90.13(7) . . ?
N8 Co2 N6 178.98(8) . . ?
N5 Co2 Co3 89.72(5) . . ?
N7 Co2 Co3 89.02(5) . . ?
N8 Co2 Co3 90.60(5) . . ?
N6 Co2 Co3 88.70(5) . . ?
N5 Co2 Co1 92.42(5) . . ?
N7 Co2 Co1 88.84(5) . . ?
N8 Co2 Co1 90.20(5) . . ?
N6 Co2 Co1 90.53(5) . . ?
Co3 Co2 Co1 177.724(17) . . ?
N9 Co3 N12 88.84(7) . . ?
N9 Co3 N10 88.51(7) . . ?
N12 Co3 N10 169.66(7) . . ?
N9 Co3 N11 170.67(7) . . ?
N12 Co3 N11 90.85(7) . . ?
N10 Co3 N11 90.15(7) . . ?
N9 Co3 Co2 85.09(5) . . ?
N12 Co3 Co2 84.30(5) . . ?
N10 Co3 Co2 85.52(5) . . ?
N11 Co3 Co2 85.59(5) . . ?
N9 Co3 I2 95.15(5) . . ?
N12 Co3 I2 95.42(5) . . ?
N10 Co3 I2 94.77(5) . . ?
N11 Co3 I2 94.16(5) . . ?
Co2 Co3 I2 179.626(15) . . ?

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
N1 C1 C2 C3 -1.0(4) . . . . ?
C1 C2 C3 C4 1.5(4) . . . . ?
C2 C3 C4 C5 -1.2(4) . . . . ?
C3 C4 C5 N1 0.2(4) . . . . ?
C3 C4 C5 N5 -172.9(2) . . . . ?
N5 C6 C7 C8 -171.1(2) . . . . ?
N9 C6 C7 C8 2.8(4) . . . . ?
C6 C7 C8 C9 0.3(5) . . . . ?
C7 C8 C9 C10 -1.2(5) . . . . ?
C8 C9 C10 N9 -1.0(4) . . . . ?
N2 C11 C12 C13 -0.3(4) . . . . ?
C11 C12 C13 C14 -0.8(4) . . . . ?
C12 C13 C14 C15 0.3(4) . . . . ?
C13 C14 C15 N2 1.3(3) . . . . ?
C13 C14 C15 N6 -172.7(2) . . . . ?
N6 C16 C17 C18 -168.1(2) . . . . ?
N10 C16 C17 C18 4.2(3) . . . . ?
C16 C17 C18 C19 0.2(4) . . . . ?
C17 C18 C19 C20 -2.4(4) . . . . ?
C18 C19 C20 N10 0.3(4) . . . . ?
N3 C21 C22 C23 -0.3(4) . . . . ?
C21 C22 C23 C24 -0.5(4) . . . . ?
C22 C23 C24 C25 0.1(4) . . . . ?
C23 C24 C25 N3 1.2(3) . . . . ?
C23 C24 C25 N7 -172.7(2) . . . . ?
N7 C26 C27 C28 -170.3(2) . . . . ?
N11 C26 C27 C28 2.0(3) . . . . ?
C26 C27 C28 C29 -1.3(3) . . . . ?
C27 C28 C29 C30 0.6(3) . . . . ?
C28 C29 C30 N11 -0.7(3) . . . . ?
N4 C31 C32 C33 -1.6(4) . . . . ?
C31 C32 C33 C34 0.3(4) . . . . ?
C32 C33 C34 C35 0.4(4) . . . . ?
C33 C34 C35 N4 0.1(4) . . . . ?
C33 C34 C35 N8 -173.7(2) . . . . ?
N8 C36 C37 C38 -170.6(2) . . . . ?
N12 C36 C37 C38 3.8(3) . . . . ?
C36 C37 C38 C39 1.6(4) . . . . ?
C37 C38 C39 C40 -3.4(4) . . . . ?
C38 C39 C40 N12 -0.2(4) . . . . ?
C2 C1 N1 C5 0.0(4) . . . . ?
C2 C1 N1 Co1 175.3(2) . . . . ?
N5 C5 N1 C1 174.1(2) . . . . ?
C4 C5 N1 C1 0.4(3) . . . . ?
N5 C5 N1 Co1 -1.0(3) . . . . ?
C4 C5 N1 Co1 -174.74(17) . . . . ?
C12 C11 N2 C15 1.8(4) . . . . ?
C12 C11 N2 Co1 178.1(2) . . . . ?
N6 C15 N2 C11 172.16(19) . . . . ?
C14 C15 N2 C11 -2.3(3) . . . . ?
N6 C15 N2 Co1 -4.0(2) . . . . ?
C14 C15 N2 Co1 -178.45(16) . . . . ?
N7 C25 N3 C21 172.45(19) . . . . ?
C24 C25 N3 C21 -1.9(3) . . . . ?
N7 C25 N3 Co1 -3.6(2) . . . . ?
C24 C25 N3 Co1 -177.98(15) . . . . ?
C22 C21 N3 C25 1.5(3) . . . . ?
C22 C21 N3 Co1 177.52(18) . . . . ?
C32 C31 N4 C35 2.1(4) . . . . ?
C32 C31 N4 Co1 178.9(2) . . . . ?
N8 C35 N4 C31 173.07(19) . . . . ?
C34 C35 N4 C31 -1.3(3) . . . . ?
N8 C35 N4 Co1 -3.7(2) . . . . ?
C34 C35 N4 Co1 -178.01(17) . . . . ?
N9 C6 N5 C5 154.6(2) . . . . ?
C7 C6 N5 C5 -31.2(3) . . . . ?
N9 C6 N5 Co2 -23.0(2) . . . . ?
C7 C6 N5 Co2 151.2(2) . . . . ?
N1 C5 N5 C6 154.3(2) . . . . ?
C4 C5 N5 C6 -32.2(3) . . . . ?
N1 C5 N5 Co2 -28.1(2) . . . . ?
C4 C5 N5 Co2 145.35(19) . . . . ?
N10 C16 N6 C15 155.08(19) . . . . ?
C17 C16 N6 C15 -32.3(3) . . . . ?
N10 C16 N6 Co2 -23.7(2) . . . . ?
C17 C16 N6 Co2 148.92(19) . . . . ?
N2 C15 N6 C16 155.18(19) . . . . ?
C14 C15 N6 C16 -30.5(3) . . . . ?
N2 C15 N6 Co2 -26.1(2) . . . . ?
C14 C15 N6 Co2 148.25(18) . . . . ?
N11 C26 N7 C25 153.14(18) . . . . ?
C27 C26 N7 C25 -34.2(3) . . . . ?
N11 C26 N7 Co2 -28.1(2) . . . . ?
C27 C26 N7 Co2 144.52(16) . . . . ?
N3 C25 N7 C26 150.41(19) . . . . ?
C24 C25 N7 C26 -35.4(3) . . . . ?
N3 C25 N7 Co2 -28.3(2) . . . . ?
C24 C25 N7 Co2 145.92(18) . . . . ?
N12 C36 N8 C35 158.93(19) . . . . ?
C37 C36 N8 C35 -26.5(3) . . . . ?
N12 C36 N8 Co2 -18.8(2) . . . . ?
C37 C36 N8 Co2 155.80(18) . . . . ?
N4 C35 N8 C36 154.74(19) . . . . ?
C34 C35 N8 C36 -31.2(3) . . . . ?
N4 C35 N8 Co2 -27.6(2) . . . . ?
C34 C35 N8 Co2 146.49(19) . . . . ?
C9 C10 N9 C6 4.0(3) . . . . ?
C9 C10 N9 Co3 -178.6(2) . . . . ?
N5 C6 N9 C10 169.67(19) . . . . ?
C7 C6 N9 C10 -4.8(3) . . . . ?
N5 C6 N9 Co3 -7.8(2) . . . . ?
C7 C6 N9 Co3 177.70(17) . . . . ?
C19 C20 N10 C16 4.0(3) . . . . ?
C19 C20 N10 Co3 178.98(19) . . . . ?
N6 C16 N10 C20 166.86(19) . . . . ?
C17 C16 N10 C20 -6.1(3) . . . . ?
N6 C16 N10 Co3 -8.4(2) . . . . ?
C17 C16 N10 Co3 178.66(16) . . . . ?
C29 C30 N11 C26 1.4(3) . . . . ?
C29 C30 N11 Co3 175.25(16) . . . . ?
N7 C26 N11 C30 170.93(17) . . . . ?
C27 C26 N11 C30 -2.0(3) . . . . ?
N7 C26 N11 Co3 -3.2(2) . . . . ?
C27 C26 N11 Co3 -176.12(14) . . . . ?
C39 C40 N12 C36 5.5(3) . . . . ?
C39 C40 N12 Co3 -174.82(18) . . . . ?
N8 C36 N12 C40 167.70(19) . . . . ?
C37 C36 N12 C40 -7.2(3) . . . . ?
N8 C36 N12 Co3 -12.0(2) . . . . ?
C37 C36 N12 Co3 173.12(16) . . . . ?
C44 C43 O1 C42 -176.2(4) . . . . ?
C41 C42 O1 C43 -180.0(4) . . . . ?
C6 N5 Co2 N8 -55.22(16) . . . . ?
C5 N5 Co2 N8 127.03(16) . . . . ?
C6 N5 Co2 N6 124.08(16) . . . . ?
C5 N5 Co2 N6 -53.67(16) . . . . ?
C6 N5 Co2 Co3 35.38(15) . . . . ?
C5 N5 Co2 Co3 -142.37(15) . . . . ?
C6 N5 Co2 Co1 -145.39(15) . . . . ?
C5 N5 Co2 Co1 36.86(15) . . . . ?

_refine_diff_density_max         0.767
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.056


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile, ether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_4-CLCH22-298K
_database_code_depnum_ccdc_archive 'CCDC 1865588'
_audit_update_record             
;
2018-09-03 deposited with the CCDC.
2018-11-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C40 H32 Co3 I2 N12, C2 H4 Cl2'
_chemical_formula_sum            'C42 H36 Cl2 Co3 I2 N12'
_chemical_formula_weight         1210.32

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'
Cl Cl 0.1484 0.1585 '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'
I I -0.4742 1.8119 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/n'
_space_group_name_Hall           '-P 2yac'

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

_cell_length_a                   13.127(3)
_cell_length_b                   11.755(2)
_cell_length_c                   14.317(3)
_cell_angle_alpha                90
_cell_angle_beta                 94.369(8)
_cell_angle_gamma                90
_cell_volume                     2202.9(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9968
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      26.23

_exptl_crystal_description       needle
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.825
_exptl_crystal_F_000             1186
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.049
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.013
_exptl_absorpt_coefficient_mu    2.686
_shelx_estimated_absorpt_T_min   0.880
_shelx_estimated_absorpt_T_max   0.966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6457
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SADABS (Bruker, 2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            46915
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.029
_diffrn_reflns_theta_max         26.433
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4531
_reflns_number_gt                3507
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2014)'
_computing_publication_material  'SHELXL-2016/4 (Sheldrick, 2016)'
_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)+(0.0297P)²+2.6506P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_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_number_reflns         4531
_refine_ls_number_parameters     331
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0267
_refine_ls_wR_factor_ref         0.0694
_refine_ls_wR_factor_gt          0.0631
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.029
_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
C1 C 0.9296(2) 0.0712(3) 0.1186(2) 0.0393(8) Uani 1 1 d . . . . .
H1 H 0.997862 0.092862 0.120592 0.047 Uiso 1 1 calc R U . . .
C2 C 0.9060(3) -0.0389(3) 0.0956(3) 0.0511(9) Uani 1 1 d . . . . .
H2 H 0.956291 -0.089522 0.079687 0.061 Uiso 1 1 calc R U . . .
C3 C 0.8052(3) -0.0734(3) 0.0966(3) 0.0536(10) Uani 1 1 d . . . . .
H3 H 0.786713 -0.148128 0.082440 0.064 Uiso 1 1 calc R U . . .
C4 C 0.7334(3) 0.0040(3) 0.1188(3) 0.0447(9) Uani 1 1 d . . . . .
H4 H 0.665587 -0.018316 0.120794 0.054 Uiso 1 1 calc R U . . .
C5 C 0.7613(2) 0.1169(2) 0.13859(19) 0.0266(6) Uani 1 1 d . . . . .
C6 C 0.4367(2) 0.2786(3) 0.1728(2) 0.0382(8) Uani 1 1 d . . . . .
H6 H 0.397994 0.320700 0.212155 0.046 Uiso 1 1 calc R U . . .
C7 C 0.3908(3) 0.2422(3) 0.0896(3) 0.0482(9) Uani 1 1 d . . . . .
H7 H 0.322328 0.257923 0.073082 0.058 Uiso 1 1 calc R U . . .
C8 C 0.4489(3) 0.1810(3) 0.0306(3) 0.0498(9) Uani 1 1 d . . . . .
H8 H 0.419204 0.153612 -0.026062 0.060 Uiso 1 1 calc R U . . .
C9 C 0.5496(3) 0.1609(3) 0.0553(2) 0.0415(8) Uani 1 1 d . . . . .
H9 H 0.589087 0.120633 0.015298 0.050 Uiso 1 1 calc R U . . .
C10 C 0.5932(2) 0.2012(2) 0.1413(2) 0.0272(6) Uani 1 1 d . . . . .
C11 C 0.9618(2) 0.5577(3) 0.1754(2) 0.0369(7) Uani 1 1 d . . . . .
H11 H 0.991274 0.537459 0.120721 0.044 Uiso 1 1 calc R U . . .
C12 C 0.9709(3) 0.6675(3) 0.2047(3) 0.0498(9) Uani 1 1 d . . . . .
H12 H 1.006273 0.720354 0.171235 0.060 Uiso 1 1 calc R U . . .
C13 C 0.9265(3) 0.6989(3) 0.2847(3) 0.0538(10) Uani 1 1 d . . . . .
H13 H 0.932832 0.773137 0.306757 0.065 Uiso 1 1 calc R U . . .
C14 C 0.8731(3) 0.6203(3) 0.3318(2) 0.0416(8) Uani 1 1 d . . . . .
H14 H 0.842231 0.641140 0.385578 0.050 Uiso 1 1 calc R U . . .
C15 C 0.8652(2) 0.5082(2) 0.29874(19) 0.0260(6) Uani 1 1 d . . . . .
C16 C 0.8298(2) 0.3442(3) -0.0273(2) 0.0367(7) Uani 1 1 d . . . . .
H16 H 0.889116 0.303784 -0.036547 0.044 Uiso 1 1 calc R U . . .
C17 C 0.7692(3) 0.3770(3) -0.1040(2) 0.0475(9) Uani 1 1 d . . . . .
H17 H 0.787188 0.359927 -0.164040 0.057 Uiso 1 1 calc R U . . .
C18 C 0.6807(3) 0.4360(3) -0.0908(2) 0.0459(8) Uani 1 1 d . . . . .
H18 H 0.638482 0.460237 -0.141986 0.055 Uiso 1 1 calc R U . . .
C19 C 0.6555(2) 0.4587(3) -0.0015(2) 0.0381(7) Uani 1 1 d . . . . .
H19 H 0.595841 0.498295 0.008138 0.046 Uiso 1 1 calc R U . . .
C20 C 0.7194(2) 0.4221(2) 0.07502(18) 0.0245(6) Uani 1 1 d . . . . .
Co1 Co 0.90193(3) 0.31363(3) 0.17238(3) 0.02725(10) Uani 1 1 d . . . . .
Co2 Co 0.750000 0.31274(4) 0.250000 0.01994(11) Uani 1 2 d S T P . .
I1 I 1.08690(2) 0.31482(2) 0.08098(2) 0.04265(8) Uani 1 1 d . . . . .
N1 N 0.86054(17) 0.1500(2) 0.13836(16) 0.0267(5) Uani 1 1 d . . . . .
N2 N 0.53544(17) 0.2572(2) 0.20131(16) 0.0270(5) Uani 1 1 d . . . . .
N3 N 0.91275(17) 0.4766(2) 0.22098(16) 0.0264(5) Uani 1 1 d . . . . .
N4 N 0.80855(17) 0.3672(2) 0.06159(15) 0.0262(5) Uani 1 1 d . . . . .
N5 N 0.69552(17) 0.19782(19) 0.16781(16) 0.0247(5) Uani 1 1 d . . . . .
N6 N 0.69548(16) 0.42663(19) 0.16644(15) 0.0236(5) Uani 1 1 d . . . . .
Cl1 Cl 0.1471(14) -0.0899(14) 0.3178(9) 0.189(8) Uani 0.356(4) 1 d D U P A -1
C21 C 0.2436(18) 0.0065(17) 0.3263(16) 0.125(6) Uani 0.356(4) 1 d D U P A -1
H21A H 0.216443 0.077098 0.349230 0.150 Uiso 0.356(4) 1 calc R U P A -1
H21B H 0.294655 -0.020394 0.373733 0.150 Uiso 0.356(4) 1 calc R U P A -1
C22 C 0.2926(14) 0.0312(12) 0.2467(14) 0.103(4) Uani 0.356(4) 1 d D U P A -1
H22A H 0.333692 0.099145 0.257547 0.124 Uiso 0.356(4) 1 calc R U P A -1
H22B H 0.241905 0.046763 0.195375 0.124 Uiso 0.356(4) 1 calc R U P A -1
Cl2 Cl 0.3723(9) -0.0823(17) 0.2144(10) 0.192(7) Uani 0.356(4) 1 d D U P A -1
Cl3 Cl 0.236(3) -0.080(2) 0.3614(12) 0.165(10) Uani 0.144(4) 1 d D U P A -2
C23 C 0.299(4) 0.017(3) 0.2886(19) 0.112(6) Uani 0.144(4) 1 d D U P A -2
H23A H 0.258828 0.085521 0.280702 0.134 Uiso 0.144(4) 1 calc R U P A -2
H23B H 0.365054 0.037272 0.319577 0.134 Uiso 0.144(4) 1 calc R U P A -2
C24 C 0.315(2) -0.030(4) 0.1972(18) 0.101(6) Uani 0.144(4) 1 d D U P A -2
H24A H 0.357724 -0.097341 0.205119 0.121 Uiso 0.144(4) 1 calc R U P A -2
H24B H 0.350802 0.025065 0.161716 0.121 Uiso 0.144(4) 1 calc R U P A -2
Cl4 Cl 0.1984(16) -0.068(2) 0.1324(14) 0.166(10) Uani 0.144(4) 1 d D 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
C1 N1 1.342(4) . ?
C1 C2 1.365(5) . ?
C2 C3 1.385(5) . ?
C3 C4 1.365(5) . ?
C4 C5 1.400(4) . ?
C5 N1 1.360(3) . ?
C5 N5 1.372(4) . ?
C6 N2 1.352(4) . ?
C6 C7 1.362(5) . ?
C7 C8 1.383(5) . ?
C8 C9 1.363(5) . ?
C9 C10 1.400(4) . ?
C10 N2 1.359(4) . ?
C10 N5 1.368(3) . ?
C11 N3 1.347(4) . ?
C11 C12 1.359(5) . ?
C12 C13 1.374(5) . ?
C13 C14 1.368(5) . ?
C14 C15 1.401(4) . ?
C15 N6 1.365(3) 2_655 ?
C15 N3 1.369(3) . ?
C16 N4 1.350(4) . ?
C16 C17 1.362(5) . ?
C17 C18 1.379(5) . ?
C18 C19 1.371(4) . ?
C19 C20 1.396(4) . ?
C20 N4 1.362(3) . ?
C20 N6 1.370(3) . ?
Co1 N4 2.029(2) . ?
Co1 N2 2.039(2) 2_655 ?
Co1 N3 2.040(2) . ?
Co1 N1 2.047(2) . ?
Co1 Co2 2.3558(5) . ?
Co1 I1 2.8447(6) . ?
Co2 N5 1.895(2) . ?
Co2 N5 1.895(2) 2_655 ?
Co2 N6 1.899(2) 2_655 ?
Co2 N6 1.899(2) . ?
Cl1 C21 1.696(16) . ?
C21 C22 1.383(16) . ?
C22 Cl2 1.777(15) . ?
Cl3 C23 1.791(16) . ?
C23 C24 1.448(19) . ?
C24 Cl4 1.784(16) . ?

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
N1 C1 C2 124.1(3) . . ?
C1 C2 C3 118.3(3) . . ?
C4 C3 C2 119.0(3) . . ?
C3 C4 C5 120.2(3) . . ?
N1 C5 N5 115.3(2) . . ?
N1 C5 C4 120.5(3) . . ?
N5 C5 C4 123.9(3) . . ?
N2 C6 C7 123.8(3) . . ?
C6 C7 C8 118.0(3) . . ?
C9 C8 C7 120.1(3) . . ?
C8 C9 C10 119.5(3) . . ?
N2 C10 N5 114.9(2) . . ?
N2 C10 C9 120.7(3) . . ?
N5 C10 C9 124.1(3) . . ?
N3 C11 C12 123.8(3) . . ?
C11 C12 C13 118.6(3) . . ?
C14 C13 C12 119.7(3) . . ?
C13 C14 C15 119.7(3) . . ?
N6 C15 N3 115.0(2) 2_655 . ?
N6 C15 C14 124.6(3) 2_655 . ?
N3 C15 C14 120.2(3) . . ?
N4 C16 C17 123.6(3) . . ?
C16 C17 C18 118.5(3) . . ?
C19 C18 C17 119.5(3) . . ?
C18 C19 C20 119.8(3) . . ?
N4 C20 N6 114.5(2) . . ?
N4 C20 C19 120.5(2) . . ?
N6 C20 C19 124.7(2) . . ?
N4 Co1 N2 166.56(9) . 2_655 ?
N4 Co1 N3 89.86(9) . . ?
N2 Co1 N3 89.43(9) 2_655 . ?
N4 Co1 N1 88.38(9) . . ?
N2 Co1 N1 89.28(9) 2_655 . ?
N3 Co1 N1 166.91(9) . . ?
N4 Co1 Co2 83.54(6) . . ?
N2 Co1 Co2 83.05(6) 2_655 . ?
N3 Co1 Co2 83.27(6) . . ?
N1 Co1 Co2 83.64(6) . . ?
N4 Co1 I1 97.17(6) . . ?
N2 Co1 I1 96.25(6) 2_655 . ?
N3 Co1 I1 96.46(6) . . ?
N1 Co1 I1 96.63(6) . . ?
Co2 Co1 I1 179.246(17) . . ?
N5 Co2 N5 89.09(14) . 2_655 ?
N5 Co2 N6 179.31(10) . 2_655 ?
N5 Co2 N6 90.30(10) 2_655 2_655 ?
N5 Co2 N6 90.29(10) . . ?
N5 Co2 N6 179.31(10) 2_655 . ?
N6 Co2 N6 90.32(14) 2_655 . ?
N5 Co2 Co1 90.17(7) . 2_655 ?
N5 Co2 Co1 90.19(7) 2_655 2_655 ?
N6 Co2 Co1 89.52(6) 2_655 2_655 ?
N6 Co2 Co1 90.12(6) . 2_655 ?
N5 Co2 Co1 90.19(7) . . ?
N5 Co2 Co1 90.17(7) 2_655 . ?
N6 Co2 Co1 90.12(6) 2_655 . ?
N6 Co2 Co1 89.52(6) . . ?
Co1 Co2 Co1 179.49(3) 2_655 . ?
C1 N1 C5 117.7(3) . . ?
C1 N1 Co1 121.9(2) . . ?
C5 N1 Co1 120.38(18) . . ?
C6 N2 C10 117.8(3) . . ?
C6 N2 Co1 121.3(2) . 2_655 ?
C10 N2 Co1 120.78(18) . 2_655 ?
C11 N3 C15 117.8(2) . . ?
C11 N3 Co1 121.55(19) . . ?
C15 N3 Co1 120.52(18) . . ?
C16 N4 C20 118.0(2) . . ?
C16 N4 Co1 121.2(2) . . ?
C20 N4 Co1 120.70(18) . . ?
C10 N5 C5 124.3(2) . . ?
C10 N5 Co2 117.89(18) . . ?
C5 N5 Co2 117.85(18) . . ?
C15 N6 C20 124.0(2) 2_655 . ?
C15 N6 Co2 117.88(17) 2_655 . ?
C20 N6 Co2 118.13(18) . . ?
C22 C21 Cl1 118.2(15) . . ?
C21 C22 Cl2 112.1(14) . . ?
C24 C23 Cl3 112.7(15) . . ?
C23 C24 Cl4 113.0(16) . . ?

_refine_diff_density_max         0.403
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.071


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dichloroethane'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_3-Et2O-85K
_database_code_depnum_ccdc_archive 'CCDC 1865586'
_audit_update_record             
;
2018-09-03 deposited with the CCDC.
2018-11-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C40 H32 Br2 Co3 N12, C4 H10 O'
_chemical_formula_sum            'C44 H42 Br2 Co3 N12 O'
_chemical_formula_weight         1091.50

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   16.0028(4)
_cell_length_b                   15.7192(4)
_cell_length_c                   17.0322(4)
_cell_angle_alpha                90
_cell_angle_beta                 100.480(1)
_cell_angle_gamma                90
_cell_volume                     4213.00(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    85(2)
_cell_measurement_reflns_used    9945
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      36.30

_exptl_crystal_description       block
_exptl_crystal_colour            'light brown'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_F_000             2196
_exptl_transmission_factor_min   0.6104
_exptl_transmission_factor_max   0.7471
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    3.117
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6661
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_process_details   '(SADABS; Bruker, 2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      85(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            177381
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.777
_diffrn_reflns_theta_max         36.363
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             20493
_reflns_number_gt                17333
_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       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_structure_solution    'SHELXS2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'CWingGX (Farrugia, 2012)'
_computing_publication_material  'SHELXL-2016/4 (Sheldrick, 2016)'
_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)+(0.0307P)²+2.4979P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         20493
_refine_ls_number_parameters     561
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0263
_refine_ls_wR_factor_ref         0.0682
_refine_ls_wR_factor_gt          0.0655
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.004
_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
C1 C 0.47850(7) 0.47438(7) 0.72578(7) 0.01090(18) Uani 1 1 d . . . . .
H1 H 0.458533 0.524711 0.747121 0.013 Uiso 1 1 calc R U . . .
C1S C 0.16760(10) 0.45292(10) 0.61239(9) 0.0229(3) Uani 1 1 d . . . . .
H1SA H 0.128251 0.494792 0.627930 0.034 Uiso 1 1 calc R U . . .
H1SB H 0.138901 0.420988 0.565782 0.034 Uiso 1 1 calc R U . . .
H1SC H 0.217185 0.482305 0.599032 0.034 Uiso 1 1 calc R U . . .
C2 C 0.41993(7) 0.42181(8) 0.68032(7) 0.01250(19) Uani 1 1 d . . . . .
H2 H 0.360956 0.434601 0.671976 0.015 Uiso 1 1 calc R U . . .
C2S C 0.19596(8) 0.39252(8) 0.68063(7) 0.0145(2) Uani 1 1 d . . . . .
H2SA H 0.146350 0.361535 0.693599 0.017 Uiso 1 1 calc R U . . .
H2SB H 0.236217 0.350357 0.665567 0.017 Uiso 1 1 calc R U . . .
C3 C 0.44946(7) 0.34927(8) 0.64683(7) 0.01182(19) Uani 1 1 d . . . . .
H3 H 0.410662 0.311870 0.615000 0.014 Uiso 1 1 calc R U . . .
C3S C 0.27644(8) 0.38647(8) 0.81143(7) 0.0148(2) Uani 1 1 d . . . . .
H3SA H 0.317990 0.348776 0.792179 0.018 Uiso 1 1 calc R U . . .
H3SB H 0.233516 0.350480 0.830608 0.018 Uiso 1 1 calc R U . . .
C4 C 0.53551(7) 0.33230(7) 0.66034(7) 0.01040(18) Uani 1 1 d . . . . .
H4 H 0.556282 0.283758 0.636767 0.012 Uiso 1 1 calc R U . . .
C4S C 0.32111(9) 0.44203(10) 0.87847(8) 0.0197(2) Uani 1 1 d . . . . .
H4SA H 0.362285 0.478588 0.858576 0.029 Uiso 1 1 calc R U . . .
H4SB H 0.350798 0.406106 0.921734 0.029 Uiso 1 1 calc R U . . .
H4SC H 0.279227 0.477462 0.898592 0.029 Uiso 1 1 calc R U . . .
C5 C 0.59267(7) 0.38707(7) 0.70919(6) 0.00800(16) Uani 1 1 d . . . . .
C6 C 0.71942(7) 0.30154(7) 0.72119(6) 0.00797(16) Uani 1 1 d . . . . .
C7 C 0.68582(8) 0.22201(7) 0.73862(7) 0.01144(18) Uani 1 1 d . . . . .
H7 H 0.628397 0.217990 0.745626 0.014 Uiso 1 1 calc R U . . .
C8 C 0.73607(8) 0.15043(7) 0.74547(7) 0.0140(2) Uani 1 1 d . . . . .
H8 H 0.713268 0.096653 0.755854 0.017 Uiso 1 1 calc R U . . .
C9 C 0.82105(8) 0.15766(7) 0.73698(7) 0.0140(2) Uani 1 1 d . . . . .
H9 H 0.857696 0.109636 0.743748 0.017 Uiso 1 1 calc R U . . .
C10 C 0.85028(8) 0.23645(7) 0.71849(7) 0.01103(18) Uani 1 1 d . . . . .
H10 H 0.908169 0.241534 0.713279 0.013 Uiso 1 1 calc R U . . .
C11 C 0.57463(7) 0.69221(7) 0.71305(7) 0.01085(18) Uani 1 1 d . . . . .
H11 H 0.559385 0.708506 0.762280 0.013 Uiso 1 1 calc R U . . .
C12 C 0.55095(8) 0.74471(7) 0.64796(7) 0.01315(19) Uani 1 1 d . . . . .
H12 H 0.517518 0.794011 0.651537 0.016 Uiso 1 1 calc R U . . .
C13 C 0.57736(8) 0.72358(8) 0.57649(7) 0.0134(2) Uani 1 1 d . . . . .
H13 H 0.562892 0.758816 0.530715 0.016 Uiso 1 1 calc R U . . .
C14 C 0.62469(8) 0.65084(7) 0.57363(7) 0.01159(19) Uani 1 1 d . . . . .
H14 H 0.645092 0.637015 0.526200 0.014 Uiso 1 1 calc R U . . .
C15 C 0.64319(7) 0.59644(7) 0.64096(6) 0.00828(16) Uani 1 1 d . . . . .
C16 C 0.68782(7) 0.47388(7) 0.57571(6) 0.00811(16) Uani 1 1 d . . . . .
C17 C 0.61850(8) 0.47027(7) 0.51129(7) 0.01186(19) Uani 1 1 d . . . . .
H17 H 0.571535 0.507507 0.510186 0.014 Uiso 1 1 calc R U . . .
C18 C 0.61862(8) 0.41310(8) 0.45010(7) 0.0138(2) Uani 1 1 d . . . . .
H18 H 0.571556 0.409861 0.407248 0.017 Uiso 1 1 calc R U . . .
C19 C 0.68869(8) 0.36002(8) 0.45183(7) 0.0137(2) Uani 1 1 d . . . . .
H19 H 0.690951 0.320773 0.409847 0.016 Uiso 1 1 calc R U . . .
C20 C 0.75475(8) 0.36601(7) 0.51622(6) 0.01117(18) Uani 1 1 d . . . . .
H20 H 0.802389 0.329647 0.517448 0.013 Uiso 1 1 calc R U . . .
C21 C 0.73306(8) 0.65135(7) 0.92844(6) 0.01085(18) Uani 1 1 d . . . . .
H21 H 0.683414 0.642402 0.950604 0.013 Uiso 1 1 calc R U . . .
C22 C 0.79644(8) 0.70149(8) 0.97015(7) 0.01284(19) Uani 1 1 d . . . . .
H22 H 0.789768 0.728415 1.018567 0.015 Uiso 1 1 calc R U . . .
C23 C 0.87102(8) 0.71167(8) 0.93915(7) 0.01217(19) Uani 1 1 d . . . . .
H23 H 0.916216 0.745622 0.966513 0.015 Uiso 1 1 calc R U . . .
C24 C 0.87830(7) 0.67201(7) 0.86864(6) 0.01007(18) Uani 1 1 d . . . . .
H24 H 0.929424 0.677094 0.848082 0.012 Uiso 1 1 calc R U . . .
C25 C 0.81001(7) 0.62382(7) 0.82681(6) 0.00727(16) Uani 1 1 d . . . . .
C26 C 0.86330(7) 0.60009(7) 0.70489(6) 0.00753(16) Uani 1 1 d . . . . .
C27 C 0.89412(7) 0.68297(7) 0.69486(6) 0.01027(18) Uani 1 1 d . . . . .
H27 H 0.879696 0.728390 0.726689 0.012 Uiso 1 1 calc R U . . .
C28 C 0.94491(8) 0.69819(7) 0.63924(7) 0.01185(19) Uani 1 1 d . . . . .
H28 H 0.967508 0.753363 0.634032 0.014 Uiso 1 1 calc R U . . .
C29 C 0.96291(8) 0.63141(8) 0.59040(7) 0.01201(19) Uani 1 1 d . . . . .
H29 H 0.998379 0.640038 0.552027 0.014 Uiso 1 1 calc R U . . .
C30 C 0.92765(7) 0.55283(7) 0.59965(6) 0.01033(18) Uani 1 1 d . . . . .
H30 H 0.936915 0.508365 0.564438 0.012 Uiso 1 1 calc R U . . .
C31 C 0.62567(8) 0.42924(7) 0.93634(7) 0.01127(18) Uani 1 1 d . . . . .
H31 H 0.569628 0.451692 0.925899 0.014 Uiso 1 1 calc R U . . .
C32 C 0.64779(8) 0.37565(8) 1.00094(7) 0.0141(2) Uani 1 1 d . . . . .
H32 H 0.608726 0.363072 1.035179 0.017 Uiso 1 1 calc R U . . .
C33 C 0.72900(8) 0.34054(7) 1.01450(7) 0.0136(2) Uani 1 1 d . . . . .
H33 H 0.747102 0.305319 1.059719 0.016 Uiso 1 1 calc R U . . .
C34 C 0.78304(8) 0.35724(7) 0.96183(7) 0.01115(18) Uani 1 1 d . . . . .
H34 H 0.837096 0.330442 0.968786 0.013 Uiso 1 1 calc R U . . .
C35 C 0.75819(7) 0.41408(7) 0.89759(6) 0.00816(16) Uani 1 1 d . . . . .
C36 C 0.89162(7) 0.42579(7) 0.84888(6) 0.00759(16) Uani 1 1 d . . . . .
C37 C 0.94991(7) 0.42729(7) 0.92216(7) 0.01126(18) Uani 1 1 d . . . . .
H37 H 0.929722 0.423702 0.971171 0.014 Uiso 1 1 calc R U . . .
C38 C 1.03585(8) 0.43393(8) 0.92255(7) 0.01277(19) Uani 1 1 d . . . . .
H38 H 1.074920 0.434468 0.971745 0.015 Uiso 1 1 calc R U . . .
C39 C 1.06544(7) 0.43987(8) 0.85036(7) 0.01312(19) Uani 1 1 d . . . . .
H39 H 1.124164 0.447250 0.849380 0.016 Uiso 1 1 calc R U . . .
C40 C 1.00644(7) 0.43464(7) 0.78077(7) 0.01062(18) Uani 1 1 d . . . . .
H40 H 1.026056 0.438045 0.731461 0.013 Uiso 1 1 calc R U . . .
N1 N 0.56314(6) 0.45816(6) 0.74171(5) 0.00827(15) Uani 1 1 d . . . . .
N2 N 0.61846(6) 0.61863(6) 0.71086(5) 0.00818(15) Uani 1 1 d . . . . .
N3 N 0.73732(6) 0.61389(6) 0.85744(5) 0.00784(15) Uani 1 1 d . . . . .
N4 N 0.67960(6) 0.45162(6) 0.88689(5) 0.00825(15) Uani 1 1 d . . . . .
N5 N 0.67885(6) 0.37778(6) 0.72289(5) 0.00768(14) Uani 1 1 d . . . . .
N6 N 0.68865(6) 0.52290(6) 0.64240(5) 0.00765(15) Uani 1 1 d . . . . .
N7 N 0.81257(6) 0.57881(6) 0.75833(5) 0.00733(14) Uani 1 1 d . . . . .
N8 N 0.80529(6) 0.43254(6) 0.84018(5) 0.00752(14) Uani 1 1 d . . . . .
N9 N 0.80076(6) 0.30694(6) 0.70739(5) 0.00810(15) Uani 1 1 d . . . . .
N10 N 0.75547(6) 0.42084(6) 0.57779(5) 0.00796(15) Uani 1 1 d . . . . .
N11 N 0.88047(6) 0.53557(6) 0.65628(5) 0.00742(14) Uani 1 1 d . . . . .
N12 N 0.92203(6) 0.42490(6) 0.77875(5) 0.00793(15) Uani 1 1 d . . . . .
O1S O 0.23624(6) 0.44017(6) 0.74826(5) 0.01286(15) Uani 1 1 d . . . . .
CO1 Co 0.64315(2) 0.54010(2) 0.80339(2) 0.00632(3) Uani 1 1 d . . . . .
CO2 Co 0.74652(2) 0.47769(2) 0.74180(2) 0.00586(3) Uani 1 1 d . . . . .
CO3 Co 0.84540(2) 0.41769(2) 0.67455(2) 0.00603(3) Uani 1 1 d . . . . .
BR1 Br 0.52732(2) 0.60994(2) 0.87976(2) 0.01273(3) Uani 1 1 d . . . . .
BR2 Br 0.95608(2) 0.34092(2) 0.60332(2) 0.01261(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.3563(15) . ?
C1 C2 1.3772(17) . ?
C1 H1 0.9500 . ?
C1S C2S 1.5055(19) . ?
C1S H1SA 0.9800 . ?
C1S H1SB 0.9800 . ?
C1S H1SC 0.9800 . ?
C2 C3 1.3953(17) . ?
C2 H2 0.9500 . ?
C2S O1S 1.4259(15) . ?
C2S H2SA 0.9900 . ?
C2S H2SB 0.9900 . ?
C3 C4 1.3803(17) . ?
C3 H3 0.9500 . ?
C3S O1S 1.4255(15) . ?
C3S C4S 1.5102(19) . ?
C3S H3SA 0.9900 . ?
C3S H3SB 0.9900 . ?
C4 C5 1.4119(15) . ?
C4 H4 0.9500 . ?
C4S H4SA 0.9800 . ?
C4S H4SB 0.9800 . ?
C4S H4SC 0.9800 . ?
C5 N5 1.3639(14) . ?
C5 N1 1.3691(14) . ?
C6 N5 1.3658(14) . ?
C6 N9 1.3667(14) . ?
C6 C7 1.4137(15) . ?
C7 C8 1.3755(17) . ?
C7 H7 0.9500 . ?
C8 C9 1.3982(18) . ?
C8 H8 0.9500 . ?
C9 C10 1.3803(17) . ?
C9 H9 0.9500 . ?
C10 N9 1.3554(14) . ?
C10 H10 0.9500 . ?
C11 N2 1.3567(14) . ?
C11 C12 1.3788(16) . ?
C11 H11 0.9500 . ?
C12 C13 1.3992(17) . ?
C12 H12 0.9500 . ?
C13 C14 1.3773(17) . ?
C13 H13 0.9500 . ?
C14 C15 1.4179(15) . ?
C14 H14 0.9500 . ?
C15 N6 1.3637(14) . ?
C15 N2 1.3664(14) . ?
C16 N10 1.3617(14) . ?
C16 N6 1.3708(14) . ?
C16 C17 1.4124(15) . ?
C17 C18 1.3765(16) . ?
C17 H17 0.9500 . ?
C18 C19 1.3937(18) . ?
C18 H18 0.9500 . ?
C19 C20 1.3812(17) . ?
C19 H19 0.9500 . ?
C20 N10 1.3558(14) . ?
C20 H20 0.9500 . ?
C21 N3 1.3578(14) . ?
C21 C22 1.3758(17) . ?
C21 H21 0.9500 . ?
C22 C23 1.3993(17) . ?
C22 H22 0.9500 . ?
C23 C24 1.3768(15) . ?
C23 H23 0.9500 . ?
C24 C25 1.4116(15) . ?
C24 H24 0.9500 . ?
C25 N3 1.3677(14) . ?
C25 N7 1.3711(13) . ?
C26 N7 1.3668(13) . ?
C26 N11 1.3684(14) . ?
C26 C27 1.4142(15) . ?
C27 C28 1.3767(15) . ?
C27 H27 0.9500 . ?
C28 C29 1.4015(17) . ?
C28 H28 0.9500 . ?
C29 C30 1.3790(16) . ?
C29 H29 0.9500 . ?
C30 N11 1.3560(14) . ?
C30 H30 0.9500 . ?
C31 N4 1.3573(14) . ?
C31 C32 1.3799(16) . ?
C31 H31 0.9500 . ?
C32 C33 1.3920(18) . ?
C32 H32 0.9500 . ?
C33 C34 1.3797(16) . ?
C33 H33 0.9500 . ?
C34 C35 1.4125(15) . ?
C34 H34 0.9500 . ?
C35 N8 1.3697(14) . ?
C35 N4 1.3711(14) . ?
C36 N8 1.3666(14) . ?
C36 N12 1.3695(13) . ?
C36 C37 1.4159(15) . ?
C37 C38 1.3781(17) . ?
C37 H37 0.9500 . ?
C38 C39 1.3987(17) . ?
C38 H38 0.9500 . ?
C39 C40 1.3770(16) . ?
C39 H39 0.9500 . ?
C40 N12 1.3537(15) . ?
C40 H40 0.9500 . ?
N1 CO1 1.9780(10) . ?
N2 CO1 1.9843(9) . ?
N3 CO1 1.9898(10) . ?
N4 CO1 1.9988(9) . ?
N5 CO2 1.9016(9) . ?
N6 CO2 1.9128(9) . ?
N7 CO2 1.9013(9) . ?
N8 CO2 1.9033(9) . ?
N9 CO3 1.9998(9) . ?
N10 CO3 1.9816(9) . ?
N11 CO3 1.9771(9) . ?
N12 CO3 1.9685(9) . ?
CO1 CO2 2.3303(2) . ?
CO1 BR1 2.68524(19) . ?
CO2 CO3 2.3162(2) . ?
CO3 BR2 2.61670(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
N1 C1 C2 123.54(11) . . ?
N1 C1 H1 118.2 . . ?
C2 C1 H1 118.2 . . ?
C2S C1S H1SA 109.5 . . ?
C2S C1S H1SB 109.5 . . ?
H1SA C1S H1SB 109.5 . . ?
C2S C1S H1SC 109.5 . . ?
H1SA C1S H1SC 109.5 . . ?
H1SB C1S H1SC 109.5 . . ?
C1 C2 C3 118.28(11) . . ?
C1 C2 H2 120.9 . . ?
C3 C2 H2 120.9 . . ?
O1S C2S C1S 108.71(11) . . ?
O1S C2S H2SA 109.9 . . ?
C1S C2S H2SA 109.9 . . ?
O1S C2S H2SB 109.9 . . ?
C1S C2S H2SB 109.9 . . ?
H2SA C2S H2SB 108.3 . . ?
C4 C3 C2 119.44(11) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
O1S C3S C4S 108.35(10) . . ?
O1S C3S H3SA 110.0 . . ?
C4S C3S H3SA 110.0 . . ?
O1S C3S H3SB 110.0 . . ?
C4S C3S H3SB 110.0 . . ?
H3SA C3S H3SB 108.4 . . ?
C3 C4 C5 120.02(11) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C3S C4S H4SA 109.5 . . ?
C3S C4S H4SB 109.5 . . ?
H4SA C4S H4SB 109.5 . . ?
C3S C4S H4SC 109.5 . . ?
H4SA C4S H4SC 109.5 . . ?
H4SB C4S H4SC 109.5 . . ?
N5 C5 N1 115.52(9) . . ?
N5 C5 C4 124.20(10) . . ?
N1 C5 C4 120.12(10) . . ?
N5 C6 N9 114.87(9) . . ?
N5 C6 C7 124.82(10) . . ?
N9 C6 C7 120.11(10) . . ?
C8 C7 C6 120.16(11) . . ?
C8 C7 H7 119.9 . . ?
C6 C7 H7 119.9 . . ?
C7 C8 C9 119.30(11) . . ?
C7 C8 H8 120.4 . . ?
C9 C8 H8 120.4 . . ?
C10 C9 C8 118.22(11) . . ?
C10 C9 H9 120.9 . . ?
C8 C9 H9 120.9 . . ?
N9 C10 C9 123.48(11) . . ?
N9 C10 H10 118.3 . . ?
C9 C10 H10 118.3 . . ?
N2 C11 C12 123.77(10) . . ?
N2 C11 H11 118.1 . . ?
C12 C11 H11 118.1 . . ?
C11 C12 C13 118.38(11) . . ?
C11 C12 H12 120.8 . . ?
C13 C12 H12 120.8 . . ?
C14 C13 C12 118.87(11) . . ?
C14 C13 H13 120.6 . . ?
C12 C13 H13 120.6 . . ?
C13 C14 C15 120.49(10) . . ?
C13 C14 H14 119.8 . . ?
C15 C14 H14 119.8 . . ?
N6 C15 N2 116.03(9) . . ?
N6 C15 C14 123.92(10) . . ?
N2 C15 C14 119.98(10) . . ?
N10 C16 N6 115.77(9) . . ?
N10 C16 C17 120.27(10) . . ?
N6 C16 C17 123.65(10) . . ?
C18 C17 C16 120.35(11) . . ?
C18 C17 H17 119.8 . . ?
C16 C17 H17 119.8 . . ?
C17 C18 C19 119.14(11) . . ?
C17 C18 H18 120.4 . . ?
C19 C18 H18 120.4 . . ?
C20 C19 C18 118.20(11) . . ?
C20 C19 H19 120.9 . . ?
C18 C19 H19 120.9 . . ?
N10 C20 C19 123.72(11) . . ?
N10 C20 H20 118.1 . . ?
C19 C20 H20 118.1 . . ?
N3 C21 C22 123.82(11) . . ?
N3 C21 H21 118.1 . . ?
C22 C21 H21 118.1 . . ?
C21 C22 C23 118.03(10) . . ?
C21 C22 H22 121.0 . . ?
C23 C22 H22 121.0 . . ?
C24 C23 C22 119.39(11) . . ?
C24 C23 H23 120.3 . . ?
C22 C23 H23 120.3 . . ?
C23 C24 C25 120.18(10) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
N3 C25 N7 115.13(9) . . ?
N3 C25 C24 120.18(9) . . ?
N7 C25 C24 124.48(10) . . ?
N7 C26 N11 115.50(9) . . ?
N7 C26 C27 124.63(10) . . ?
N11 C26 C27 119.79(9) . . ?
C28 C27 C26 120.38(10) . . ?
C28 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
C27 C28 C29 119.28(11) . . ?
C27 C28 H28 120.4 . . ?
C29 C28 H28 120.4 . . ?
C30 C29 C28 118.07(10) . . ?
C30 C29 H29 121.0 . . ?
C28 C29 H29 121.0 . . ?
N11 C30 C29 123.56(10) . . ?
N11 C30 H30 118.2 . . ?
C29 C30 H30 118.2 . . ?
N4 C31 C32 123.59(11) . . ?
N4 C31 H31 118.2 . . ?
C32 C31 H31 118.2 . . ?
C31 C32 C33 118.08(11) . . ?
C31 C32 H32 121.0 . . ?
C33 C32 H32 121.0 . . ?
C34 C33 C32 119.57(11) . . ?
C34 C33 H33 120.2 . . ?
C32 C33 H33 120.2 . . ?
C33 C34 C35 120.17(11) . . ?
C33 C34 H34 119.9 . . ?
C35 C34 H34 119.9 . . ?
N8 C35 N4 115.12(9) . . ?
N8 C35 C34 124.96(10) . . ?
N4 C35 C34 119.82(10) . . ?
N8 C36 N12 114.76(9) . . ?
N8 C36 C37 125.82(10) . . ?
N12 C36 C37 119.17(10) . . ?
C38 C37 C36 120.16(10) . . ?
C38 C37 H37 119.9 . . ?
C36 C37 H37 119.9 . . ?
C37 C38 C39 119.86(11) . . ?
C37 C38 H38 120.1 . . ?
C39 C38 H38 120.1 . . ?
C40 C39 C38 117.64(11) . . ?
C40 C39 H39 121.2 . . ?
C38 C39 H39 121.2 . . ?
N12 C40 C39 123.60(10) . . ?
N12 C40 H40 118.2 . . ?
C39 C40 H40 118.2 . . ?
C1 N1 C5 118.56(10) . . ?
C1 N1 CO1 120.69(8) . . ?
C5 N1 CO1 120.57(7) . . ?
C11 N2 C15 118.35(9) . . ?
C11 N2 CO1 122.53(7) . . ?
C15 N2 CO1 119.07(7) . . ?
C21 N3 C25 118.31(10) . . ?
C21 N3 CO1 120.55(8) . . ?
C25 N3 CO1 121.01(7) . . ?
C31 N4 C35 118.51(9) . . ?
C31 N4 CO1 119.06(8) . . ?
C35 N4 CO1 122.40(7) . . ?
C5 N5 C6 124.06(9) . . ?
C5 N5 CO2 117.87(7) . . ?
C6 N5 CO2 118.03(7) . . ?
C15 N6 C16 122.47(9) . . ?
C15 N6 CO2 120.12(7) . . ?
C16 N6 CO2 117.05(7) . . ?
C26 N7 C25 123.60(9) . . ?
C26 N7 CO2 119.18(7) . . ?
C25 N7 CO2 117.10(7) . . ?
C36 N8 C35 125.65(9) . . ?
C36 N8 CO2 116.89(7) . . ?
C35 N8 CO2 117.36(7) . . ?
C10 N9 C6 118.43(10) . . ?
C10 N9 CO3 121.41(8) . . ?
C6 N9 CO3 120.13(7) . . ?
C20 N10 C16 118.31(10) . . ?
C20 N10 CO3 122.01(8) . . ?
C16 N10 CO3 119.38(7) . . ?
C30 N11 C26 118.76(9) . . ?
C30 N11 CO3 120.67(7) . . ?
C26 N11 CO3 120.36(7) . . ?
C40 N12 C36 119.21(9) . . ?
C40 N12 CO3 118.98(7) . . ?
C36 N12 CO3 121.68(7) . . ?
C3S O1S C2S 111.98(9) . . ?
N1 CO1 N2 88.12(4) . . ?
N1 CO1 N3 171.08(4) . . ?
N2 CO1 N3 91.68(4) . . ?
N1 CO1 N4 90.10(4) . . ?
N2 CO1 N4 171.18(4) . . ?
N3 CO1 N4 88.74(4) . . ?
N1 CO1 CO2 86.03(3) . . ?
N2 CO1 CO2 87.68(3) . . ?
N3 CO1 CO2 85.05(3) . . ?
N4 CO1 CO2 83.58(3) . . ?
N1 CO1 BR1 94.95(3) . . ?
N2 CO1 BR1 94.31(3) . . ?
N3 CO1 BR1 93.96(3) . . ?
N4 CO1 BR1 94.45(3) . . ?
CO2 CO1 BR1 177.811(8) . . ?
N7 CO2 N5 178.55(4) . . ?
N7 CO2 N8 90.52(4) . . ?
N5 CO2 N8 90.92(4) . . ?
N7 CO2 N6 89.25(4) . . ?
N5 CO2 N6 89.30(4) . . ?
N8 CO2 N6 179.32(4) . . ?
N7 CO2 CO3 90.13(3) . . ?
N5 CO2 CO3 89.96(3) . . ?
N8 CO2 CO3 90.63(3) . . ?
N6 CO2 CO3 88.73(3) . . ?
N7 CO2 CO1 90.14(3) . . ?
N5 CO2 CO1 89.71(3) . . ?
N8 CO2 CO1 92.19(3) . . ?
N6 CO2 CO1 88.45(3) . . ?
CO3 CO2 CO1 177.165(9) . . ?
N12 CO3 N11 86.55(4) . . ?
N12 CO3 N10 170.93(4) . . ?
N11 CO3 N10 91.70(4) . . ?
N12 CO3 N9 89.63(4) . . ?
N11 CO3 N9 170.39(4) . . ?
N10 CO3 N9 90.69(4) . . ?
N12 CO3 CO2 84.27(3) . . ?
N11 CO3 CO2 86.29(3) . . ?
N10 CO3 CO2 86.73(3) . . ?
N9 CO3 CO2 84.56(3) . . ?
N12 CO3 BR2 94.66(3) . . ?
N11 CO3 BR2 97.11(3) . . ?
N10 CO3 BR2 94.38(3) . . ?
N9 CO3 BR2 91.98(3) . . ?
CO2 CO3 BR2 176.380(8) . . ?

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
N1 C1 C2 C3 -2.01(18) . . . . ?
C1 C2 C3 C4 0.26(17) . . . . ?
C2 C3 C4 C5 1.45(17) . . . . ?
C3 C4 C5 N5 -176.77(10) . . . . ?
C3 C4 C5 N1 -1.55(16) . . . . ?
N5 C6 C7 C8 -171.43(11) . . . . ?
N9 C6 C7 C8 3.06(16) . . . . ?
C6 C7 C8 C9 1.58(18) . . . . ?
C7 C8 C9 C10 -2.77(18) . . . . ?
C8 C9 C10 N9 -0.66(18) . . . . ?
N2 C11 C12 C13 -3.57(18) . . . . ?
C11 C12 C13 C14 0.95(18) . . . . ?
C12 C13 C14 C15 2.67(18) . . . . ?
C13 C14 C15 N6 179.15(11) . . . . ?
C13 C14 C15 N2 -3.98(17) . . . . ?
N10 C16 C17 C18 0.07(17) . . . . ?
N6 C16 C17 C18 -173.28(11) . . . . ?
C16 C17 C18 C19 -1.20(18) . . . . ?
C17 C18 C19 C20 1.28(18) . . . . ?
C18 C19 C20 N10 -0.24(18) . . . . ?
N3 C21 C22 C23 -2.67(18) . . . . ?
C21 C22 C23 C24 0.30(18) . . . . ?
C22 C23 C24 C25 2.03(17) . . . . ?
C23 C24 C25 N3 -2.20(17) . . . . ?
C23 C24 C25 N7 -176.77(11) . . . . ?
N7 C26 C27 C28 -179.92(11) . . . . ?
N11 C26 C27 C28 -3.34(17) . . . . ?
C26 C27 C28 C29 2.59(17) . . . . ?
C27 C28 C29 C30 0.83(17) . . . . ?
C28 C29 C30 N11 -3.77(18) . . . . ?
N4 C31 C32 C33 -2.15(18) . . . . ?
C31 C32 C33 C34 -2.66(18) . . . . ?
C32 C33 C34 C35 4.20(18) . . . . ?
C33 C34 C35 N8 -177.26(11) . . . . ?
C33 C34 C35 N4 -1.06(17) . . . . ?
N8 C36 C37 C38 -169.35(11) . . . . ?
N12 C36 C37 C38 4.61(17) . . . . ?
C36 C37 C38 C39 0.50(18) . . . . ?
C37 C38 C39 C40 -3.07(18) . . . . ?
C38 C39 C40 N12 0.61(18) . . . . ?
C2 C1 N1 C5 1.92(16) . . . . ?
C2 C1 N1 CO1 177.10(9) . . . . ?
N5 C5 N1 C1 175.52(9) . . . . ?
C4 C5 N1 C1 -0.11(15) . . . . ?
N5 C5 N1 CO1 0.33(13) . . . . ?
C4 C5 N1 CO1 -175.29(8) . . . . ?
C12 C11 N2 C15 2.30(17) . . . . ?
C12 C11 N2 CO1 -174.85(9) . . . . ?
N6 C15 N2 C11 178.61(10) . . . . ?
C14 C15 N2 C11 1.50(16) . . . . ?
N6 C15 N2 CO1 -4.14(13) . . . . ?
C14 C15 N2 CO1 178.75(8) . . . . ?
C22 C21 N3 C25 2.52(17) . . . . ?
C22 C21 N3 CO1 178.44(9) . . . . ?
N7 C25 N3 C21 175.02(10) . . . . ?
C24 C25 N3 C21 -0.03(15) . . . . ?
N7 C25 N3 CO1 -0.88(13) . . . . ?
C24 C25 N3 CO1 -175.93(8) . . . . ?
C32 C31 N4 C35 5.28(17) . . . . ?
C32 C31 N4 CO1 -173.04(9) . . . . ?
N8 C35 N4 C31 172.99(10) . . . . ?
C34 C35 N4 C31 -3.56(15) . . . . ?
N8 C35 N4 CO1 -8.75(13) . . . . ?
C34 C35 N4 CO1 174.69(8) . . . . ?
N1 C5 N5 C6 156.19(10) . . . . ?
C4 C5 N5 C6 -28.39(16) . . . . ?
N1 C5 N5 CO2 -26.13(12) . . . . ?
C4 C5 N5 CO2 149.29(9) . . . . ?
N9 C6 N5 C5 157.27(10) . . . . ?
C7 C6 N5 C5 -27.99(16) . . . . ?
N9 C6 N5 CO2 -20.41(12) . . . . ?
C7 C6 N5 CO2 154.33(9) . . . . ?
N2 C15 N6 C16 151.99(10) . . . . ?
C14 C15 N6 C16 -31.02(17) . . . . ?
N2 C15 N6 CO2 -20.89(13) . . . . ?
C14 C15 N6 CO2 156.09(9) . . . . ?
N10 C16 N6 C15 158.12(10) . . . . ?
C17 C16 N6 C15 -28.26(16) . . . . ?
N10 C16 N6 CO2 -28.79(12) . . . . ?
C17 C16 N6 CO2 144.83(9) . . . . ?
N11 C26 N7 C25 158.46(10) . . . . ?
C27 C26 N7 C25 -24.82(17) . . . . ?
N11 C26 N7 CO2 -17.46(13) . . . . ?
C27 C26 N7 CO2 159.26(9) . . . . ?
N3 C25 N7 C26 157.44(10) . . . . ?
C24 C25 N7 C26 -27.75(16) . . . . ?
N3 C25 N7 CO2 -26.56(12) . . . . ?
C24 C25 N7 CO2 148.25(9) . . . . ?
N12 C36 N8 C35 162.91(10) . . . . ?
C37 C36 N8 C35 -22.89(17) . . . . ?
N12 C36 N8 CO2 -20.92(12) . . . . ?
C37 C36 N8 CO2 153.27(9) . . . . ?
N4 C35 N8 C36 158.65(10) . . . . ?
C34 C35 N8 C36 -25.00(17) . . . . ?
N4 C35 N8 CO2 -17.50(12) . . . . ?
C34 C35 N8 CO2 158.85(9) . . . . ?
C9 C10 N9 C6 5.26(16) . . . . ?
C9 C10 N9 CO3 -176.43(9) . . . . ?
N5 C6 N9 C10 168.67(9) . . . . ?
C7 C6 N9 C10 -6.35(15) . . . . ?
N5 C6 N9 CO3 -9.67(12) . . . . ?
C7 C6 N9 CO3 175.32(8) . . . . ?
C19 C20 N10 C16 -0.89(17) . . . . ?
C19 C20 N10 CO3 172.75(9) . . . . ?
N6 C16 N10 C20 174.81(10) . . . . ?
C17 C16 N10 C20 0.96(15) . . . . ?
N6 C16 N10 CO3 1.00(13) . . . . ?
C17 C16 N10 CO3 -172.85(8) . . . . ?
C29 C30 N11 C26 3.06(17) . . . . ?
C29 C30 N11 CO3 -171.76(9) . . . . ?
N7 C26 N11 C30 177.44(10) . . . . ?
C27 C26 N11 C30 0.55(15) . . . . ?
N7 C26 N11 CO3 -7.72(13) . . . . ?
C27 C26 N11 CO3 175.39(8) . . . . ?
C39 C40 N12 C36 4.52(17) . . . . ?
C39 C40 N12 CO3 -179.62(9) . . . . ?
N8 C36 N12 C40 167.60(10) . . . . ?
C37 C36 N12 C40 -7.01(15) . . . . ?
N8 C36 N12 CO3 -8.15(13) . . . . ?
C37 C36 N12 CO3 177.25(8) . . . . ?
C4S C3S O1S C2S 177.05(10) . . . . ?
C1S C2S O1S C3S -170.94(11) . . . . ?

_refine_diff_density_max         0.737
_refine_diff_density_min         -1.083
_refine_diff_density_rms         0.092


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: DMF, ether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_4-Et2O-298K
_database_code_depnum_ccdc_archive 'CCDC 1865592'
_audit_update_record             
;
2018-09-03 deposited with the CCDC.
2018-11-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C40 H32 Co3 I2 N12, C4 H10 O'
_chemical_formula_sum            'C44 H42 Co3 I2 N12 O'
_chemical_formula_weight         1185.48

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

_cell_length_a                   37.533(9)
_cell_length_b                   12.746(6)
_cell_length_c                   19.056(2)
_cell_angle_alpha                90
_cell_angle_beta                 91.606(10)
_cell_angle_gamma                90
_cell_volume                     9113(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9728
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      25.16

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_F_000             4680
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    2.483
_shelx_estimated_absorpt_T_min   0.772
_shelx_estimated_absorpt_T_max   0.952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4834
_exptl_absorpt_correction_T_max  0.5619
_exptl_absorpt_process_details   '(SADABS; Bruker, 2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            60534
_diffrn_reflns_av_unetI/netI     0.0501
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.989
_diffrn_reflns_theta_max         25.463
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8370
_reflns_number_gt                5506
_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       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_structure_solution    'SHELXS2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_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)+112.7025P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8370
_refine_ls_number_parameters     561
_refine_ls_number_restraints     23
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_gt           0.0493
_refine_ls_wR_factor_ref         0.1036
_refine_ls_wR_factor_gt          0.0830
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_restrained_S_all      1.127
_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
C1 C 0.0583(2) 0.7697(6) 0.1570(4) 0.050(2) Uani 1 1 d . . . . .
H1 H 0.059383 0.833888 0.133927 0.061 Uiso 1 1 calc R U . . .
C2 C 0.0380(2) 0.6918(7) 0.1265(4) 0.061(2) Uani 1 1 d . . . . .
H2 H 0.025856 0.702668 0.083976 0.073 Uiso 1 1 calc R U . . .
C3 C 0.03628(19) 0.5972(7) 0.1607(4) 0.054(2) Uani 1 1 d . . . . .
H3 H 0.022940 0.542509 0.141242 0.065 Uiso 1 1 calc R U . . .
C4 C 0.05428(19) 0.5838(6) 0.2238(4) 0.0485(19) Uani 1 1 d . . . . .
H4 H 0.053001 0.519967 0.247254 0.058 Uiso 1 1 calc R U . . .
C5 C 0.07452(17) 0.6659(6) 0.2527(3) 0.0362(16) Uani 1 1 d . . . . .
C6 C 0.08991(17) 0.5910(5) 0.3661(3) 0.0348(16) Uani 1 1 d . . . . .
C7 C 0.0554(2) 0.5650(7) 0.3884(4) 0.059(2) Uani 1 1 d . . . . .
H7 H 0.035405 0.583071 0.361133 0.071 Uiso 1 1 calc R U . . .
C8 C 0.0518(2) 0.5123(8) 0.4511(4) 0.070(3) Uani 1 1 d . . . . .
H8 H 0.029294 0.496087 0.467147 0.084 Uiso 1 1 calc R U . . .
C9 C 0.0819(2) 0.4841(7) 0.4895(4) 0.067(3) Uani 1 1 d . . . . .
H9 H 0.079860 0.448264 0.531723 0.080 Uiso 1 1 calc R U . . .
C10 C 0.1145(2) 0.5089(6) 0.4655(4) 0.0454(19) Uani 1 1 d . . . . .
H10 H 0.134523 0.490400 0.492539 0.055 Uiso 1 1 calc R U . . .
C11 C 0.1602(2) 0.9171(6) 0.1351(4) 0.0473(19) Uani 1 1 d . . . . .
H11 H 0.151043 0.984736 0.137626 0.057 Uiso 1 1 calc R U . . .
C12 C 0.1852(2) 0.8967(6) 0.0860(4) 0.063(2) Uani 1 1 d . . . . .
H12 H 0.192868 0.949548 0.056314 0.076 Uiso 1 1 calc R U . . .
C13 C 0.1987(2) 0.7969(6) 0.0811(4) 0.052(2) Uani 1 1 d . . . . .
H13 H 0.215417 0.781107 0.047516 0.062 Uiso 1 1 calc R U . . .
C14 C 0.1875(2) 0.7213(6) 0.1258(3) 0.0435(18) Uani 1 1 d . . . . .
H14 H 0.196710 0.653753 0.122974 0.052 Uiso 1 1 calc R U . . .
C15 C 0.16224(17) 0.7446(5) 0.1760(3) 0.0303(15) Uani 1 1 d . . . . .
C16 C 0.15212(17) 0.5704(5) 0.2211(3) 0.0305(15) Uani 1 1 d . . . . .
C17 C 0.1448(2) 0.5169(6) 0.1574(3) 0.0437(18) Uani 1 1 d . . . . .
H17 H 0.144131 0.553405 0.115120 0.052 Uiso 1 1 calc R U . . .
C18 C 0.1387(2) 0.4116(6) 0.1583(4) 0.059(2) Uani 1 1 d . . . . .
H18 H 0.133879 0.375750 0.116574 0.071 Uiso 1 1 calc R U . . .
C19 C 0.1397(2) 0.3582(6) 0.2214(4) 0.054(2) Uani 1 1 d . . . . .
H19 H 0.134553 0.286824 0.222818 0.065 Uiso 1 1 calc R U . . .
C20 C 0.14835(19) 0.4117(5) 0.2816(4) 0.0440(18) Uani 1 1 d . . . . .
H20 H 0.149198 0.375065 0.323826 0.053 Uiso 1 1 calc R U . . .
C21 C 0.1486(2) 1.0690(5) 0.3337(3) 0.0431(18) Uani 1 1 d . . . . .
H21 H 0.127892 1.104241 0.319768 0.052 Uiso 1 1 calc R U . . .
C22 C 0.1741(2) 1.1217(6) 0.3729(4) 0.051(2) Uani 1 1 d . . . . .
H22 H 0.170571 1.191467 0.384995 0.062 Uiso 1 1 calc R U . . .
C23 C 0.2052(2) 1.0709(6) 0.3943(4) 0.052(2) Uani 1 1 d . . . . .
H23 H 0.222827 1.106018 0.420108 0.063 Uiso 1 1 calc R U . . .
C24 C 0.2092(2) 0.9677(5) 0.3765(3) 0.0417(18) Uani 1 1 d . . . . .
H24 H 0.229579 0.931593 0.391345 0.050 Uiso 1 1 calc R U . . .
C25 C 0.18287(18) 0.9159(5) 0.3362(3) 0.0328(16) Uani 1 1 d . . . . .
C26 C 0.21311(17) 0.7540(5) 0.3119(3) 0.0294(15) Uani 1 1 d . . . . .
C27 C 0.24299(18) 0.7946(6) 0.2784(3) 0.0394(17) Uani 1 1 d . . . . .
H27 H 0.244163 0.865890 0.268492 0.047 Uiso 1 1 calc R U . . .
C28 C 0.27041(19) 0.7300(6) 0.2603(4) 0.0437(18) Uani 1 1 d . . . . .
H28 H 0.290077 0.756407 0.237527 0.052 Uiso 1 1 calc R U . . .
C29 C 0.26812(19) 0.6235(6) 0.2770(3) 0.0454(19) Uani 1 1 d . . . . .
H29 H 0.286378 0.577752 0.265637 0.054 Uiso 1 1 calc R U . . .
C30 C 0.23906(18) 0.5879(5) 0.3097(3) 0.0350(16) Uani 1 1 d . . . . .
H30 H 0.237884 0.516765 0.320080 0.042 Uiso 1 1 calc R U . . .
C31 C 0.0474(2) 0.9213(6) 0.3484(4) 0.052(2) Uani 1 1 d . . . . .
H31 H 0.038474 0.949957 0.306607 0.063 Uiso 1 1 calc R U . . .
C32 C 0.0258(2) 0.9214(7) 0.4047(5) 0.062(2) Uani 1 1 d . . . . .
H32 H 0.003019 0.950279 0.401771 0.074 Uiso 1 1 calc R U . . .
C33 C 0.0389(2) 0.8769(7) 0.4661(5) 0.067(2) Uani 1 1 d . . . . .
H33 H 0.024927 0.875921 0.505545 0.080 Uiso 1 1 calc R U . . .
C34 C 0.0722(2) 0.8344(6) 0.4695(4) 0.055(2) Uani 1 1 d . . . . .
H34 H 0.080736 0.803631 0.510921 0.065 Uiso 1 1 calc R U . . .
C35 C 0.09341(19) 0.8373(5) 0.4101(4) 0.0391(17) Uani 1 1 d . . . . .
C36 C 0.14940(17) 0.7709(5) 0.4607(3) 0.0312(15) Uani 1 1 d . . . . .
C37 C 0.15171(19) 0.8335(5) 0.5212(3) 0.0416(18) Uani 1 1 d . . . . .
H37 H 0.134748 0.885278 0.528468 0.050 Uiso 1 1 calc R U . . .
C38 C 0.1788(2) 0.8186(6) 0.5691(4) 0.051(2) Uani 1 1 d . . . . .
H38 H 0.179722 0.857293 0.610499 0.061 Uiso 1 1 calc R U . . .
C39 C 0.2049(2) 0.7450(6) 0.5558(4) 0.050(2) Uani 1 1 d . . . . .
H39 H 0.224560 0.737337 0.586215 0.060 Uiso 1 1 calc R U . . .
C40 C 0.20139(19) 0.6842(6) 0.4972(3) 0.0421(18) Uani 1 1 d . . . . .
H40 H 0.218898 0.634555 0.488509 0.051 Uiso 1 1 calc R U . . .
C41 C -0.0192(5) 0.3009(12) 0.3697(10) 0.187(7) Uani 1 1 d D . . . .
H41A H -0.034011 0.241870 0.380085 0.281 Uiso 1 1 calc R U . . .
H41B H -0.028848 0.337126 0.329334 0.281 Uiso 1 1 calc R U . . .
H41C H -0.018339 0.347758 0.409218 0.281 Uiso 1 1 calc R U . . .
C42 C 0.0168(5) 0.2645(15) 0.3554(9) 0.183(7) Uani 1 1 d D . . . .
H42A H 0.029950 0.319403 0.332154 0.220 Uiso 1 1 calc R U . . .
H42B H 0.015672 0.203871 0.324661 0.220 Uiso 1 1 calc R U . . .
C43 C 0.0701(4) 0.2047(13) 0.4096(8) 0.166(6) Uani 1 1 d D . . . .
H43A H 0.083959 0.263253 0.392556 0.200 Uiso 1 1 calc R U . . .
H43B H 0.070328 0.149458 0.374557 0.200 Uiso 1 1 calc R U . . .
C44 C 0.0860(4) 0.1657(14) 0.4769(7) 0.182(7) Uani 1 1 d D . . . .
H44A H 0.093150 0.224250 0.505708 0.274 Uiso 1 1 calc R U . . .
H44B H 0.106362 0.122973 0.467683 0.274 Uiso 1 1 calc R U . . .
H44C H 0.068631 0.124795 0.500922 0.274 Uiso 1 1 calc R U . . .
N1 N 0.07676(14) 0.7593(5) 0.2185(3) 0.0408(14) Uani 1 1 d . . . . .
N2 N 0.14824(15) 0.8440(4) 0.1801(3) 0.0355(13) Uani 1 1 d . . . . .
N3 N 0.15269(15) 0.9666(4) 0.3146(3) 0.0363(13) Uani 1 1 d . . . . .
N4 N 0.08081(15) 0.8824(4) 0.3494(3) 0.0397(14) Uani 1 1 d . . . . .
N5 N 0.09632(13) 0.6558(4) 0.3113(3) 0.0313(12) Uani 1 1 d . . . . .
N6 N 0.15260(14) 0.6769(4) 0.2280(2) 0.0289(12) Uani 1 1 d . . . . .
N7 N 0.18289(13) 0.8099(4) 0.3223(2) 0.0270(12) Uani 1 1 d . . . . .
N8 N 0.12588(13) 0.7877(4) 0.4052(2) 0.0301(12) Uani 1 1 d . . . . .
N9 N 0.11929(14) 0.5594(4) 0.4040(3) 0.0333(13) Uani 1 1 d . . . . .
N10 N 0.15576(14) 0.5159(4) 0.2826(3) 0.0306(12) Uani 1 1 d . . . . .
N11 N 0.21157(13) 0.6495(4) 0.3282(2) 0.0296(12) Uani 1 1 d . . . . .
N12 N 0.17331(14) 0.6930(4) 0.4508(2) 0.0298(12) Uani 1 1 d . . . . .
O1 O 0.0348(3) 0.2369(8) 0.4207(5) 0.140(3) Uani 1 1 d D . . . .
Co1 Co 0.11105(3) 0.88584(7) 0.25673(5) 0.0387(2) Uani 1 1 d . . . . .
Co2 Co 0.13931(2) 0.73400(6) 0.31628(4) 0.02587(19) Uani 1 1 d . . . . .
Co3 Co 0.16743(2) 0.59401(7) 0.37068(4) 0.0274(2) Uani 1 1 d . . . . .
I1 I 0.07970(2) 1.05341(4) 0.18882(3) 0.06437(18) Uani 1 1 d . . . . .
I2 I 0.20277(2) 0.42061(4) 0.43891(3) 0.05095(15) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.351(8) . ?
C1 C2 1.370(11) . ?
C1 H1 0.9300 . ?
C2 C3 1.373(11) . ?
C2 H2 0.9300 . ?
C3 C4 1.372(10) . ?
C3 H3 0.9300 . ?
C4 C5 1.397(9) . ?
C4 H4 0.9300 . ?
C5 N1 1.361(9) . ?
C5 N5 1.372(8) . ?
C6 N5 1.358(8) . ?
C6 N9 1.362(8) . ?
C6 C7 1.413(9) . ?
C7 C8 1.380(11) . ?
C7 H7 0.9300 . ?
C8 C9 1.376(11) . ?
C8 H8 0.9300 . ?
C9 C10 1.357(10) . ?
C9 H9 0.9300 . ?
C10 N9 1.353(8) . ?
C10 H10 0.9300 . ?
C11 N2 1.353(8) . ?
C11 C12 1.367(10) . ?
C11 H11 0.9300 . ?
C12 C13 1.374(11) . ?
C12 H12 0.9300 . ?
C13 C14 1.361(9) . ?
C13 H13 0.9300 . ?
C14 C15 1.397(9) . ?
C14 H14 0.9300 . ?
C15 N6 1.370(8) . ?
C15 N2 1.375(8) . ?
C16 N6 1.365(8) . ?
C16 N10 1.366(7) . ?
C16 C17 1.412(8) . ?
C17 C18 1.363(10) . ?
C17 H17 0.9300 . ?
C18 C19 1.381(10) . ?
C18 H18 0.9300 . ?
C19 C20 1.367(9) . ?
C19 H19 0.9300 . ?
C20 N10 1.357(8) . ?
C20 H20 0.9300 . ?
C21 N3 1.365(8) . ?
C21 C22 1.373(10) . ?
C21 H21 0.9300 . ?
C22 C23 1.384(11) . ?
C22 H22 0.9300 . ?
C23 C24 1.368(10) . ?
C23 H23 0.9300 . ?
C24 C25 1.399(9) . ?
C24 H24 0.9300 . ?
C25 N3 1.358(8) . ?
C25 N7 1.377(8) . ?
C26 N7 1.359(8) . ?
C26 N11 1.369(8) . ?
C26 C27 1.404(9) . ?
C27 C28 1.370(9) . ?
C27 H27 0.9300 . ?
C28 C29 1.397(10) . ?
C28 H28 0.9300 . ?
C29 C30 1.350(9) . ?
C29 H29 0.9300 . ?
C30 N11 1.351(8) . ?
C30 H30 0.9300 . ?
C31 N4 1.349(9) . ?
C31 C32 1.362(10) . ?
C31 H31 0.9300 . ?
C32 C33 1.380(11) . ?
C32 H32 0.9300 . ?
C33 C34 1.359(11) . ?
C33 H33 0.9300 . ?
C34 C35 1.403(10) . ?
C34 H34 0.9300 . ?
C35 N4 1.366(8) . ?
C35 N8 1.379(8) . ?
C36 N12 1.355(8) . ?
C36 N8 1.376(7) . ?
C36 C37 1.402(8) . ?
C37 C38 1.361(9) . ?
C37 H37 0.9300 . ?
C38 C39 1.386(10) . ?
C38 H38 0.9300 . ?
C39 C40 1.363(9) . ?
C39 H39 0.9300 . ?
C40 N12 1.361(8) . ?
C40 H40 0.9300 . ?
C41 C42 1.463(17) . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 O1 1.442(14) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 O1 1.410(13) . ?
C43 C44 1.485(16) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
N1 Co1 2.176(6) . ?
N2 Co1 2.116(5) . ?
N3 Co1 2.150(6) . ?
N4 Co1 2.126(6) . ?
N5 Co2 1.897(5) . ?
N6 Co2 1.912(5) . ?
N7 Co2 1.901(5) . ?
N8 Co2 1.907(5) . ?
N9 Co3 1.981(5) . ?
N10 Co3 1.990(5) . ?
N11 Co3 1.994(5) . ?
N12 Co3 1.988(5) . ?
Co1 Co2 2.4679(14) . ?
Co1 I1 2.7453(13) . ?
Co2 Co3 2.3046(13) . ?
Co3 I2 2.8703(13) . ?

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
N1 C1 C2 124.2(8) . . ?
N1 C1 H1 117.9 . . ?
C2 C1 H1 117.9 . . ?
C1 C2 C3 118.0(7) . . ?
C1 C2 H2 121.0 . . ?
C3 C2 H2 121.0 . . ?
C2 C3 C4 119.8(7) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C3 C4 C5 120.0(7) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
N1 C5 N5 115.3(6) . . ?
N1 C5 C4 120.5(6) . . ?
N5 C5 C4 123.8(6) . . ?
N5 C6 N9 115.4(6) . . ?
N5 C6 C7 123.9(6) . . ?
N9 C6 C7 120.4(6) . . ?
C8 C7 C6 119.2(7) . . ?
C8 C7 H7 120.4 . . ?
C6 C7 H7 120.4 . . ?
C9 C8 C7 119.3(8) . . ?
C9 C8 H8 120.4 . . ?
C7 C8 H8 120.4 . . ?
C10 C9 C8 119.6(8) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
N9 C10 C9 123.1(7) . . ?
N9 C10 H10 118.4 . . ?
C9 C10 H10 118.4 . . ?
N2 C11 C12 123.3(7) . . ?
N2 C11 H11 118.3 . . ?
C12 C11 H11 118.3 . . ?
C11 C12 C13 119.0(7) . . ?
C11 C12 H12 120.5 . . ?
C13 C12 H12 120.5 . . ?
C14 C13 C12 119.5(7) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C13 C14 C15 120.4(7) . . ?
C13 C14 H14 119.8 . . ?
C15 C14 H14 119.8 . . ?
N6 C15 N2 115.4(5) . . ?
N6 C15 C14 124.0(6) . . ?
N2 C15 C14 120.2(6) . . ?
N6 C16 N10 115.0(5) . . ?
N6 C16 C17 124.4(6) . . ?
N10 C16 C17 120.3(6) . . ?
C18 C17 C16 119.6(6) . . ?
C18 C17 H17 120.2 . . ?
C16 C17 H17 120.2 . . ?
C17 C18 C19 119.8(7) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 H18 120.1 . . ?
C20 C19 C18 119.0(7) . . ?
C20 C19 H19 120.5 . . ?
C18 C19 H19 120.5 . . ?
N10 C20 C19 123.0(7) . . ?
N10 C20 H20 118.5 . . ?
C19 C20 H20 118.5 . . ?
N3 C21 C22 122.0(7) . . ?
N3 C21 H21 119.0 . . ?
C22 C21 H21 119.0 . . ?
C21 C22 C23 120.0(7) . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C24 C23 C22 118.4(7) . . ?
C24 C23 H23 120.8 . . ?
C22 C23 H23 120.8 . . ?
C23 C24 C25 120.5(7) . . ?
C23 C24 H24 119.7 . . ?
C25 C24 H24 119.7 . . ?
N3 C25 N7 114.4(6) . . ?
N3 C25 C24 120.8(6) . . ?
N7 C25 C24 124.3(6) . . ?
N7 C26 N11 115.9(5) . . ?
N7 C26 C27 123.6(6) . . ?
N11 C26 C27 120.0(6) . . ?
C28 C27 C26 120.6(7) . . ?
C28 C27 H27 119.7 . . ?
C26 C27 H27 119.7 . . ?
C27 C28 C29 118.4(7) . . ?
C27 C28 H28 120.8 . . ?
C29 C28 H28 120.8 . . ?
C30 C29 C28 119.1(7) . . ?
C30 C29 H29 120.4 . . ?
C28 C29 H29 120.4 . . ?
C29 C30 N11 123.9(7) . . ?
C29 C30 H30 118.0 . . ?
N11 C30 H30 118.0 . . ?
N4 C31 C32 124.3(7) . . ?
N4 C31 H31 117.8 . . ?
C32 C31 H31 117.8 . . ?
C31 C32 C33 117.4(8) . . ?
C31 C32 H32 121.3 . . ?
C33 C32 H32 121.3 . . ?
C34 C33 C32 120.8(8) . . ?
C34 C33 H33 119.6 . . ?
C32 C33 H33 119.6 . . ?
C33 C34 C35 119.4(8) . . ?
C33 C34 H34 120.3 . . ?
C35 C34 H34 120.3 . . ?
N4 C35 N8 114.9(6) . . ?
N4 C35 C34 120.3(7) . . ?
N8 C35 C34 124.5(6) . . ?
N12 C36 N8 114.8(5) . . ?
N12 C36 C37 120.4(6) . . ?
N8 C36 C37 124.6(6) . . ?
C38 C37 C36 120.0(7) . . ?
C38 C37 H37 120.0 . . ?
C36 C37 H37 120.0 . . ?
C37 C38 C39 119.4(6) . . ?
C37 C38 H38 120.3 . . ?
C39 C38 H38 120.3 . . ?
C40 C39 C38 118.8(7) . . ?
C40 C39 H39 120.6 . . ?
C38 C39 H39 120.6 . . ?
N12 C40 C39 122.8(7) . . ?
N12 C40 H40 118.6 . . ?
C39 C40 H40 118.6 . . ?
C42 C41 H41A 109.5 . . ?
C42 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C42 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C41 C42 O1 109.2(15) . . ?
C41 C42 H42A 109.8 . . ?
O1 C42 H42A 109.8 . . ?
C41 C42 H42B 109.8 . . ?
O1 C42 H42B 109.8 . . ?
H42A C42 H42B 108.3 . . ?
O1 C43 C44 108.8(13) . . ?
O1 C43 H43A 109.9 . . ?
C44 C43 H43A 109.9 . . ?
O1 C43 H43B 109.9 . . ?
C44 C43 H43B 109.9 . . ?
H43A C43 H43B 108.3 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C1 N1 C5 117.6(6) . . ?
C1 N1 Co1 120.1(5) . . ?
C5 N1 Co1 122.2(4) . . ?
C11 N2 C15 117.7(6) . . ?
C11 N2 Co1 120.1(5) . . ?
C15 N2 Co1 122.2(4) . . ?
C25 N3 C21 118.2(6) . . ?
C25 N3 Co1 121.1(4) . . ?
C21 N3 Co1 120.6(5) . . ?
C31 N4 C35 117.8(6) . . ?
C31 N4 Co1 120.0(5) . . ?
C35 N4 Co1 122.2(5) . . ?
C6 N5 C5 124.6(6) . . ?
C6 N5 Co2 116.7(4) . . ?
C5 N5 Co2 118.6(4) . . ?
C16 N6 C15 124.0(5) . . ?
C16 N6 Co2 117.4(4) . . ?
C15 N6 Co2 118.6(4) . . ?
C26 N7 C25 123.2(5) . . ?
C26 N7 Co2 116.4(4) . . ?
C25 N7 Co2 120.4(4) . . ?
C36 N8 C35 124.6(5) . . ?
C36 N8 Co2 116.6(4) . . ?
C35 N8 Co2 118.8(4) . . ?
C10 N9 C6 118.3(6) . . ?
C10 N9 Co3 121.9(5) . . ?
C6 N9 Co3 119.8(4) . . ?
C20 N10 C16 118.1(5) . . ?
C20 N10 Co3 122.8(4) . . ?
C16 N10 Co3 118.9(4) . . ?
C30 N11 C26 117.9(5) . . ?
C30 N11 Co3 123.3(4) . . ?
C26 N11 Co3 118.6(4) . . ?
C36 N12 C40 118.2(5) . . ?
C36 N12 Co3 120.9(4) . . ?
C40 N12 Co3 120.9(4) . . ?
C43 O1 C42 111.0(12) . . ?
N2 Co1 N4 161.0(2) . . ?
N2 Co1 N3 89.5(2) . . ?
N4 Co1 N3 88.9(2) . . ?
N2 Co1 N1 88.7(2) . . ?
N4 Co1 N1 86.5(2) . . ?
N3 Co1 N1 160.3(2) . . ?
N2 Co1 Co2 80.57(14) . . ?
N4 Co1 Co2 80.48(16) . . ?
N3 Co1 Co2 80.97(15) . . ?
N1 Co1 Co2 79.35(15) . . ?
N2 Co1 I1 98.82(14) . . ?
N4 Co1 I1 100.11(16) . . ?
N3 Co1 I1 99.50(15) . . ?
N1 Co1 I1 100.20(15) . . ?
Co2 Co1 I1 179.25(5) . . ?
N5 Co2 N7 178.8(2) . . ?
N5 Co2 N8 89.3(2) . . ?
N7 Co2 N8 90.7(2) . . ?
N5 Co2 N6 89.9(2) . . ?
N7 Co2 N6 90.1(2) . . ?
N8 Co2 N6 178.7(2) . . ?
N5 Co2 Co3 89.65(16) . . ?
N7 Co2 Co3 89.12(15) . . ?
N8 Co2 Co3 90.42(16) . . ?
N6 Co2 Co3 88.49(15) . . ?
N5 Co2 Co1 92.02(16) . . ?
N7 Co2 Co1 89.22(15) . . ?
N8 Co2 Co1 90.36(16) . . ?
N6 Co2 Co1 90.76(15) . . ?
Co3 Co2 Co1 178.17(5) . . ?
N9 Co3 N12 88.7(2) . . ?
N9 Co3 N10 88.7(2) . . ?
N12 Co3 N10 169.2(2) . . ?
N9 Co3 N11 169.9(2) . . ?
N12 Co3 N11 90.6(2) . . ?
N10 Co3 N11 90.0(2) . . ?
N9 Co3 Co2 84.62(16) . . ?
N12 Co3 Co2 83.89(15) . . ?
N10 Co3 Co2 85.45(15) . . ?
N11 Co3 Co2 85.29(15) . . ?
N9 Co3 I2 95.59(16) . . ?
N12 Co3 I2 95.79(15) . . ?
N10 Co3 I2 94.87(15) . . ?
N11 Co3 I2 94.50(15) . . ?
Co2 Co3 I2 179.61(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
N1 C1 C2 C3 0.3(12) . . . . ?
C1 C2 C3 C4 0.6(12) . . . . ?
C2 C3 C4 C5 -0.5(12) . . . . ?
C3 C4 C5 N1 -0.5(11) . . . . ?
C3 C4 C5 N5 -172.7(7) . . . . ?
N5 C6 C7 C8 -169.7(8) . . . . ?
N9 C6 C7 C8 3.7(12) . . . . ?
C6 C7 C8 C9 -1.6(14) . . . . ?
C7 C8 C9 C10 0.4(14) . . . . ?
C8 C9 C10 N9 -1.1(13) . . . . ?
N2 C11 C12 C13 0.7(13) . . . . ?
C11 C12 C13 C14 -1.1(13) . . . . ?
C12 C13 C14 C15 0.5(12) . . . . ?
C13 C14 C15 N6 -172.1(7) . . . . ?
C13 C14 C15 N2 0.6(10) . . . . ?
N6 C16 C17 C18 -168.3(7) . . . . ?
N10 C16 C17 C18 5.0(11) . . . . ?
C16 C17 C18 C19 0.1(12) . . . . ?
C17 C18 C19 C20 -2.8(13) . . . . ?
C18 C19 C20 N10 0.6(12) . . . . ?
N3 C21 C22 C23 -0.1(11) . . . . ?
C21 C22 C23 C24 -1.1(11) . . . . ?
C22 C23 C24 C25 1.5(10) . . . . ?
C23 C24 C25 N3 -0.7(10) . . . . ?
C23 C24 C25 N7 -172.7(6) . . . . ?
N7 C26 C27 C28 -170.3(6) . . . . ?
N11 C26 C27 C28 1.5(9) . . . . ?
C26 C27 C28 C29 -1.0(10) . . . . ?
C27 C28 C29 C30 0.4(10) . . . . ?
C28 C29 C30 N11 -0.4(10) . . . . ?
N4 C31 C32 C33 -1.2(13) . . . . ?
C31 C32 C33 C34 -0.3(13) . . . . ?
C32 C33 C34 C35 0.9(13) . . . . ?
C33 C34 C35 N4 0.0(11) . . . . ?
C33 C34 C35 N8 -173.1(7) . . . . ?
N12 C36 C37 C38 2.2(10) . . . . ?
N8 C36 C37 C38 -171.7(7) . . . . ?
C36 C37 C38 C39 3.5(11) . . . . ?
C37 C38 C39 C40 -4.8(12) . . . . ?
C38 C39 C40 N12 0.5(12) . . . . ?
C2 C1 N1 C5 -1.2(11) . . . . ?
C2 C1 N1 Co1 175.3(6) . . . . ?
N5 C5 N1 C1 174.1(6) . . . . ?
C4 C5 N1 C1 1.2(10) . . . . ?
N5 C5 N1 Co1 -2.3(8) . . . . ?
C4 C5 N1 Co1 -175.2(5) . . . . ?
C12 C11 N2 C15 0.4(11) . . . . ?
C12 C11 N2 Co1 177.6(6) . . . . ?
N6 C15 N2 C11 172.3(6) . . . . ?
C14 C15 N2 C11 -1.0(9) . . . . ?
N6 C15 N2 Co1 -4.8(7) . . . . ?
C14 C15 N2 Co1 -178.1(5) . . . . ?
N7 C25 N3 C21 172.2(5) . . . . ?
C24 C25 N3 C21 -0.5(9) . . . . ?
N7 C25 N3 Co1 -4.4(7) . . . . ?
C24 C25 N3 Co1 -177.1(5) . . . . ?
C22 C21 N3 C25 0.9(9) . . . . ?
C22 C21 N3 Co1 177.6(5) . . . . ?
C32 C31 N4 C35 2.1(11) . . . . ?
C32 C31 N4 Co1 179.1(6) . . . . ?
N8 C35 N4 C31 172.3(6) . . . . ?
C34 C35 N4 C31 -1.4(10) . . . . ?
N8 C35 N4 Co1 -4.6(8) . . . . ?
C34 C35 N4 Co1 -178.3(5) . . . . ?
N9 C6 N5 C5 154.5(6) . . . . ?
C7 C6 N5 C5 -31.8(10) . . . . ?
N9 C6 N5 Co2 -23.6(7) . . . . ?
C7 C6 N5 Co2 150.1(6) . . . . ?
N1 C5 N5 C6 154.5(6) . . . . ?
C4 C5 N5 C6 -32.9(10) . . . . ?
N1 C5 N5 Co2 -27.4(8) . . . . ?
C4 C5 N5 Co2 145.3(6) . . . . ?
N10 C16 N6 C15 155.3(6) . . . . ?
C17 C16 N6 C15 -31.1(10) . . . . ?
N10 C16 N6 Co2 -24.2(7) . . . . ?
C17 C16 N6 Co2 149.4(5) . . . . ?
N2 C15 N6 C16 155.0(6) . . . . ?
C14 C15 N6 C16 -32.0(10) . . . . ?
N2 C15 N6 Co2 -25.5(7) . . . . ?
C14 C15 N6 Co2 147.5(5) . . . . ?
N11 C26 N7 C25 153.2(5) . . . . ?
C27 C26 N7 C25 -34.7(8) . . . . ?
N11 C26 N7 Co2 -27.2(6) . . . . ?
C27 C26 N7 Co2 145.0(5) . . . . ?
N3 C25 N7 C26 151.8(5) . . . . ?
C24 C25 N7 C26 -35.8(9) . . . . ?
N3 C25 N7 Co2 -27.9(7) . . . . ?
C24 C25 N7 Co2 144.6(5) . . . . ?
N12 C36 N8 C35 159.0(6) . . . . ?
C37 C36 N8 C35 -26.8(10) . . . . ?
N12 C36 N8 Co2 -19.1(7) . . . . ?
C37 C36 N8 Co2 155.1(5) . . . . ?
N4 C35 N8 C36 155.3(6) . . . . ?
C34 C35 N8 C36 -31.3(10) . . . . ?
N4 C35 N8 Co2 -26.6(7) . . . . ?
C34 C35 N8 Co2 146.8(6) . . . . ?
C9 C10 N9 C6 3.2(11) . . . . ?
C9 C10 N9 Co3 -179.9(6) . . . . ?
N5 C6 N9 C10 169.6(6) . . . . ?
C7 C6 N9 C10 -4.4(10) . . . . ?
N5 C6 N9 Co3 -7.4(7) . . . . ?
C7 C6 N9 Co3 178.6(5) . . . . ?
C19 C20 N10 C16 4.3(11) . . . . ?
C19 C20 N10 Co3 178.8(6) . . . . ?
N6 C16 N10 C20 166.9(6) . . . . ?
C17 C16 N10 C20 -7.0(9) . . . . ?
N6 C16 N10 Co3 -7.8(7) . . . . ?
C17 C16 N10 Co3 178.3(5) . . . . ?
C29 C30 N11 C26 0.9(9) . . . . ?
C29 C30 N11 Co3 175.8(5) . . . . ?
N7 C26 N11 C30 171.0(5) . . . . ?
C27 C26 N11 C30 -1.5(8) . . . . ?
N7 C26 N11 Co3 -4.1(7) . . . . ?
C27 C26 N11 Co3 -176.5(4) . . . . ?
N8 C36 N12 C40 168.1(6) . . . . ?
C37 C36 N12 C40 -6.4(9) . . . . ?
N8 C36 N12 Co3 -12.1(7) . . . . ?
C37 C36 N12 Co3 173.5(5) . . . . ?
C39 C40 N12 C36 5.1(10) . . . . ?
C39 C40 N12 Co3 -174.7(6) . . . . ?
C44 C43 O1 C42 -173.6(14) . . . . ?
C41 C42 O1 C43 -178.0(15) . . . . ?
C6 N5 Co2 N8 -54.7(5) . . . . ?
C5 N5 Co2 N8 127.0(5) . . . . ?
C6 N5 Co2 N6 124.2(5) . . . . ?
C5 N5 Co2 N6 -54.1(5) . . . . ?
C6 N5 Co2 Co3 35.7(5) . . . . ?
C5 N5 Co2 Co3 -142.5(5) . . . . ?
C6 N5 Co2 Co1 -145.0(4) . . . . ?
C5 N5 Co2 Co1 36.7(5) . . . . ?

_refine_diff_density_max         1.249
_refine_diff_density_min         -0.737
_refine_diff_density_rms         0.119


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile, ether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_4-Et2O-170K
_database_code_depnum_ccdc_archive 'CCDC 1865590'
_audit_update_record             
;
2018-09-03 deposited with the CCDC.
2018-11-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C40 H32 Co3 I2 N12, C4 H10 O'
_chemical_formula_sum            'C44 H42 Co3 I2 N12 O'
_chemical_formula_weight         1185.48

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

_cell_length_a                   37.280(4)
_cell_length_b                   12.6433(11)
_cell_length_c                   18.8935(19)
_cell_angle_alpha                90
_cell_angle_beta                 91.748(5)
_cell_angle_gamma                90
_cell_volume                     8901.2(15)
_cell_formula_units_Z            8
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    7641
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      24.41

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.769
_exptl_crystal_F_000             4680
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    2.543
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6740
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   'SADABS (Bruker, 2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            75167
_diffrn_reflns_av_unetI/netI     0.0575
_diffrn_reflns_av_R_equivalents  0.0868
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.005
_diffrn_reflns_theta_max         25.378
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8155
_reflns_number_gt                5776
_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       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_structure_solution    'SHELXS2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_publication_material  'SHELXL-2016/4 (Sheldrick, 2016)'
_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)+(0.0252P)²+29.7514P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8155
_refine_ls_number_parameters     561
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0371
_refine_ls_wR_factor_ref         0.0770
_refine_ls_wR_factor_gt          0.0675
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_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
C1 C 0.05745(12) 0.7714(4) 0.1574(2) 0.0261(12) Uani 1 1 d . . . . .
H1 H 0.058654 0.837984 0.134255 0.031 Uiso 1 1 calc R U . . .
C2 C 0.03736(13) 0.6932(4) 0.1260(3) 0.0318(13) Uani 1 1 d . . . . .
H2 H 0.024525 0.705621 0.082546 0.038 Uiso 1 1 calc R U . . .
C3 C 0.03615(12) 0.5959(4) 0.1587(3) 0.0302(12) Uani 1 1 d . . . . .
H3 H 0.023086 0.539405 0.136977 0.036 Uiso 1 1 calc R U . . .
C4 C 0.05384(12) 0.5807(4) 0.2226(2) 0.0241(11) Uani 1 1 d . . . . .
H4 H 0.052466 0.514370 0.245946 0.029 Uiso 1 1 calc R U . . .
C5 C 0.07391(12) 0.6631(3) 0.2534(2) 0.0181(10) Uani 1 1 d . . . . .
C6 C 0.08989(12) 0.5848(3) 0.3667(2) 0.0168(10) Uani 1 1 d . . . . .
C7 C 0.05562(13) 0.5542(4) 0.3882(3) 0.0274(12) Uani 1 1 d . . . . .
H7 H 0.034871 0.573291 0.360662 0.033 Uiso 1 1 calc R U . . .
C8 C 0.05236(14) 0.4965(4) 0.4493(3) 0.0335(13) Uani 1 1 d . . . . .
H8 H 0.029331 0.475105 0.464073 0.040 Uiso 1 1 calc R U . . .
C9 C 0.08261(14) 0.4699(4) 0.4892(3) 0.0326(13) Uani 1 1 d . . . . .
H9 H 0.080763 0.431024 0.531959 0.039 Uiso 1 1 calc R U . . .
C10 C 0.11528(13) 0.5006(4) 0.4658(2) 0.0243(11) Uani 1 1 d . . . . .
H10 H 0.136018 0.483160 0.493849 0.029 Uiso 1 1 calc R U . . .
C11 C 0.15832(13) 0.9191(4) 0.1353(2) 0.0265(12) Uani 1 1 d . . . . .
H11 H 0.148868 0.988627 0.139117 0.032 Uiso 1 1 calc R U . . .
C12 C 0.18286(15) 0.9007(4) 0.0842(3) 0.0331(13) Uani 1 1 d . . . . .
H12 H 0.190044 0.955875 0.053593 0.040 Uiso 1 1 calc R U . . .
C13 C 0.19691(14) 0.8002(4) 0.0783(3) 0.0300(12) Uani 1 1 d . . . . .
H13 H 0.213946 0.784880 0.043368 0.036 Uiso 1 1 calc R U . . .
C14 C 0.18593(13) 0.7226(3) 0.1237(2) 0.0237(11) Uani 1 1 d . . . . .
H14 H 0.195235 0.652936 0.119962 0.028 Uiso 1 1 calc R U . . .
C15 C 0.16093(11) 0.7463(3) 0.1755(2) 0.0155(10) Uani 1 1 d . . . . .
C16 C 0.15179(11) 0.5701(3) 0.2209(2) 0.0141(9) Uani 1 1 d . . . . .
C17 C 0.14369(12) 0.5160(4) 0.1570(2) 0.0227(11) Uani 1 1 d . . . . .
H17 H 0.142234 0.554010 0.113614 0.027 Uiso 1 1 calc R U . . .
C18 C 0.13796(13) 0.4098(4) 0.1572(3) 0.0284(12) Uani 1 1 d . . . . .
H18 H 0.132639 0.373705 0.114073 0.034 Uiso 1 1 calc R U . . .
C19 C 0.13987(13) 0.3545(3) 0.2202(3) 0.0258(12) Uani 1 1 d . . . . .
H19 H 0.135279 0.280599 0.221300 0.031 Uiso 1 1 calc R U . . .
C20 C 0.14863(12) 0.4091(3) 0.2817(2) 0.0213(11) Uani 1 1 d . . . . .
H20 H 0.149661 0.371347 0.325153 0.026 Uiso 1 1 calc R U . . .
C21 C 0.14742(14) 1.0705(4) 0.3358(2) 0.0263(12) Uani 1 1 d . . . . .
H21 H 0.125862 1.105828 0.321784 0.032 Uiso 1 1 calc R U . . .
C22 C 0.17233(14) 1.1257(4) 0.3743(2) 0.0286(12) Uani 1 1 d . . . . .
H22 H 0.168401 1.197576 0.386534 0.034 Uiso 1 1 calc R U . . .
C23 C 0.20385(14) 1.0739(4) 0.3954(2) 0.0280(12) Uani 1 1 d . . . . .
H23 H 0.221970 1.110297 0.422161 0.034 Uiso 1 1 calc R U . . .
C24 C 0.20850(12) 0.9698(3) 0.3772(2) 0.0203(11) Uani 1 1 d . . . . .
H24 H 0.229854 0.933559 0.391384 0.024 Uiso 1 1 calc R U . . .
C25 C 0.18159(12) 0.9172(3) 0.3375(2) 0.0168(10) Uani 1 1 d . . . . .
C26 C 0.21280(11) 0.7558(3) 0.3115(2) 0.0139(10) Uani 1 1 d . . . . .
C27 C 0.24238(12) 0.7975(3) 0.2765(2) 0.0184(10) Uani 1 1 d . . . . .
H27 H 0.243228 0.871062 0.266422 0.022 Uiso 1 1 calc R U . . .
C28 C 0.27000(12) 0.7335(4) 0.2569(2) 0.0220(11) Uani 1 1 d . . . . .
H28 H 0.289636 0.761365 0.232011 0.026 Uiso 1 1 calc R U . . .
C29 C 0.26859(12) 0.6267(4) 0.2743(2) 0.0209(11) Uani 1 1 d . . . . .
H29 H 0.287627 0.580598 0.262557 0.025 Uiso 1 1 calc R U . . .
C30 C 0.23938(11) 0.5890(3) 0.3086(2) 0.0163(10) Uani 1 1 d . . . . .
H30 H 0.238572 0.515579 0.319236 0.020 Uiso 1 1 calc R U . . .
C31 C 0.04581(12) 0.9213(4) 0.3506(3) 0.0273(12) Uani 1 1 d . . . . .
H31 H 0.036604 0.951304 0.307640 0.033 Uiso 1 1 calc R U . . .
C32 C 0.02427(13) 0.9213(4) 0.4072(3) 0.0292(12) Uani 1 1 d . . . . .
H32 H 0.001201 0.953188 0.404497 0.035 Uiso 1 1 calc R U . . .
C33 C 0.03704(13) 0.8728(4) 0.4698(3) 0.0313(13) Uani 1 1 d . . . . .
H33 H 0.022354 0.868842 0.509939 0.038 Uiso 1 1 calc R U . . .
C34 C 0.07081(12) 0.8314(4) 0.4723(2) 0.0247(11) Uani 1 1 d . . . . .
H34 H 0.079937 0.800077 0.514856 0.030 Uiso 1 1 calc R U . . .
C35 C 0.09230(12) 0.8346(3) 0.4123(2) 0.0169(10) Uani 1 1 d . . . . .
C36 C 0.14868(11) 0.7693(3) 0.4623(2) 0.0154(10) Uani 1 1 d . . . . .
C37 C 0.15094(12) 0.8311(3) 0.5249(2) 0.0201(11) Uani 1 1 d . . . . .
H37 H 0.133001 0.882353 0.533941 0.024 Uiso 1 1 calc R U . . .
C38 C 0.17906(13) 0.8168(4) 0.5722(2) 0.0255(12) Uani 1 1 d . . . . .
H38 H 0.180421 0.857305 0.614551 0.031 Uiso 1 1 calc R U . . .
C39 C 0.20547(12) 0.7435(4) 0.5585(2) 0.0242(11) Uani 1 1 d . . . . .
H39 H 0.225684 0.735080 0.589848 0.029 Uiso 1 1 calc R U . . .
C40 C 0.20167(12) 0.6834(3) 0.4985(2) 0.0191(10) Uani 1 1 d . . . . .
H40 H 0.219906 0.633393 0.488858 0.023 Uiso 1 1 calc R U . . .
C41 C -0.0226(2) 0.3025(5) 0.3686(4) 0.077(2) Uani 1 1 d . . . . .
H41A H -0.037153 0.239648 0.377716 0.115 Uiso 1 1 calc R U . . .
H41B H -0.032993 0.340959 0.327857 0.115 Uiso 1 1 calc R U . . .
H41C H -0.022295 0.348508 0.410378 0.115 Uiso 1 1 calc R U . . .
C42 C 0.0139(2) 0.2704(6) 0.3536(4) 0.073(2) Uani 1 1 d . . . . .
H42A H 0.013436 0.212783 0.318088 0.087 Uiso 1 1 calc R U . . .
H42B H 0.027193 0.330946 0.333865 0.087 Uiso 1 1 calc R U . . .
C43 C 0.0668(2) 0.1997(5) 0.4083(4) 0.064(2) Uani 1 1 d . . . . .
H43A H 0.081490 0.259156 0.391229 0.077 Uiso 1 1 calc R U . . .
H43B H 0.066647 0.143331 0.371939 0.077 Uiso 1 1 calc R U . . .
C44 C 0.0829(2) 0.1579(6) 0.4767(4) 0.075(2) Uani 1 1 d . . . . .
H44A H 0.084457 0.215122 0.511675 0.113 Uiso 1 1 calc R U . . .
H44B H 0.106942 0.130168 0.468576 0.113 Uiso 1 1 calc R U . . .
H44C H 0.067691 0.101104 0.494555 0.113 Uiso 1 1 calc R U . . .
N1 N 0.07584(10) 0.7590(3) 0.22023(19) 0.0198(9) Uani 1 1 d . . . . .
N2 N 0.14674(9) 0.8453(3) 0.18041(18) 0.0165(8) Uani 1 1 d . . . . .
N3 N 0.15123(10) 0.9682(3) 0.31590(19) 0.0189(9) Uani 1 1 d . . . . .
N4 N 0.07967(10) 0.8812(3) 0.35105(19) 0.0194(9) Uani 1 1 d . . . . .
N5 N 0.09568(9) 0.6530(3) 0.31247(18) 0.0158(8) Uani 1 1 d . . . . .
N6 N 0.15184(9) 0.6775(3) 0.22803(18) 0.0135(8) Uani 1 1 d . . . . .
N7 N 0.18207(9) 0.8104(3) 0.32363(18) 0.0138(8) Uani 1 1 d . . . . .
N8 N 0.12516(9) 0.7857(3) 0.40729(18) 0.0137(8) Uani 1 1 d . . . . .
N9 N 0.11978(9) 0.5543(3) 0.40495(19) 0.0167(8) Uani 1 1 d . . . . .
N10 N 0.15584(9) 0.5146(3) 0.28263(18) 0.0138(8) Uani 1 1 d . . . . .
N11 N 0.21163(9) 0.6502(3) 0.32814(18) 0.0145(8) Uani 1 1 d . . . . .
N12 N 0.17374(9) 0.6911(3) 0.45263(17) 0.0131(8) Uani 1 1 d . . . . .
O1 O 0.03175(13) 0.2344(3) 0.4184(2) 0.0582(12) Uani 1 1 d . . . . .
CO1 Co 0.11013(2) 0.88527(5) 0.25882(3) 0.02112(15) Uani 1 1 d . . . . .
CO2 Co 0.13854(2) 0.73265(4) 0.31754(3) 0.01293(14) Uani 1 1 d . . . . .
CO3 Co 0.16775(2) 0.59300(4) 0.37104(3) 0.01299(14) Uani 1 1 d . . . . .
I1 I 0.07765(2) 1.05411(3) 0.19075(2) 0.03480(11) Uani 1 1 d . . . . .
I2 I 0.20466(2) 0.41998(2) 0.43837(2) 0.02719(9) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.362(6) . ?
C1 C2 1.365(7) . ?
C1 H1 0.9500 . ?
C2 C3 1.379(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.372(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.399(6) . ?
C4 H4 0.9500 . ?
C5 N5 1.366(5) . ?
C5 N1 1.368(5) . ?
C6 N5 1.361(5) . ?
C6 N9 1.365(6) . ?
C6 C7 1.407(6) . ?
C7 C8 1.374(7) . ?
C7 H7 0.9500 . ?
C8 C9 1.379(7) . ?
C8 H8 0.9500 . ?
C9 C10 1.365(6) . ?
C9 H9 0.9500 . ?
C10 N9 1.350(6) . ?
C10 H10 0.9500 . ?
C11 N2 1.344(5) . ?
C11 C12 1.370(7) . ?
C11 H11 0.9500 . ?
C12 C13 1.381(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.373(6) . ?
C13 H13 0.9500 . ?
C14 C15 1.405(6) . ?
C14 H14 0.9500 . ?
C15 N2 1.363(5) . ?
C15 N6 1.369(5) . ?
C16 N6 1.365(5) . ?
C16 N10 1.366(5) . ?
C16 C17 1.412(6) . ?
C17 C18 1.360(6) . ?
C17 H17 0.9500 . ?
C18 C19 1.381(7) . ?
C18 H18 0.9500 . ?
C19 C20 1.381(6) . ?
C19 H19 0.9500 . ?
C20 N10 1.361(5) . ?
C20 H20 0.9500 . ?
C21 N3 1.356(5) . ?
C21 C22 1.356(7) . ?
C21 H21 0.9500 . ?
C22 C23 1.393(7) . ?
C22 H22 0.9500 . ?
C23 C24 1.373(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.402(6) . ?
C24 H24 0.9500 . ?
C25 N3 1.355(5) . ?
C25 N7 1.375(5) . ?
C26 N7 1.363(5) . ?
C26 N11 1.373(5) . ?
C26 C27 1.405(6) . ?
C27 C28 1.370(6) . ?
C27 H27 0.9500 . ?
C28 C29 1.391(6) . ?
C28 H28 0.9500 . ?
C29 C30 1.370(6) . ?
C29 H29 0.9500 . ?
C30 N11 1.352(5) . ?
C30 H30 0.9500 . ?
C31 C32 1.357(7) . ?
C31 N4 1.360(6) . ?
C31 H31 0.9500 . ?
C32 C33 1.403(7) . ?
C32 H32 0.9500 . ?
C33 C34 1.363(6) . ?
C33 H33 0.9500 . ?
C34 C35 1.408(6) . ?
C34 H34 0.9500 . ?
C35 N4 1.369(5) . ?
C35 N8 1.378(5) . ?
C36 N8 1.356(5) . ?
C36 N12 1.376(5) . ?
C36 C37 1.417(6) . ?
C37 C38 1.369(6) . ?
C37 H37 0.9500 . ?
C38 C39 1.383(6) . ?
C38 H38 0.9500 . ?
C39 C40 1.369(6) . ?
C39 H39 0.9500 . ?
C40 N12 1.338(5) . ?
C40 H40 0.9500 . ?
C41 C42 1.458(10) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 O1 1.450(8) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 O1 1.396(7) . ?
C43 C44 1.505(9) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
N1 CO1 2.158(4) . ?
N2 CO1 2.106(4) . ?
N3 CO1 2.123(4) . ?
N4 CO1 2.109(4) . ?
N5 CO2 1.889(3) . ?
N6 CO2 1.909(3) . ?
N7 CO2 1.898(3) . ?
N8 CO2 1.904(3) . ?
N9 CO3 1.979(4) . ?
N10 CO3 1.981(3) . ?
N11 CO3 1.984(3) . ?
N12 CO3 1.986(3) . ?
CO1 CO2 2.4504(8) . ?
CO1 I1 2.7535(7) . ?
CO2 CO3 2.2928(8) . ?
CO3 I2 2.8620(7) . ?

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
N1 C1 C2 123.4(5) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C1 C2 C3 118.5(5) . . ?
C1 C2 H2 120.8 . . ?
C3 C2 H2 120.8 . . ?
C4 C3 C2 119.8(5) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C3 C4 C5 119.9(5) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
N5 C5 N1 114.8(4) . . ?
N5 C5 C4 124.5(4) . . ?
N1 C5 C4 120.3(4) . . ?
N5 C6 N9 115.6(4) . . ?
N5 C6 C7 123.9(4) . . ?
N9 C6 C7 120.2(4) . . ?
C8 C7 C6 119.5(5) . . ?
C8 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
C7 C8 C9 119.8(4) . . ?
C7 C8 H8 120.1 . . ?
C9 C8 H8 120.1 . . ?
C10 C9 C8 118.5(5) . . ?
C10 C9 H9 120.8 . . ?
C8 C9 H9 120.8 . . ?
N9 C10 C9 123.7(5) . . ?
N9 C10 H10 118.2 . . ?
C9 C10 H10 118.2 . . ?
N2 C11 C12 124.3(4) . . ?
N2 C11 H11 117.9 . . ?
C12 C11 H11 117.9 . . ?
C11 C12 C13 118.5(4) . . ?
C11 C12 H12 120.8 . . ?
C13 C12 H12 120.8 . . ?
C14 C13 C12 119.1(4) . . ?
C14 C13 H13 120.5 . . ?
C12 C13 H13 120.5 . . ?
C13 C14 C15 120.0(4) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
N2 C15 N6 115.4(4) . . ?
N2 C15 C14 120.7(4) . . ?
N6 C15 C14 123.6(4) . . ?
N6 C16 N10 115.2(4) . . ?
N6 C16 C17 124.5(4) . . ?
N10 C16 C17 119.8(4) . . ?
C18 C17 C16 120.3(4) . . ?
C18 C17 H17 119.8 . . ?
C16 C17 H17 119.8 . . ?
C17 C18 C19 119.9(4) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?
C18 C19 C20 118.4(4) . . ?
C18 C19 H19 120.8 . . ?
C20 C19 H19 120.8 . . ?
N10 C20 C19 122.9(4) . . ?
N10 C20 H20 118.6 . . ?
C19 C20 H20 118.6 . . ?
N3 C21 C22 124.4(5) . . ?
N3 C21 H21 117.8 . . ?
C22 C21 H21 117.8 . . ?
C21 C22 C23 118.0(4) . . ?
C21 C22 H22 121.0 . . ?
C23 C22 H22 121.0 . . ?
C24 C23 C22 119.4(5) . . ?
C24 C23 H23 120.3 . . ?
C22 C23 H23 120.3 . . ?
C23 C24 C25 119.7(4) . . ?
C23 C24 H24 120.2 . . ?
C25 C24 H24 120.2 . . ?
N3 C25 N7 115.2(4) . . ?
N3 C25 C24 120.9(4) . . ?
N7 C25 C24 123.7(4) . . ?
N7 C26 N11 114.9(4) . . ?
N7 C26 C27 124.4(4) . . ?
N11 C26 C27 120.3(4) . . ?
C28 C27 C26 120.8(4) . . ?
C28 C27 H27 119.6 . . ?
C26 C27 H27 119.6 . . ?
C27 C28 C29 118.4(4) . . ?
C27 C28 H28 120.8 . . ?
C29 C28 H28 120.8 . . ?
C30 C29 C28 119.1(4) . . ?
C30 C29 H29 120.5 . . ?
C28 C29 H29 120.5 . . ?
N11 C30 C29 123.7(4) . . ?
N11 C30 H30 118.1 . . ?
C29 C30 H30 118.1 . . ?
C32 C31 N4 124.5(5) . . ?
C32 C31 H31 117.8 . . ?
N4 C31 H31 117.8 . . ?
C31 C32 C33 118.1(4) . . ?
C31 C32 H32 120.9 . . ?
C33 C32 H32 120.9 . . ?
C34 C33 C32 119.1(5) . . ?
C34 C33 H33 120.5 . . ?
C32 C33 H33 120.5 . . ?
C33 C34 C35 120.6(5) . . ?
C33 C34 H34 119.7 . . ?
C35 C34 H34 119.7 . . ?
N4 C35 N8 114.7(4) . . ?
N4 C35 C34 120.2(4) . . ?
N8 C35 C34 124.8(4) . . ?
N8 C36 N12 115.7(4) . . ?
N8 C36 C37 125.2(4) . . ?
N12 C36 C37 119.0(4) . . ?
C38 C37 C36 119.8(4) . . ?
C38 C37 H37 120.1 . . ?
C36 C37 H37 120.1 . . ?
C37 C38 C39 120.1(4) . . ?
C37 C38 H38 119.9 . . ?
C39 C38 H38 119.9 . . ?
C40 C39 C38 118.1(4) . . ?
C40 C39 H39 121.0 . . ?
C38 C39 H39 121.0 . . ?
N12 C40 C39 123.7(4) . . ?
N12 C40 H40 118.1 . . ?
C39 C40 H40 118.1 . . ?
C42 C41 H41A 109.5 . . ?
C42 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C42 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O1 C42 C41 109.3(6) . . ?
O1 C42 H42A 109.8 . . ?
C41 C42 H42A 109.8 . . ?
O1 C42 H42B 109.8 . . ?
C41 C42 H42B 109.8 . . ?
H42A C42 H42B 108.3 . . ?
O1 C43 C44 110.0(5) . . ?
O1 C43 H43A 109.7 . . ?
C44 C43 H43A 109.7 . . ?
O1 C43 H43B 109.7 . . ?
C44 C43 H43B 109.7 . . ?
H43A C43 H43B 108.2 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C1 N1 C5 118.0(4) . . ?
C1 N1 CO1 119.1(3) . . ?
C5 N1 CO1 122.7(3) . . ?
C11 N2 C15 117.5(4) . . ?
C11 N2 CO1 120.5(3) . . ?
C15 N2 CO1 121.9(3) . . ?
C25 N3 C21 117.7(4) . . ?
C25 N3 CO1 120.1(3) . . ?
C21 N3 CO1 122.1(3) . . ?
C31 N4 C35 117.5(4) . . ?
C31 N4 CO1 120.5(3) . . ?
C35 N4 CO1 121.9(3) . . ?
C6 N5 C5 124.8(4) . . ?
C6 N5 CO2 116.9(3) . . ?
C5 N5 CO2 118.2(3) . . ?
C16 N6 C15 124.0(4) . . ?
C16 N6 CO2 116.9(3) . . ?
C15 N6 CO2 119.1(3) . . ?
C26 N7 C25 123.0(3) . . ?
C26 N7 CO2 116.7(3) . . ?
C25 N7 CO2 120.3(3) . . ?
C36 N8 C35 124.8(4) . . ?
C36 N8 CO2 116.7(3) . . ?
C35 N8 CO2 118.5(3) . . ?
C10 N9 C6 118.2(4) . . ?
C10 N9 CO3 122.5(3) . . ?
C6 N9 CO3 119.3(3) . . ?
C20 N10 C16 118.4(4) . . ?
C20 N10 CO3 122.7(3) . . ?
C16 N10 CO3 118.6(3) . . ?
C30 N11 C26 117.6(4) . . ?
C30 N11 CO3 123.4(3) . . ?
C26 N11 CO3 118.7(3) . . ?
C40 N12 C36 119.0(4) . . ?
C40 N12 CO3 121.6(3) . . ?
C36 N12 CO3 119.4(3) . . ?
C43 O1 C42 112.9(5) . . ?
N2 CO1 N4 162.17(14) . . ?
N2 CO1 N3 90.15(14) . . ?
N4 CO1 N3 89.47(14) . . ?
N2 CO1 N1 88.56(13) . . ?
N4 CO1 N1 86.15(14) . . ?
N3 CO1 N1 161.37(14) . . ?
N2 CO1 CO2 81.32(10) . . ?
N4 CO1 CO2 80.96(10) . . ?
N3 CO1 CO2 82.15(10) . . ?
N1 CO1 CO2 79.28(10) . . ?
N2 CO1 I1 98.20(10) . . ?
N4 CO1 I1 99.48(10) . . ?
N3 CO1 I1 98.91(10) . . ?
N1 CO1 I1 99.68(10) . . ?
CO2 CO1 I1 178.85(3) . . ?
N5 CO2 N7 178.85(15) . . ?
N5 CO2 N8 89.35(15) . . ?
N7 CO2 N8 90.59(14) . . ?
N5 CO2 N6 90.14(15) . . ?
N7 CO2 N6 89.90(14) . . ?
N8 CO2 N6 179.20(15) . . ?
N5 CO2 CO3 90.07(11) . . ?
N7 CO2 CO3 88.78(10) . . ?
N8 CO2 CO3 90.71(10) . . ?
N6 CO2 CO3 88.66(10) . . ?
N5 CO2 CO1 92.50(11) . . ?
N7 CO2 CO1 88.65(10) . . ?
N8 CO2 CO1 90.26(10) . . ?
N6 CO2 CO1 90.39(10) . . ?
CO3 CO2 CO1 177.26(3) . . ?
N9 CO3 N10 88.16(14) . . ?
N9 CO3 N11 170.62(14) . . ?
N10 CO3 N11 90.24(14) . . ?
N9 CO3 N12 89.11(14) . . ?
N10 CO3 N12 169.75(14) . . ?
N11 CO3 N12 90.85(14) . . ?
N9 CO3 CO2 84.92(10) . . ?
N10 CO3 CO2 85.55(10) . . ?
N11 CO3 CO2 85.74(10) . . ?
N12 CO3 CO2 84.37(10) . . ?
N9 CO3 I2 95.40(10) . . ?
N10 CO3 I2 94.86(10) . . ?
N11 CO3 I2 93.94(10) . . ?
N12 CO3 I2 95.23(10) . . ?
CO2 CO3 I2 179.49(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
N1 C1 C2 C3 -1.3(7) . . . . ?
C1 C2 C3 C4 2.3(7) . . . . ?
C2 C3 C4 C5 -1.9(7) . . . . ?
C3 C4 C5 N5 -172.3(4) . . . . ?
C3 C4 C5 N1 0.3(7) . . . . ?
N5 C6 C7 C8 -171.2(4) . . . . ?
N9 C6 C7 C8 2.3(7) . . . . ?
C6 C7 C8 C9 0.4(7) . . . . ?
C7 C8 C9 C10 -1.0(8) . . . . ?
C8 C9 C10 N9 -1.1(7) . . . . ?
N2 C11 C12 C13 -0.2(8) . . . . ?
C11 C12 C13 C14 -0.1(8) . . . . ?
C12 C13 C14 C15 -0.5(7) . . . . ?
C13 C14 C15 N2 1.5(7) . . . . ?
C13 C14 C15 N6 -171.8(4) . . . . ?
N6 C16 C17 C18 -168.1(4) . . . . ?
N10 C16 C17 C18 3.6(7) . . . . ?
C16 C17 C18 C19 0.3(7) . . . . ?
C17 C18 C19 C20 -1.7(7) . . . . ?
C18 C19 C20 N10 -0.8(7) . . . . ?
N3 C21 C22 C23 -0.5(7) . . . . ?
C21 C22 C23 C24 -0.4(7) . . . . ?
C22 C23 C24 C25 0.2(7) . . . . ?
C23 C24 C25 N3 1.0(6) . . . . ?
C23 C24 C25 N7 -172.4(4) . . . . ?
N7 C26 C27 C28 -170.1(4) . . . . ?
N11 C26 C27 C28 1.7(6) . . . . ?
C26 C27 C28 C29 -1.9(7) . . . . ?
C27 C28 C29 C30 1.7(6) . . . . ?
C28 C29 C30 N11 -1.3(7) . . . . ?
N4 C31 C32 C33 -2.8(7) . . . . ?
C31 C32 C33 C34 2.4(7) . . . . ?
C32 C33 C34 C35 -1.7(7) . . . . ?
C33 C34 C35 N4 1.1(7) . . . . ?
C33 C34 C35 N8 -173.0(4) . . . . ?
N8 C36 C37 C38 -170.5(4) . . . . ?
N12 C36 C37 C38 4.1(6) . . . . ?
C36 C37 C38 C39 1.1(7) . . . . ?
C37 C38 C39 C40 -2.9(7) . . . . ?
C38 C39 C40 N12 -0.5(7) . . . . ?
C2 C1 N1 C5 -0.2(7) . . . . ?
C2 C1 N1 CO1 174.7(4) . . . . ?
N5 C5 N1 C1 174.0(4) . . . . ?
C4 C5 N1 C1 0.7(6) . . . . ?
N5 C5 N1 CO1 -0.7(5) . . . . ?
C4 C5 N1 CO1 -174.0(3) . . . . ?
C12 C11 N2 C15 1.2(7) . . . . ?
C12 C11 N2 CO1 178.0(4) . . . . ?
N6 C15 N2 C11 172.1(4) . . . . ?
C14 C15 N2 C11 -1.8(6) . . . . ?
N6 C15 N2 CO1 -4.7(5) . . . . ?
C14 C15 N2 CO1 -178.5(3) . . . . ?
N7 C25 N3 C21 172.1(4) . . . . ?
C24 C25 N3 C21 -1.9(6) . . . . ?
N7 C25 N3 CO1 -4.0(5) . . . . ?
C24 C25 N3 CO1 -177.9(3) . . . . ?
C22 C21 N3 C25 1.7(6) . . . . ?
C22 C21 N3 CO1 177.6(3) . . . . ?
C32 C31 N4 C35 2.3(7) . . . . ?
C32 C31 N4 CO1 179.5(4) . . . . ?
N8 C35 N4 C31 173.4(4) . . . . ?
C34 C35 N4 C31 -1.3(6) . . . . ?
N8 C35 N4 CO1 -3.8(5) . . . . ?
C34 C35 N4 CO1 -178.5(3) . . . . ?
N9 C6 N5 C5 154.4(4) . . . . ?
C7 C6 N5 C5 -31.8(6) . . . . ?
N9 C6 N5 CO2 -21.7(5) . . . . ?
C7 C6 N5 CO2 152.1(4) . . . . ?
N1 C5 N5 C6 155.6(4) . . . . ?
C4 C5 N5 C6 -31.5(7) . . . . ?
N1 C5 N5 CO2 -28.4(5) . . . . ?
C4 C5 N5 CO2 144.5(4) . . . . ?
N10 C16 N6 C15 155.7(4) . . . . ?
C17 C16 N6 C15 -32.3(6) . . . . ?
N10 C16 N6 CO2 -24.0(5) . . . . ?
C17 C16 N6 CO2 148.1(4) . . . . ?
N2 C15 N6 C16 155.5(4) . . . . ?
C14 C15 N6 C16 -30.9(6) . . . . ?
N2 C15 N6 CO2 -24.9(5) . . . . ?
C14 C15 N6 CO2 148.8(4) . . . . ?
N11 C26 N7 C25 153.5(4) . . . . ?
C27 C26 N7 C25 -34.2(6) . . . . ?
N11 C26 N7 CO2 -28.5(4) . . . . ?
C27 C26 N7 CO2 143.7(3) . . . . ?
N3 C25 N7 C26 150.0(4) . . . . ?
C24 C25 N7 C26 -36.2(6) . . . . ?
N3 C25 N7 CO2 -27.8(5) . . . . ?
C24 C25 N7 CO2 145.9(4) . . . . ?
N12 C36 N8 C35 159.4(4) . . . . ?
C37 C36 N8 C35 -25.8(6) . . . . ?
N12 C36 N8 CO2 -18.6(5) . . . . ?
C37 C36 N8 CO2 156.1(3) . . . . ?
N4 C35 N8 C36 154.5(4) . . . . ?
C34 C35 N8 C36 -31.1(6) . . . . ?
N4 C35 N8 CO2 -27.5(5) . . . . ?
C34 C35 N8 CO2 147.0(4) . . . . ?
C9 C10 N9 C6 3.8(7) . . . . ?
C9 C10 N9 CO3 -177.7(4) . . . . ?
N5 C6 N9 C10 169.7(4) . . . . ?
C7 C6 N9 C10 -4.3(6) . . . . ?
N5 C6 N9 CO3 -8.7(5) . . . . ?
C7 C6 N9 CO3 177.2(3) . . . . ?
C19 C20 N10 C16 4.7(6) . . . . ?
C19 C20 N10 CO3 179.2(3) . . . . ?
N6 C16 N10 C20 166.5(4) . . . . ?
C17 C16 N10 C20 -6.0(6) . . . . ?
N6 C16 N10 CO3 -8.2(5) . . . . ?
C17 C16 N10 CO3 179.3(3) . . . . ?
C29 C30 N11 C26 1.0(6) . . . . ?
C29 C30 N11 CO3 175.1(3) . . . . ?
N7 C26 N11 C30 171.4(4) . . . . ?
C27 C26 N11 C30 -1.2(6) . . . . ?
N7 C26 N11 CO3 -3.0(5) . . . . ?
C27 C26 N11 CO3 -175.5(3) . . . . ?
C39 C40 N12 C36 5.6(6) . . . . ?
C39 C40 N12 CO3 -174.6(3) . . . . ?
N8 C36 N12 C40 167.8(4) . . . . ?
C37 C36 N12 C40 -7.3(6) . . . . ?
N8 C36 N12 CO3 -12.0(5) . . . . ?
C37 C36 N12 CO3 172.9(3) . . . . ?
C44 C43 O1 C42 -176.8(5) . . . . ?
C41 C42 O1 C43 178.6(5) . . . . ?
C6 N5 CO2 N8 -56.3(3) . . . . ?
C5 N5 CO2 N8 127.3(3) . . . . ?
C6 N5 CO2 N6 123.0(3) . . . . ?
C5 N5 CO2 N6 -53.3(3) . . . . ?
C6 N5 CO2 CO3 34.4(3) . . . . ?
C5 N5 CO2 CO3 -142.0(3) . . . . ?
C6 N5 CO2 CO1 -146.6(3) . . . . ?
C5 N5 CO2 CO1 37.1(3) . . . . ?
C26 N7 CO2 N8 129.5(3) . . . . ?
C25 N7 CO2 N8 -52.5(3) . . . . ?
C26 N7 CO2 N6 -49.9(3) . . . . ?
C25 N7 CO2 N6 128.1(3) . . . . ?
C26 N7 CO2 CO3 38.8(3) . . . . ?
C25 N7 CO2 CO3 -143.2(3) . . . . ?
C26 N7 CO2 CO1 -140.3(3) . . . . ?
C25 N7 CO2 CO1 37.7(3) . . . . ?

_refine_diff_density_max         0.703
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.115


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile, ether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_4-CLCH22-85K
_database_code_depnum_ccdc_archive 'CCDC 1865589'
_audit_update_record             
;
2018-09-03 deposited with the CCDC.
2018-11-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C40 H32 Co3 I2 N12, C2 H4 Cl2'
_chemical_formula_sum            'C42 H36 Cl2 Co3 I2 N12'
_chemical_formula_weight         1210.32

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'
Cl Cl 0.1484 0.1585 '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'
I I -0.4742 1.8119 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/n'
_space_group_name_Hall           '-P 2yac'

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

_cell_length_a                   13.0572(5)
_cell_length_b                   11.4574(4)
_cell_length_c                   14.2468(5)
_cell_angle_alpha                90
_cell_angle_beta                 94.467(2)
_cell_angle_gamma                90
_cell_volume                     2124.87(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    85(2)
_cell_measurement_reflns_used    9872
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      27.48

_exptl_crystal_description       needle
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.892
_exptl_crystal_F_000             1186
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    2.785
_shelx_estimated_absorpt_T_min   0.337
_shelx_estimated_absorpt_T_max   0.713
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6505
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS (Bruker, 2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      85(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            41086
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.777
_diffrn_reflns_theta_max         27.510
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4881
_reflns_number_gt                4311
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2014)'
_computing_publication_material  'SHELXL-2016/4 (Sheldrick, 2016)'
_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)+(0.0186P)²+3.9022P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_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_number_reflns         4881
_refine_ls_number_parameters     326
_refine_ls_number_restraints     62
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0211
_refine_ls_wR_factor_ref         0.0506
_refine_ls_wR_factor_gt          0.0486
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.004
_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
C1 C 0.93287(16) 0.07455(19) 0.11751(15) 0.0104(4) Uani 1 1 d . . . . .
H1 H 1.002427 0.098815 0.117323 0.012 Uiso 1 1 calc R U . . .
C2 C 0.91000(17) -0.0406(2) 0.09749(16) 0.0134(4) Uani 1 1 d . . . . .
H2 H 0.961864 -0.093090 0.080745 0.016 Uiso 1 1 calc R U . . .
C3 C 0.80913(18) -0.0784(2) 0.10234(17) 0.0149(5) Uani 1 1 d . . . . .
H3 H 0.791237 -0.157675 0.090533 0.018 Uiso 1 1 calc R U . . .
C4 C 0.73558(17) 0.00155(19) 0.12463(16) 0.0118(4) Uani 1 1 d . . . . .
H4 H 0.666758 -0.023197 0.129502 0.014 Uiso 1 1 calc R U . . .
C5 C 0.76206(16) 0.11928(18) 0.14012(14) 0.0081(4) Uani 1 1 d . . . . .
C6 C 0.43378(16) 0.28012(19) 0.17910(15) 0.0107(4) Uani 1 1 d . . . . .
H6 H 0.394873 0.325463 0.219370 0.013 Uiso 1 1 calc R U . . .
C7 C 0.38499(17) 0.2374(2) 0.09729(16) 0.0147(5) Uani 1 1 d . . . . .
H7 H 0.314099 0.252061 0.081656 0.018 Uiso 1 1 calc R U . . .
C8 C 0.44264(18) 0.1720(2) 0.03791(16) 0.0157(5) Uani 1 1 d . . . . .
H8 H 0.410585 0.139321 -0.018225 0.019 Uiso 1 1 calc R U . . .
C9 C 0.54556(18) 0.1546(2) 0.06044(16) 0.0135(5) Uani 1 1 d . . . . .
H9 H 0.585169 0.111069 0.019566 0.016 Uiso 1 1 calc R U . . .
C10 C 0.59228(16) 0.20185(18) 0.14465(15) 0.0085(4) Uani 1 1 d . . . . .
C11 C 0.96877(16) 0.56443(19) 0.17532(15) 0.0102(4) Uani 1 1 d . . . . .
H11 H 0.996576 0.542867 0.118145 0.012 Uiso 1 1 calc R U . . .
C12 C 0.98483(18) 0.67681(19) 0.20813(16) 0.0134(4) Uani 1 1 d . . . . .
H12 H 1.024434 0.730344 0.175131 0.016 Uiso 1 1 calc R U . . .
C13 C 0.94205(18) 0.7102(2) 0.29025(16) 0.0147(5) Uani 1 1 d . . . . .
H13 H 0.953029 0.786667 0.314850 0.018 Uiso 1 1 calc R U . . .
C14 C 0.88351(17) 0.6312(2) 0.33562(16) 0.0124(4) Uani 1 1 d . . . . .
H14 H 0.852462 0.653587 0.391006 0.015 Uiso 1 1 calc R U . . .
C15 C 0.86974(15) 0.51710(18) 0.29970(14) 0.0079(4) Uani 1 1 d . . . . .
C16 C 0.83047(16) 0.34634(19) -0.02717(15) 0.0101(4) Uani 1 1 d . . . . .
H16 H 0.891354 0.303618 -0.035906 0.012 Uiso 1 1 calc R U . . .
C17 C 0.76831(17) 0.3773(2) -0.10558(15) 0.0132(5) Uani 1 1 d . . . . .
H17 H 0.786049 0.356516 -0.166794 0.016 Uiso 1 1 calc R U . . .
C18 C 0.67876(17) 0.4399(2) -0.09343(16) 0.0131(4) Uani 1 1 d . . . . .
H18 H 0.635049 0.463807 -0.146364 0.016 Uiso 1 1 calc R U . . .
C19 C 0.65465(16) 0.4665(2) -0.00359(15) 0.0113(4) Uani 1 1 d . . . . .
H19 H 0.594031 0.509441 0.005766 0.014 Uiso 1 1 calc R U . . .
C20 C 0.71962(16) 0.43028(18) 0.07457(15) 0.0079(4) Uani 1 1 d . . . . .
Co1 Co 0.89936(2) 0.31911(2) 0.17254(2) 0.00585(6) Uani 1 1 d . . . . .
Co2 Co 0.750000 0.32090(3) 0.250000 0.00637(8) Uani 1 2 d S T P . .
I1 I 1.08640(2) 0.32160(2) 0.07657(2) 0.01172(5) Uani 1 1 d . . . . .
N1 N 0.86178(13) 0.15521(15) 0.13747(12) 0.0079(3) Uani 1 1 d . . . . .
N2 N 0.53460(13) 0.26106(15) 0.20556(12) 0.0078(3) Uani 1 1 d . . . . .
N3 N 0.91539(13) 0.48339(15) 0.22050(12) 0.0074(3) Uani 1 1 d . . . . .
N4 N 0.80948(13) 0.37349(15) 0.06184(12) 0.0075(3) Uani 1 1 d . . . . .
N5 N 0.69539(13) 0.20224(15) 0.16827(12) 0.0081(3) Uani 1 1 d . . . . .
N6 N 0.69500(13) 0.43672(16) 0.16624(12) 0.0079(3) Uani 1 1 d . . . . .
Cl1 Cl 0.1325(8) -0.0738(13) 0.3155(11) 0.047(4) Uani 0.0985(16) 1 d D U P A -1
C21 C 0.2565(16) -0.008(2) 0.3350(14) 0.025(4) Uani 0.0985(16) 1 d D U P A -1
H21A H 0.252427 0.060209 0.377496 0.030 Uiso 0.0985(16) 1 calc R U P A -1
H21B H 0.305523 -0.064555 0.365611 0.030 Uiso 0.0985(16) 1 calc R U P A -1
C22 C 0.293(2) 0.0306(19) 0.2446(18) 0.019(6) Uiso 0.0985(16) 1 d D U P A -1
H22A H 0.356408 0.077956 0.257480 0.023 Uiso 0.0985(16) 1 calc R U P A -1
H22B H 0.240649 0.081268 0.211756 0.023 Uiso 0.0985(16) 1 calc R U P A -1
Cl2 Cl 0.3212(14) -0.0883(15) 0.1682(12) 0.076(6) Uani 0.0985(16) 1 d D U P A
-1
Cl3 Cl 0.2870(13) -0.0787(11) 0.3630(10) 0.034(3) Uani 0.4015(16) 1 d D U P A
-2
C23 C 0.291(2) 0.0384(11) 0.2805(13) 0.018(3) Uani 0.4015(16) 1 d D U P A -2
H23A H 0.296021 0.113500 0.314890 0.022 Uiso 0.4015(16) 1 calc R U P A -2
H23B H 0.352504 0.030200 0.244832 0.022 Uiso 0.4015(16) 1 calc R U P A -2
C24 C 0.197(2) 0.0395(13) 0.2135(15) 0.022(3) Uani 0.4015(16) 1 d D U P A -2
H24A H 0.195117 0.112973 0.176868 0.026 Uiso 0.4015(16) 1 calc R U P A -2
H24B H 0.135237 0.036637 0.249275 0.026 Uiso 0.4015(16) 1 calc R U P A -2
Cl4 Cl 0.1961(13) -0.0821(8) 0.1344(9) 0.0205(10) Uani 0.4015(16) 1 d D 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
C1 N1 1.356(3) . ?
C1 C2 1.378(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.393(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.382(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.406(3) . ?
C4 H4 0.9500 . ?
C5 N1 1.369(3) . ?
C5 N5 1.370(3) . ?
C6 N2 1.358(3) . ?
C6 C7 1.374(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.394(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.372(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.411(3) . ?
C9 H9 0.9500 . ?
C10 N5 1.362(3) . ?
C10 N2 1.372(3) . ?
C11 N3 1.353(3) . ?
C11 C12 1.380(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.389(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.378(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.411(3) . ?
C14 H14 0.9500 . ?
C15 N6 1.365(3) 2_655 ?
C15 N3 1.372(3) . ?
C16 N4 1.354(3) . ?
C16 C17 1.375(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.394(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.376(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.409(3) . ?
C19 H19 0.9500 . ?
C20 N4 1.366(3) . ?
C20 N6 1.371(3) . ?
Co1 N4 1.9910(17) . ?
Co1 N2 1.9922(17) 2_655 ?
Co1 N1 1.9947(18) . ?
Co1 N3 2.0078(18) . ?
Co1 Co2 2.3146(3) . ?
Co1 I1 2.8904(3) . ?
Co2 N6 1.8888(18) 2_655 ?
Co2 N6 1.8888(18) . ?
Co2 N5 1.8929(18) 2_655 ?
Co2 N5 1.8929(18) . ?
Cl1 C21 1.790(17) . ?
C21 C22 1.477(17) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 Cl2 1.799(18) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
Cl3 C23 1.787(9) . ?
C23 C24 1.491(8) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 Cl4 1.791(9) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?

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
N1 C1 C2 123.7(2) . . ?
N1 C1 H1 118.1 . . ?
C2 C1 H1 118.1 . . ?
C1 C2 C3 118.5(2) . . ?
C1 C2 H2 120.7 . . ?
C3 C2 H2 120.7 . . ?
C4 C3 C2 118.8(2) . . ?
C4 C3 H3 120.6 . . ?
C2 C3 H3 120.6 . . ?
C3 C4 C5 120.3(2) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
N1 C5 N5 115.27(18) . . ?
N1 C5 C4 120.47(19) . . ?
N5 C5 C4 123.9(2) . . ?
N2 C6 C7 123.6(2) . . ?
N2 C6 H6 118.2 . . ?
C7 C6 H6 118.2 . . ?
C6 C7 C8 118.0(2) . . ?
C6 C7 H7 121.0 . . ?
C8 C7 H7 121.0 . . ?
C9 C8 C7 120.1(2) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C8 C9 C10 119.6(2) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
N5 C10 N2 115.02(18) . . ?
N5 C10 C9 124.4(2) . . ?
N2 C10 C9 120.35(19) . . ?
N3 C11 C12 123.3(2) . . ?
N3 C11 H11 118.3 . . ?
C12 C11 H11 118.3 . . ?
C11 C12 C13 118.8(2) . . ?
C11 C12 H12 120.6 . . ?
C13 C12 H12 120.6 . . ?
C14 C13 C12 119.2(2) . . ?
C14 C13 H13 120.4 . . ?
C12 C13 H13 120.4 . . ?
C13 C14 C15 119.9(2) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
N6 C15 N3 115.04(18) 2_655 . ?
N6 C15 C14 124.16(19) 2_655 . ?
N3 C15 C14 120.54(19) . . ?
N4 C16 C17 123.5(2) . . ?
N4 C16 H16 118.3 . . ?
C17 C16 H16 118.3 . . ?
C16 C17 C18 118.7(2) . . ?
C16 C17 H17 120.7 . . ?
C18 C17 H17 120.7 . . ?
C19 C18 C17 119.0(2) . . ?
C19 C18 H18 120.5 . . ?
C17 C18 H18 120.5 . . ?
C18 C19 C20 120.2(2) . . ?
C18 C19 H19 119.9 . . ?
C20 C19 H19 119.9 . . ?
N4 C20 N6 114.81(18) . . ?
N4 C20 C19 120.40(19) . . ?
N6 C20 C19 124.44(19) . . ?
N4 Co1 N2 169.54(7) . 2_655 ?
N4 Co1 N1 88.73(7) . . ?
N2 Co1 N1 89.16(7) 2_655 . ?
N4 Co1 N3 90.90(7) . . ?
N2 Co1 N3 89.41(7) 2_655 . ?
N1 Co1 N3 170.03(7) . . ?
N4 Co1 Co2 84.74(5) . . ?
N2 Co1 Co2 84.88(5) 2_655 . ?
N1 Co1 Co2 85.86(5) . . ?
N3 Co1 Co2 84.19(5) . . ?
N4 Co1 I1 95.16(5) . . ?
N2 Co1 I1 95.24(5) 2_655 . ?
N1 Co1 I1 95.24(5) . . ?
N3 Co1 I1 94.72(5) . . ?
Co2 Co1 I1 178.902(16) . . ?
N6 Co2 N6 90.73(11) 2_655 . ?
N6 Co2 N5 90.54(8) 2_655 2_655 ?
N6 Co2 N5 178.69(8) . 2_655 ?
N6 Co2 N5 178.69(8) 2_655 . ?
N6 Co2 N5 90.54(8) . . ?
N5 Co2 N5 88.19(11) 2_655 . ?
N6 Co2 Co1 89.88(5) 2_655 2_655 ?
N6 Co2 Co1 90.83(5) . 2_655 ?
N5 Co2 Co1 89.51(5) 2_655 2_655 ?
N5 Co2 Co1 89.77(5) . 2_655 ?
N6 Co2 Co1 90.83(5) 2_655 . ?
N6 Co2 Co1 89.88(5) . . ?
N5 Co2 Co1 89.77(5) 2_655 . ?
N5 Co2 Co1 89.51(5) . . ?
Co1 Co2 Co1 178.99(2) 2_655 . ?
C1 N1 C5 117.97(18) . . ?
C1 N1 Co1 122.36(15) . . ?
C5 N1 Co1 119.49(14) . . ?
C6 N2 C10 118.15(18) . . ?
C6 N2 Co1 122.17(15) . 2_655 ?
C10 N2 Co1 119.66(14) . 2_655 ?
C11 N3 C15 118.08(18) . . ?
C11 N3 Co1 121.67(14) . . ?
C15 N3 Co1 120.22(14) . . ?
C16 N4 C20 118.18(18) . . ?
C16 N4 Co1 121.33(14) . . ?
C20 N4 Co1 120.22(14) . . ?
C10 N5 C5 124.32(18) . . ?
C10 N5 Co2 118.17(14) . . ?
C5 N5 Co2 117.44(14) . . ?
C15 N6 C20 124.95(18) 2_655 . ?
C15 N6 Co2 117.71(14) 2_655 . ?
C20 N6 Co2 117.27(14) . . ?
C22 C21 Cl1 110.1(14) . . ?
C22 C21 H21A 109.6 . . ?
Cl1 C21 H21A 109.6 . . ?
C22 C21 H21B 109.6 . . ?
Cl1 C21 H21B 109.6 . . ?
H21A C21 H21B 108.2 . . ?
C21 C22 Cl2 113.4(15) . . ?
C21 C22 H22A 108.9 . . ?
Cl2 C22 H22A 108.9 . . ?
C21 C22 H22B 108.9 . . ?
Cl2 C22 H22B 108.9 . . ?
H22A C22 H22B 107.7 . . ?
C24 C23 Cl3 111.3(9) . . ?
C24 C23 H23A 109.4 . . ?
Cl3 C23 H23A 109.4 . . ?
C24 C23 H23B 109.4 . . ?
Cl3 C23 H23B 109.4 . . ?
H23A C23 H23B 108.0 . . ?
C23 C24 Cl4 111.3(9) . . ?
C23 C24 H24A 109.4 . . ?
Cl4 C24 H24A 109.4 . . ?
C23 C24 H24B 109.4 . . ?
Cl4 C24 H24B 109.4 . . ?
H24A C24 H24B 108.0 . . ?

_refine_diff_density_max         0.475
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.083


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dichloroethane'
####################################################################### 
# 
# 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_2-Et2O-350K
_database_code_depnum_ccdc_archive 'CCDC 1877180'
_audit_update_record             
;
2018-11-05 deposited with the CCDC.
2018-11-07 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         'C40 H32 Cl2 Co3 N12, C4 H10 O'
_chemical_formula_sum            'C44 H42 Cl2 Co3 N12 O'
_chemical_formula_weight         1002.58

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'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   16.0520(12)
_cell_length_b                   15.9094(11)
_cell_length_c                   17.1371(11)
_cell_angle_alpha                90
_cell_angle_beta                 97.995(3)
_cell_angle_gamma                90
_cell_volume                     4333.9(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    350(2)
_cell_measurement_reflns_used    9945
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      26.24

_exptl_crystal_description       Blocks
_exptl_crystal_colour            'Dark green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_F_000             2052
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.291
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.170
_exptl_absorpt_coefficient_mu    1.309
_shelx_estimated_absorpt_T_min   0.702
_shelx_estimated_absorpt_T_max   0.808
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4857
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      350(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            36512
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.755
_diffrn_reflns_theta_max         26.386
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             8839
_reflns_number_gt                6200
_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       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_structure_solution    'SHELXS2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_publication_material  'SHELXL-2016/4 (Sheldrick, 2016)'
_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)+(0.0489P)²+2.9202P] 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_number_reflns         8839
_refine_ls_number_parameters     559
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0404
_refine_ls_wR_factor_ref         0.1162
_refine_ls_wR_factor_gt          0.1038
_refine_ls_goodness_of_fit_ref   1.040
_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
C1 C 0.4778(2) 0.4814(3) 0.7256(2) 0.0554(10) Uani 1 1 d . . . . .
H1 H 0.4585 0.5306 0.7462 0.066 Uiso 1 1 calc R U . . .
C2 C 0.4210(3) 0.4314(3) 0.6821(2) 0.0618(11) Uani 1 1 d . . . . .
H2 H 0.3642 0.4456 0.6735 0.074 Uiso 1 1 calc R U . . .
C3 C 0.4496(3) 0.3592(3) 0.6511(2) 0.0589(10) Uani 1 1 d . . . . .
H3 H 0.4119 0.3232 0.6216 0.071 Uiso 1 1 calc R U . . .
C4 C 0.5336(2) 0.3400(2) 0.6635(2) 0.0488(9) Uani 1 1 d . . . . .
H4 H 0.5532 0.2920 0.6411 0.059 Uiso 1 1 calc R U . . .
C5 C 0.5898(2) 0.39310(19) 0.70998(18) 0.0372(7) Uani 1 1 d . . . . .
C6 C 0.7139(2) 0.30569(19) 0.72275(18) 0.0375(7) Uani 1 1 d . . . . .
C7 C 0.6782(3) 0.2287(2) 0.7419(2) 0.0518(9) Uani 1 1 d . . . . .
H7 H 0.6224 0.2267 0.7508 0.062 Uiso 1 1 calc R U . . .
C8 C 0.7253(3) 0.1574(2) 0.7474(2) 0.0623(11) Uani 1 1 d . . . . .
H8 H 0.7017 0.1065 0.7594 0.075 Uiso 1 1 calc R U . . .
C9 C 0.8084(3) 0.1613(2) 0.7349(2) 0.0668(12) Uani 1 1 d . . . . .
H9 H 0.8417 0.1132 0.7392 0.080 Uiso 1 1 calc R U . . .
C10 C 0.8408(3) 0.2365(2) 0.7164(2) 0.0537(10) Uani 1 1 d . . . . .
H10 H 0.8972 0.2389 0.7093 0.064 Uiso 1 1 calc R U . . .
C11 C 0.5806(3) 0.6982(2) 0.7054(2) 0.0573(10) Uani 1 1 d . . . . .
H11 H 0.5651 0.7169 0.7527 0.069 Uiso 1 1 calc R U . . .
C12 C 0.5597(3) 0.7466(2) 0.6403(3) 0.0698(12) Uani 1 1 d . . . . .
H12 H 0.5277 0.7951 0.6423 0.084 Uiso 1 1 calc R U . . .
C13 C 0.5874(3) 0.7221(2) 0.5712(2) 0.0665(12) Uani 1 1 d . . . . .
H13 H 0.5754 0.7547 0.5260 0.080 Uiso 1 1 calc R U . . .
C14 C 0.6323(3) 0.6498(2) 0.5696(2) 0.0536(10) Uani 1 1 d . . . . .
H14 H 0.6527 0.6339 0.5236 0.064 Uiso 1 1 calc R U . . .
C15 C 0.6481(2) 0.5990(2) 0.63713(18) 0.0390(7) Uani 1 1 d . . . . .
C16 C 0.6914(2) 0.47351(19) 0.57608(18) 0.0369(7) Uani 1 1 d . . . . .
C17 C 0.6247(3) 0.4676(2) 0.5138(2) 0.0541(9) Uani 1 1 d . . . . .
H17 H 0.5789 0.5036 0.5126 0.065 Uiso 1 1 calc R U . . .
C18 C 0.6261(3) 0.4105(3) 0.4553(2) 0.0664(12) Uani 1 1 d . . . . .
H18 H 0.5815 0.4065 0.4146 0.080 Uiso 1 1 calc R U . . .
C19 C 0.6953(3) 0.3583(3) 0.4574(2) 0.0713(13) Uani 1 1 d . . . . .
H19 H 0.6986 0.3195 0.4174 0.086 Uiso 1 1 calc R U . . .
C20 C 0.7590(3) 0.3644(2) 0.5194(2) 0.0558(10) Uani 1 1 d . . . . .
H20 H 0.8049 0.3285 0.5208 0.067 Uiso 1 1 calc R U . . .
C21 C 0.7369(3) 0.6576(2) 0.9250(2) 0.0531(10) Uani 1 1 d . . . . .
H21 H 0.6876 0.6530 0.9475 0.064 Uiso 1 1 calc R U . . .
C22 C 0.8015(3) 0.7021(3) 0.9642(2) 0.0669(12) Uani 1 1 d . . . . .
H22 H 0.7959 0.7289 1.0115 0.080 Uiso 1 1 calc R U . . .
C23 C 0.8760(3) 0.7070(2) 0.9325(2) 0.0600(11) Uani 1 1 d . . . . .
H23 H 0.9214 0.7370 0.9583 0.072 Uiso 1 1 calc R U . . .
C24 C 0.8821(2) 0.6676(2) 0.8632(2) 0.0487(9) Uani 1 1 d . . . . .
H24 H 0.9326 0.6692 0.8423 0.058 Uiso 1 1 calc R U . . .
C25 C 0.8123(2) 0.62418(18) 0.82263(17) 0.0359(7) Uani 1 1 d . . . . .
C26 C 0.8660(2) 0.59742(19) 0.70086(17) 0.0340(7) Uani 1 1 d . . . . .
C27 C 0.8981(2) 0.6781(2) 0.68798(19) 0.0461(9) Uani 1 1 d . . . . .
H27 H 0.8854 0.7232 0.7189 0.055 Uiso 1 1 calc R U . . .
C28 C 0.9476(3) 0.6903(2) 0.6305(2) 0.0558(10) Uani 1 1 d . . . . .
H28 H 0.9700 0.7432 0.6232 0.067 Uiso 1 1 calc R U . . .
C29 C 0.9643(3) 0.6241(2) 0.5831(2) 0.0580(11) Uani 1 1 d . . . . .
H29 H 0.9980 0.6313 0.5437 0.070 Uiso 1 1 calc R U . . .
C30 C 0.9301(2) 0.5477(2) 0.5957(2) 0.0490(9) Uani 1 1 d . . . . .
H30 H 0.9397 0.5036 0.5625 0.059 Uiso 1 1 calc R U . . .
C31 C 0.6173(3) 0.4402(2) 0.9379(2) 0.0583(11) Uani 1 1 d . . . . .
H31 H 0.5646 0.4656 0.9301 0.070 Uiso 1 1 calc R U . . .
C32 C 0.6347(3) 0.3860(3) 0.9994(2) 0.0718(13) Uani 1 1 d . . . . .
H32 H 0.5956 0.3758 1.0336 0.086 Uiso 1 1 calc R U . . .
C33 C 0.7123(3) 0.3462(3) 1.0098(2) 0.0686(13) Uani 1 1 d . . . . .
H33 H 0.7270 0.3103 1.0523 0.082 Uiso 1 1 calc R U . . .
C34 C 0.7668(3) 0.3606(2) 0.9567(2) 0.0551(10) Uani 1 1 d . . . . .
H34 H 0.8174 0.3314 0.9612 0.066 Uiso 1 1 calc R U . . .
C35 C 0.7473(2) 0.41880(19) 0.89559(17) 0.0391(8) Uani 1 1 d . . . . .
C36 C 0.8820(2) 0.42698(18) 0.84768(18) 0.0371(7) Uani 1 1 d . . . . .
C37 C 0.9354(3) 0.4289(2) 0.9197(2) 0.0536(9) Uani 1 1 d . . . . .
H37 H 0.9127 0.4290 0.9668 0.064 Uiso 1 1 calc R U . . .
C38 C 1.0211(3) 0.4307(3) 0.9211(3) 0.0667(12) Uani 1 1 d . . . . .
H38 H 1.0563 0.4313 0.9690 0.080 Uiso 1 1 calc R U . . .
C39 C 1.0548(3) 0.4317(3) 0.8522(3) 0.0700(12) Uani 1 1 d . . . . .
H39 H 1.1126 0.4350 0.8521 0.084 Uiso 1 1 calc R U . . .
C40 C 1.0002(2) 0.4275(2) 0.7828(2) 0.0552(10) Uani 1 1 d . . . . .
H40 H 1.0228 0.4278 0.7357 0.066 Uiso 1 1 calc R U . . .
N1 N 0.56070(17) 0.46441(17) 0.74092(16) 0.0417(7) Uani 1 1 d . . . . .
N2 N 0.62242(18) 0.62440(16) 0.70554(16) 0.0412(7) Uani 1 1 d . . . . .
N3 N 0.73990(18) 0.61935(16) 0.85495(15) 0.0389(6) Uani 1 1 d . . . . .
N4 N 0.67222(18) 0.45909(16) 0.88756(15) 0.0409(7) Uani 1 1 d . . . . .
N5 N 0.67514(16) 0.38263(15) 0.72315(14) 0.0340(6) Uani 1 1 d . . . . .
N6 N 0.69176(17) 0.52448(15) 0.64062(14) 0.0350(6) Uani 1 1 d . . . . .
N7 N 0.81362(16) 0.57898(15) 0.75488(14) 0.0334(6) Uani 1 1 d . . . . .
N8 N 0.79671(17) 0.43594(15) 0.83822(14) 0.0360(6) Uani 1 1 d . . . . .
N9 N 0.79488(18) 0.30804(15) 0.70788(15) 0.0385(6) Uani 1 1 d . . . . .
N10 N 0.75811(18) 0.42053(16) 0.57883(14) 0.0387(6) Uani 1 1 d . . . . .
N11 N 0.88315(17) 0.53244(16) 0.65367(15) 0.0371(6) Uani 1 1 d . . . . .
N12 N 0.91639(17) 0.42295(16) 0.77930(15) 0.0389(6) Uani 1 1 d . . . . .
Cl1 Cl 0.53483(6) 0.61929(6) 0.87119(6) 0.0600(3) Uani 1 1 d . . . . .
Cl2 Cl 0.95087(6) 0.34365(6) 0.60892(6) 0.0576(3) Uani 1 1 d . . . . .
Co1 Co 0.63955(3) 0.54957(3) 0.80380(3) 0.04047(13) Uani 1 1 d . . . . .
Co2 Co 0.74421(3) 0.48075(2) 0.73966(2) 0.02999(11) Uani 1 1 d . . . . .
Co3 Co 0.84558(3) 0.41586(3) 0.67432(2) 0.03597(12) Uani 1 1 d . . . . .
C1S C 0.1712(4) 0.4581(4) 0.6165(3) 0.123(2) Uani 1 1 d D . . . .
H1SA H 0.1462 0.4311 0.5688 0.185 Uiso 1 1 calc R U . . .
H1SB H 0.1314 0.4964 0.6340 0.185 Uiso 1 1 calc R U . . .
H1SC H 0.2203 0.4886 0.6067 0.185 Uiso 1 1 calc R U . . .
C2S C 0.1974(3) 0.3881(3) 0.6836(3) 0.112(2) Uani 1 1 d D . . . .
H2SA H 0.1488 0.3570 0.6956 0.135 Uiso 1 1 calc R U . . .
H2SB H 0.2385 0.3491 0.6681 0.135 Uiso 1 1 calc R U . . .
O1S O 0.2318(2) 0.4377(2) 0.74712(19) 0.0845(9) Uani 1 1 d D . . . .
C3S C 0.2684(4) 0.3857(3) 0.8070(3) 0.105(2) Uani 1 1 d D . . . .
H3SA H 0.3098 0.3496 0.7877 0.126 Uiso 1 1 calc R U . . .
H3SB H 0.2259 0.3505 0.8256 0.126 Uiso 1 1 calc R U . . .
C4S C 0.3126(4) 0.4429(4) 0.8771(3) 0.128(2) Uani 1 1 d D . . . .
H4SA H 0.3383 0.4076 0.9192 0.192 Uiso 1 1 calc R U . . .
H4SB H 0.3548 0.4772 0.8584 0.192 Uiso 1 1 calc R U . . .
H4SC H 0.2712 0.4781 0.8961 0.192 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
C1 N1 1.347(4) . ?
C1 C2 1.354(6) . ?
C1 H1 0.9300 . ?
C2 C3 1.372(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.369(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.401(5) . ?
C4 H4 0.9300 . ?
C5 N1 1.362(4) . ?
C5 N5 1.367(4) . ?
C6 N9 1.359(4) . ?
C6 N5 1.374(4) . ?
C6 C7 1.411(4) . ?
C7 C8 1.358(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.382(6) . ?
C8 H8 0.9300 . ?
C9 C10 1.360(5) . ?
C9 H9 0.9300 . ?
C10 N9 1.353(4) . ?
C10 H10 0.9300 . ?
C11 N2 1.352(4) . ?
C11 C12 1.359(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.377(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.359(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.405(5) . ?
C14 H14 0.9300 . ?
C15 N2 1.357(4) . ?
C15 N6 1.375(4) . ?
C16 N10 1.358(4) . ?
C16 N6 1.371(4) . ?
C16 C17 1.406(5) . ?
C17 C18 1.356(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.383(6) . ?
C18 H18 0.9300 . ?
C19 C20 1.372(6) . ?
C19 H19 0.9300 . ?
C20 N10 1.355(4) . ?
C20 H20 0.9300 . ?
C21 N3 1.352(4) . ?
C21 C22 1.355(5) . ?
C21 H21 0.9300 . ?
C22 C23 1.382(6) . ?
C22 H22 0.9300 . ?
C23 C24 1.359(5) . ?
C23 H23 0.9300 . ?
C24 C25 1.414(5) . ?
C24 H24 0.9300 . ?
C25 N3 1.358(4) . ?
C25 N7 1.368(4) . ?
C26 N11 1.364(4) . ?
C26 N7 1.366(4) . ?
C26 C27 1.412(4) . ?
C27 C28 1.363(5) . ?
C27 H27 0.9300 . ?
C28 C29 1.379(5) . ?
C28 H28 0.9300 . ?
C29 C30 1.363(5) . ?
C29 H29 0.9300 . ?
C30 N11 1.350(4) . ?
C30 H30 0.9300 . ?
C31 N4 1.350(4) . ?
C31 C32 1.361(5) . ?
C31 H31 0.9300 . ?
C32 C33 1.385(6) . ?
C32 H32 0.9300 . ?
C33 C34 1.367(5) . ?
C33 H33 0.9300 . ?
C34 C35 1.401(5) . ?
C34 H34 0.9300 . ?
C35 N4 1.355(4) . ?
C35 N8 1.374(4) . ?
C36 N12 1.364(4) . ?
C36 N8 1.364(4) . ?
C36 C37 1.402(5) . ?
C37 C38 1.373(6) . ?
C37 H37 0.9300 . ?
C38 C39 1.366(6) . ?
C38 H38 0.9300 . ?
C39 C40 1.376(6) . ?
C39 H39 0.9300 . ?
C40 N12 1.340(4) . ?
C40 H40 0.9300 . ?
N1 Co1 2.054(3) . ?
N2 Co1 2.049(3) . ?
N3 Co1 2.050(3) . ?
N4 Co1 2.049(3) . ?
N5 Co2 1.913(2) . ?
N6 Co2 1.917(3) . ?
N7 Co2 1.916(2) . ?
N8 Co2 1.917(3) . ?
N9 Co3 2.016(3) . ?
N10 Co3 2.004(3) . ?
N11 Co3 1.997(3) . ?
N12 Co3 1.993(3) . ?
Cl1 Co1 2.4350(9) . ?
Cl2 Co3 2.4412(9) . ?
Co1 Co2 2.3964(6) . ?
Co2 Co3 2.3397(6) . ?
C1S C2S 1.615(6) . ?
C1S H1SA 0.9600 . ?
C1S H1SB 0.9600 . ?
C1S H1SC 0.9600 . ?
C2S O1S 1.394(4) . ?
C2S H2SA 0.9700 . ?
C2S H2SB 0.9700 . ?
O1S C3S 1.384(4) . ?
C3S C4S 1.592(6) . ?
C3S H3SA 0.9700 . ?
C3S H3SB 0.9700 . ?
C4S H4SA 0.9600 . ?
C4S H4SB 0.9600 . ?
C4S H4SC 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 124.2(4) . . ?
N1 C1 H1 117.9 . . ?
C2 C1 H1 117.9 . . ?
C1 C2 C3 117.9(4) . . ?
C1 C2 H2 121.0 . . ?
C3 C2 H2 121.0 . . ?
C4 C3 C2 120.1(4) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 119.8(4) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
N1 C5 N5 115.3(3) . . ?
N1 C5 C4 119.7(3) . . ?
N5 C5 C4 124.9(3) . . ?
N9 C6 N5 115.0(3) . . ?
N9 C6 C7 119.9(3) . . ?
N5 C6 C7 125.0(3) . . ?
C8 C7 C6 120.0(4) . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C7 C8 C9 119.5(4) . . ?
C7 C8 H8 120.2 . . ?
C9 C8 H8 120.2 . . ?
C10 C9 C8 119.0(4) . . ?
C10 C9 H9 120.5 . . ?
C8 C9 H9 120.5 . . ?
N9 C10 C9 123.0(4) . . ?
N9 C10 H10 118.5 . . ?
C9 C10 H10 118.5 . . ?
N2 C11 C12 124.0(4) . . ?
N2 C11 H11 118.0 . . ?
C12 C11 H11 118.0 . . ?
C11 C12 C13 118.2(4) . . ?
C11 C12 H12 120.9 . . ?
C13 C12 H12 120.9 . . ?
C14 C13 C12 119.5(4) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C13 C14 C15 120.3(3) . . ?
C13 C14 H14 119.8 . . ?
C15 C14 H14 119.8 . . ?
N2 C15 N6 115.7(3) . . ?
N2 C15 C14 119.9(3) . . ?
N6 C15 C14 124.3(3) . . ?
N10 C16 N6 115.1(3) . . ?
N10 C16 C17 119.9(3) . . ?
N6 C16 C17 124.7(3) . . ?
C18 C17 C16 121.1(4) . . ?
C18 C17 H17 119.4 . . ?
C16 C17 H17 119.4 . . ?
C17 C18 C19 118.6(4) . . ?
C17 C18 H18 120.7 . . ?
C19 C18 H18 120.7 . . ?
C20 C19 C18 119.1(4) . . ?
C20 C19 H19 120.4 . . ?
C18 C19 H19 120.4 . . ?
N10 C20 C19 123.0(4) . . ?
N10 C20 H20 118.5 . . ?
C19 C20 H20 118.5 . . ?
N3 C21 C22 123.8(4) . . ?
N3 C21 H21 118.1 . . ?
C22 C21 H21 118.1 . . ?
C21 C22 C23 118.6(3) . . ?
C21 C22 H22 120.7 . . ?
C23 C22 H22 120.7 . . ?
C24 C23 C22 119.3(4) . . ?
C24 C23 H23 120.3 . . ?
C22 C23 H23 120.3 . . ?
C23 C24 C25 120.4(3) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 H24 119.8 . . ?
N3 C25 N7 115.5(3) . . ?
N3 C25 C24 119.5(3) . . ?
N7 C25 C24 124.7(3) . . ?
N11 C26 N7 115.7(3) . . ?
N11 C26 C27 119.2(3) . . ?
N7 C26 C27 125.0(3) . . ?
C28 C27 C26 120.3(3) . . ?
C28 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
C27 C28 C29 119.8(3) . . ?
C27 C28 H28 120.1 . . ?
C29 C28 H28 120.1 . . ?
C30 C29 C28 118.2(3) . . ?
C30 C29 H29 120.9 . . ?
C28 C29 H29 120.9 . . ?
N11 C30 C29 123.8(3) . . ?
N11 C30 H30 118.1 . . ?
C29 C30 H30 118.1 . . ?
N4 C31 C32 123.6(4) . . ?
N4 C31 H31 118.2 . . ?
C32 C31 H31 118.2 . . ?
C31 C32 C33 118.3(4) . . ?
C31 C32 H32 120.9 . . ?
C33 C32 H32 120.9 . . ?
C34 C33 C32 119.0(4) . . ?
C34 C33 H33 120.5 . . ?
C32 C33 H33 120.5 . . ?
C33 C34 C35 120.7(4) . . ?
C33 C34 H34 119.6 . . ?
C35 C34 H34 119.6 . . ?
N4 C35 N8 115.3(3) . . ?
N4 C35 C34 119.5(3) . . ?
N8 C35 C34 125.1(3) . . ?
N12 C36 N8 115.0(3) . . ?
N12 C36 C37 119.1(3) . . ?
N8 C36 C37 125.7(3) . . ?
C38 C37 C36 120.3(4) . . ?
C38 C37 H37 119.9 . . ?
C36 C37 H37 119.9 . . ?
C39 C38 C37 120.1(4) . . ?
C39 C38 H38 119.9 . . ?
C37 C38 H38 119.9 . . ?
C38 C39 C40 117.7(4) . . ?
C38 C39 H39 121.2 . . ?
C40 C39 H39 121.2 . . ?
N12 C40 C39 123.8(4) . . ?
N12 C40 H40 118.1 . . ?
C39 C40 H40 118.1 . . ?
C1 N1 C5 118.3(3) . . ?
C1 N1 Co1 119.3(2) . . ?
C5 N1 Co1 122.3(2) . . ?
C11 N2 C15 117.8(3) . . ?
C11 N2 Co1 121.1(2) . . ?
C15 N2 Co1 121.0(2) . . ?
C21 N3 C25 118.3(3) . . ?
C21 N3 Co1 120.0(2) . . ?
C25 N3 Co1 121.5(2) . . ?
C31 N4 C35 118.7(3) . . ?
C31 N4 Co1 118.5(3) . . ?
C35 N4 Co1 122.7(2) . . ?
C5 N5 C6 123.5(3) . . ?
C5 N5 Co2 118.1(2) . . ?
C6 N5 Co2 118.3(2) . . ?
C16 N6 C15 122.0(3) . . ?
C16 N6 Co2 116.9(2) . . ?
C15 N6 Co2 120.7(2) . . ?
C26 N7 C25 123.0(3) . . ?
C26 N7 Co2 118.94(19) . . ?
C25 N7 Co2 117.86(19) . . ?
C36 N8 C35 124.4(3) . . ?
C36 N8 Co2 117.04(19) . . ?
C35 N8 Co2 118.5(2) . . ?
C10 N9 C6 118.5(3) . . ?
C10 N9 Co3 120.7(2) . . ?
C6 N9 Co3 120.7(2) . . ?
C20 N10 C16 118.2(3) . . ?
C20 N10 Co3 120.6(2) . . ?
C16 N10 Co3 120.7(2) . . ?
C30 N11 C26 118.6(3) . . ?
C30 N11 Co3 120.7(2) . . ?
C26 N11 Co3 120.53(19) . . ?
C40 N12 C36 118.8(3) . . ?
C40 N12 Co3 119.1(2) . . ?
C36 N12 Co3 122.0(2) . . ?
N2 Co1 N4 167.37(10) . . ?
N2 Co1 N3 92.55(11) . . ?
N4 Co1 N3 88.37(11) . . ?
N2 Co1 N1 87.12(11) . . ?
N4 Co1 N1 89.03(11) . . ?
N3 Co1 N1 166.33(10) . . ?
N2 Co1 Co2 84.90(7) . . ?
N4 Co1 Co2 82.70(7) . . ?
N3 Co1 Co2 83.36(7) . . ?
N1 Co1 Co2 83.00(8) . . ?
N2 Co1 Cl1 95.89(8) . . ?
N4 Co1 Cl1 96.55(8) . . ?
N3 Co1 Cl1 95.95(8) . . ?
N1 Co1 Cl1 97.68(8) . . ?
Co2 Co1 Cl1 178.98(4) . . ?
N5 Co2 N7 179.30(10) . . ?
N5 Co2 N8 90.09(11) . . ?
N7 Co2 N8 90.42(11) . . ?
N5 Co2 N6 89.49(11) . . ?
N7 Co2 N6 90.00(11) . . ?
N8 Co2 N6 179.42(10) . . ?
N5 Co2 Co3 89.80(7) . . ?
N7 Co2 Co3 89.72(7) . . ?
N8 Co2 Co3 90.45(8) . . ?
N6 Co2 Co3 89.17(7) . . ?
N5 Co2 Co1 90.68(7) . . ?
N7 Co2 Co1 89.79(7) . . ?
N8 Co2 Co1 90.92(8) . . ?
N6 Co2 Co1 89.47(8) . . ?
Co3 Co2 Co1 178.55(2) . . ?
N12 Co3 N11 87.65(11) . . ?
N12 Co3 N10 169.07(10) . . ?
N11 Co3 N10 90.88(11) . . ?
N12 Co3 N9 89.59(11) . . ?
N11 Co3 N9 169.88(10) . . ?
N10 Co3 N9 89.98(11) . . ?
N12 Co3 Co2 83.70(7) . . ?
N11 Co3 Co2 85.54(7) . . ?
N10 Co3 Co2 85.38(7) . . ?
N9 Co3 Co2 84.48(7) . . ?
N12 Co3 Cl2 95.55(8) . . ?
N11 Co3 Cl2 96.33(8) . . ?
N10 Co3 Cl2 95.38(8) . . ?
N9 Co3 Cl2 93.63(8) . . ?
Co2 Co3 Cl2 177.96(3) . . ?
C2S C1S H1SA 109.5 . . ?
C2S C1S H1SB 109.5 . . ?
H1SA C1S H1SB 109.5 . . ?
C2S C1S H1SC 109.5 . . ?
H1SA C1S H1SC 109.5 . . ?
H1SB C1S H1SC 109.5 . . ?
O1S C2S C1S 101.6(4) . . ?
O1S C2S H2SA 111.4 . . ?
C1S C2S H2SA 111.4 . . ?
O1S C2S H2SB 111.4 . . ?
C1S C2S H2SB 111.4 . . ?
H2SA C2S H2SB 109.3 . . ?
C3S O1S C2S 108.8(5) . . ?
O1S C3S C4S 108.5(4) . . ?
O1S C3S H3SA 110.0 . . ?
C4S C3S H3SA 110.0 . . ?
O1S C3S H3SB 110.0 . . ?
C4S C3S H3SB 110.0 . . ?
H3SA C3S H3SB 108.4 . . ?
C3S C4S H4SA 109.5 . . ?
C3S C4S H4SB 109.5 . . ?
H4SA C4S H4SB 109.5 . . ?
C3S C4S H4SC 109.5 . . ?
H4SA C4S H4SC 109.5 . . ?
H4SB C4S H4SC 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
N1 C1 C2 C3 -0.5(6) . . . . ?
C1 C2 C3 C4 -0.9(6) . . . . ?
C2 C3 C4 C5 2.0(5) . . . . ?
C3 C4 C5 N1 -1.6(5) . . . . ?
C3 C4 C5 N5 -176.6(3) . . . . ?
N9 C6 C7 C8 1.7(5) . . . . ?
N5 C6 C7 C8 -173.3(3) . . . . ?
C6 C7 C8 C9 0.7(6) . . . . ?
C7 C8 C9 C10 -0.9(6) . . . . ?
C8 C9 C10 N9 -1.4(6) . . . . ?
N2 C11 C12 C13 -4.3(7) . . . . ?
C11 C12 C13 C14 1.7(7) . . . . ?
C12 C13 C14 C15 2.1(7) . . . . ?
C13 C14 C15 N2 -3.6(6) . . . . ?
C13 C14 C15 N6 179.0(4) . . . . ?
N10 C16 C17 C18 -0.9(5) . . . . ?
N6 C16 C17 C18 -174.3(3) . . . . ?
C16 C17 C18 C19 -0.8(6) . . . . ?
C17 C18 C19 C20 1.7(6) . . . . ?
C18 C19 C20 N10 -0.9(6) . . . . ?
N3 C21 C22 C23 -2.1(6) . . . . ?
C21 C22 C23 C24 0.3(6) . . . . ?
C22 C23 C24 C25 1.9(6) . . . . ?
C23 C24 C25 N3 -2.5(5) . . . . ?
C23 C24 C25 N7 -176.4(3) . . . . ?
N11 C26 C27 C28 -1.8(5) . . . . ?
N7 C26 C27 C28 -177.6(3) . . . . ?
C26 C27 C28 C29 1.9(6) . . . . ?
C27 C28 C29 C30 0.1(6) . . . . ?
C28 C29 C30 N11 -2.4(6) . . . . ?
N4 C31 C32 C33 -1.8(7) . . . . ?
C31 C32 C33 C34 -2.3(7) . . . . ?
C32 C33 C34 C35 4.2(6) . . . . ?
C33 C34 C35 N4 -2.3(5) . . . . ?
C33 C34 C35 N8 -178.1(4) . . . . ?
N12 C36 C37 C38 3.0(5) . . . . ?
N8 C36 C37 C38 -171.0(3) . . . . ?
C36 C37 C38 C39 0.8(6) . . . . ?
C37 C38 C39 C40 -2.4(6) . . . . ?
C38 C39 C40 N12 0.3(6) . . . . ?
C2 C1 N1 C5 0.9(5) . . . . ?
C2 C1 N1 Co1 177.2(3) . . . . ?
N5 C5 N1 C1 175.6(3) . . . . ?
C4 C5 N1 C1 0.2(4) . . . . ?
N5 C5 N1 Co1 -0.5(4) . . . . ?
C4 C5 N1 Co1 -176.0(2) . . . . ?
C12 C11 N2 C15 2.8(6) . . . . ?
C12 C11 N2 Co1 -173.2(3) . . . . ?
N6 C15 N2 C11 178.8(3) . . . . ?
C14 C15 N2 C11 1.2(5) . . . . ?
N6 C15 N2 Co1 -5.3(4) . . . . ?
C14 C15 N2 Co1 177.2(3) . . . . ?
C22 C21 N3 C25 1.5(5) . . . . ?
C22 C21 N3 Co1 177.4(3) . . . . ?
N7 C25 N3 C21 175.2(3) . . . . ?
C24 C25 N3 C21 0.8(4) . . . . ?
N7 C25 N3 Co1 -0.7(4) . . . . ?
C24 C25 N3 Co1 -175.1(2) . . . . ?
C32 C31 N4 C35 3.8(5) . . . . ?
C32 C31 N4 Co1 -174.9(3) . . . . ?
N8 C35 N4 C31 174.6(3) . . . . ?
C34 C35 N4 C31 -1.7(5) . . . . ?
N8 C35 N4 Co1 -6.9(4) . . . . ?
C34 C35 N4 Co1 176.9(2) . . . . ?
N1 C5 N5 C6 155.9(3) . . . . ?
C4 C5 N5 C6 -28.9(5) . . . . ?
N1 C5 N5 Co2 -26.1(3) . . . . ?
C4 C5 N5 Co2 149.1(3) . . . . ?
N9 C6 N5 C5 156.8(3) . . . . ?
C7 C6 N5 C5 -28.0(5) . . . . ?
N9 C6 N5 Co2 -21.1(3) . . . . ?
C7 C6 N5 Co2 154.1(3) . . . . ?
N10 C16 N6 C15 157.0(3) . . . . ?
C17 C16 N6 C15 -29.3(5) . . . . ?
N10 C16 N6 Co2 -30.7(3) . . . . ?
C17 C16 N6 Co2 142.9(3) . . . . ?
N2 C15 N6 C16 152.2(3) . . . . ?
C14 C15 N6 C16 -30.4(5) . . . . ?
N2 C15 N6 Co2 -19.8(4) . . . . ?
C14 C15 N6 Co2 157.6(3) . . . . ?
N11 C26 N7 C25 156.6(3) . . . . ?
C27 C26 N7 C25 -27.5(5) . . . . ?
N11 C26 N7 Co2 -18.8(4) . . . . ?
C27 C26 N7 Co2 157.2(3) . . . . ?
N3 C25 N7 C26 157.0(3) . . . . ?
C24 C25 N7 C26 -28.9(5) . . . . ?
N3 C25 N7 Co2 -27.6(3) . . . . ?
C24 C25 N7 Co2 146.4(3) . . . . ?
N12 C36 N8 C35 161.5(3) . . . . ?
C37 C36 N8 C35 -24.2(5) . . . . ?
N12 C36 N8 Co2 -21.7(3) . . . . ?
C37 C36 N8 Co2 152.6(3) . . . . ?
N4 C35 N8 C36 156.5(3) . . . . ?
C34 C35 N8 C36 -27.5(5) . . . . ?
N4 C35 N8 Co2 -20.3(4) . . . . ?
C34 C35 N8 Co2 155.8(3) . . . . ?
C9 C10 N9 C6 3.8(5) . . . . ?
C9 C10 N9 Co3 -176.5(3) . . . . ?
N5 C6 N9 C10 171.6(3) . . . . ?
C7 C6 N9 C10 -3.8(5) . . . . ?
N5 C6 N9 Co3 -8.1(4) . . . . ?
C7 C6 N9 Co3 176.5(2) . . . . ?
C19 C20 N10 C16 -0.8(5) . . . . ?
C19 C20 N10 Co3 171.9(3) . . . . ?
N6 C16 N10 C20 175.6(3) . . . . ?
C17 C16 N10 C20 1.7(4) . . . . ?
N6 C16 N10 Co3 3.0(3) . . . . ?
C17 C16 N10 Co3 -171.0(2) . . . . ?
C29 C30 N11 C26 2.5(5) . . . . ?
C29 C30 N11 Co3 -173.7(3) . . . . ?
N7 C26 N11 C30 175.8(3) . . . . ?
C27 C26 N11 C30 -0.3(5) . . . . ?
N7 C26 N11 Co3 -8.0(4) . . . . ?
C27 C26 N11 Co3 175.9(2) . . . . ?
C39 C40 N12 C36 3.5(5) . . . . ?
C39 C40 N12 Co3 -179.3(3) . . . . ?
N8 C36 N12 C40 169.6(3) . . . . ?
C37 C36 N12 C40 -5.1(4) . . . . ?
N8 C36 N12 Co3 -7.5(4) . . . . ?
C37 C36 N12 Co3 177.8(2) . . . . ?
C1S C2S O1S C3S -171.7(4) . . . . ?
C2S O1S C3S C4S 176.4(4) . . . . ?

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
C1 H1 Cl1 0.93 2.71 3.352(4) 126.9 .
C2 H2 O1S 0.93 2.62 3.379(5) 138.9 .
C10 H10 Cl2 0.93 2.62 3.213(4) 121.7 .
C11 H11 Cl1 0.93 2.65 3.282(4) 125.4 .
C20 H20 Cl2 0.93 2.62 3.261(5) 126.9 .
C21 H21 Cl1 0.93 2.67 3.303(4) 126.1 .
C29 H29 Cl2 0.93 2.87 3.767(3) 161.2 3_766
C30 H30 Cl2 0.93 2.66 3.268(4) 123.2 .
C31 H31 Cl1 0.93 2.66 3.280(4) 124.5 .
C32 H32 Cl1 0.93 2.83 3.743(4) 167.7 3_667
C40 H40 Cl2 0.93 2.67 3.260(4) 121.8 .

_refine_diff_density_max         0.763
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.065

####################################################################### 
# 
# 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_3-et2o-350k
_database_code_depnum_ccdc_archive 'CCDC 1877181'
_audit_update_record             
;
2018-11-05 deposited with the CCDC.
2018-11-07 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         'C40 H32 Br2 Co3 N12, C4 H10 O'
_chemical_formula_sum            'C44 H42 Br2 Co3 N12 O'
_chemical_formula_weight         1091.50

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   16.1914(13)
_cell_length_b                   15.9355(12)
_cell_length_c                   17.2266(14)
_cell_angle_alpha                90
_cell_angle_beta                 99.293(4)
_cell_angle_gamma                90
_cell_volume                     4386.4(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    350(2)
_cell_measurement_reflns_used    9695
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      26.72

_exptl_crystal_description       Block
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_F_000             2196
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.544
_exptl_crystal_size_mid          0.403
_exptl_crystal_size_min          0.238
_exptl_absorpt_coefficient_mu    2.994
_shelx_estimated_absorpt_T_min   0.293
_shelx_estimated_absorpt_T_max   0.536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3767
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SADABS (Bruker, 2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      350(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            137516
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_av_R_equivalents  0.0576
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.752
_diffrn_reflns_theta_max         27.528
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             10059
_reflns_number_gt                7734
_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       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_structure_solution    'SHELXS2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_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)+(0.0758P)²+12.1275P] 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_number_reflns         10059
_refine_ls_number_parameters     561
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0491
_refine_ls_wR_factor_ref         0.1579
_refine_ls_wR_factor_gt          0.1389
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.002
_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
C1 C 0.4788(3) 0.4763(3) 0.7252(3) 0.0477(11) Uani 1 1 d . . . . .
H1 H 0.4588 0.5248 0.7458 0.057 Uiso 1 1 calc R U . . .
C1S C 0.1684(5) 0.4530(6) 0.6154(5) 0.104(3) Uani 1 1 d . . . . .
H1SA H 0.1339 0.4959 0.6326 0.156 Uiso 1 1 calc R U . . .
H1SB H 0.1371 0.4228 0.5722 0.156 Uiso 1 1 calc R U . . .
H1SC H 0.2165 0.4783 0.5989 0.156 Uiso 1 1 calc R U . . .
C2 C 0.4228(3) 0.4250(4) 0.6806(3) 0.0559(13) Uani 1 1 d . . . . .
H2 H 0.3660 0.4376 0.6722 0.067 Uiso 1 1 calc R U . . .
C2S C 0.1959(4) 0.3944(4) 0.6810(4) 0.0669(16) Uani 1 1 d . . . . .
H2SA H 0.1482 0.3640 0.6941 0.080 Uiso 1 1 calc R U . . .
H2SB H 0.2352 0.3540 0.6657 0.080 Uiso 1 1 calc R U . . .
C3 C 0.4522(3) 0.3542(3) 0.6484(3) 0.0509(12) Uani 1 1 d . . . . .
H3 H 0.4151 0.3184 0.6176 0.061 Uiso 1 1 calc R U . . .
C3S C 0.2717(4) 0.3889(4) 0.8095(4) 0.0675(16) Uani 1 1 d . . . . .
H3SA H 0.3124 0.3520 0.7917 0.081 Uiso 1 1 calc R U . . .
H3SB H 0.2292 0.3547 0.8278 0.081 Uiso 1 1 calc R U . . .
C4 C 0.5363(3) 0.3365(3) 0.6618(3) 0.0422(10) Uani 1 1 d . . . . .
H4 H 0.5565 0.2892 0.6394 0.051 Uiso 1 1 calc R U . . .
C4S C 0.3135(5) 0.4430(5) 0.8748(4) 0.088(2) Uani 1 1 d . . . . .
H4SA H 0.3594 0.4722 0.8580 0.132 Uiso 1 1 calc R U . . .
H4SB H 0.3340 0.4087 0.9196 0.132 Uiso 1 1 calc R U . . .
H4SC H 0.2740 0.4830 0.8887 0.132 Uiso 1 1 calc R U . . .
C5 C 0.5917(2) 0.3901(2) 0.7093(2) 0.0306(8) Uani 1 1 d . . . . .
C6 C 0.7159(3) 0.3053(2) 0.7221(2) 0.0313(8) Uani 1 1 d . . . . .
C7 C 0.6825(3) 0.2278(3) 0.7411(3) 0.0461(11) Uani 1 1 d . . . . .
H7 H 0.6274 0.2250 0.7498 0.055 Uiso 1 1 calc R U . . .
C8 C 0.7298(4) 0.1574(3) 0.7467(3) 0.0558(13) Uani 1 1 d . . . . .
H8 H 0.7068 0.1059 0.7572 0.067 Uiso 1 1 calc R U . . .
C9 C 0.8128(4) 0.1626(3) 0.7366(3) 0.0600(14) Uani 1 1 d . . . . .
H9 H 0.8472 0.1155 0.7429 0.072 Uiso 1 1 calc R U . . .
C10 C 0.8432(3) 0.2392(3) 0.7170(3) 0.0470(11) Uani 1 1 d . . . . .
H10 H 0.8988 0.2427 0.7100 0.056 Uiso 1 1 calc R U . . .
C11 C 0.5783(3) 0.6946(3) 0.7095(3) 0.0469(11) Uani 1 1 d . . . . .
H11 H 0.5629 0.7116 0.7567 0.056 Uiso 1 1 calc R U . . .
C12 C 0.5570(3) 0.7447(3) 0.6453(3) 0.0557(13) Uani 1 1 d . . . . .
H12 H 0.5251 0.7929 0.6481 0.067 Uiso 1 1 calc R U . . .
C13 C 0.5835(3) 0.7225(3) 0.5761(3) 0.0564(13) Uani 1 1 d . . . . .
H13 H 0.5708 0.7562 0.5317 0.068 Uiso 1 1 calc R U . . .
C14 C 0.6285(3) 0.6509(3) 0.5734(3) 0.0467(11) Uani 1 1 d . . . . .
H14 H 0.6483 0.6364 0.5275 0.056 Uiso 1 1 calc R U . . .
C15 C 0.6452(2) 0.5984(2) 0.6402(2) 0.0303(8) Uani 1 1 d . . . . .
C16 C 0.6880(2) 0.4749(2) 0.5773(2) 0.0313(8) Uani 1 1 d . . . . .
C17 C 0.6205(3) 0.4708(3) 0.5148(3) 0.0481(11) Uani 1 1 d . . . . .
H17 H 0.5754 0.5072 0.5137 0.058 Uiso 1 1 calc R U . . .
C18 C 0.6206(4) 0.4135(3) 0.4554(3) 0.0579(14) Uani 1 1 d . . . . .
H18 H 0.5752 0.4096 0.4149 0.069 Uiso 1 1 calc R U . . .
C19 C 0.6890(4) 0.3621(3) 0.4568(3) 0.0591(14) Uani 1 1 d . . . . .
H19 H 0.6916 0.3240 0.4164 0.071 Uiso 1 1 calc R U . . .
C20 C 0.7532(3) 0.3681(3) 0.5190(3) 0.0465(11) Uani 1 1 d . . . . .
H20 H 0.7991 0.3329 0.5197 0.056 Uiso 1 1 calc R U . . .
C21 C 0.7370(3) 0.6538(3) 0.9267(3) 0.0470(11) Uani 1 1 d . . . . .
H21 H 0.6888 0.6476 0.9491 0.056 Uiso 1 1 calc R U . . .
C22 C 0.8005(4) 0.6998(4) 0.9662(3) 0.0562(13) Uani 1 1 d . . . . .
H22 H 0.7950 0.7262 1.0132 0.067 Uiso 1 1 calc R U . . .
C23 C 0.8735(3) 0.7067(3) 0.9352(3) 0.0514(12) Uani 1 1 d . . . . .
H23 H 0.9184 0.7374 0.9614 0.062 Uiso 1 1 calc R U . . .
C24 C 0.8794(3) 0.6675(3) 0.8648(3) 0.0410(10) Uani 1 1 d . . . . .
H24 H 0.9289 0.6705 0.8441 0.049 Uiso 1 1 calc R U . . .
C25 C 0.8105(2) 0.6232(2) 0.8246(2) 0.0289(8) Uani 1 1 d . . . . .
C26 C 0.8622(2) 0.5989(2) 0.7032(2) 0.0277(7) Uani 1 1 d . . . . .
C27 C 0.8927(3) 0.6798(3) 0.6919(3) 0.0416(10) Uani 1 1 d . . . . .
H27 H 0.8793 0.7241 0.7228 0.050 Uiso 1 1 calc R U . . .
C28 C 0.9415(3) 0.6939(3) 0.6361(3) 0.0530(12) Uani 1 1 d . . . . .
H28 H 0.9637 0.7469 0.6304 0.064 Uiso 1 1 calc R U . . .
C29 C 0.9582(3) 0.6287(3) 0.5878(3) 0.0530(12) Uani 1 1 d . . . . .
H29 H 0.9917 0.6369 0.5494 0.064 Uiso 1 1 calc R U . . .
C30 C 0.9241(3) 0.5517(3) 0.5981(3) 0.0429(10) Uani 1 1 d . . . . .
H30 H 0.9326 0.5086 0.5639 0.051 Uiso 1 1 calc R U . . .
C31 C 0.6240(3) 0.4321(3) 0.9375(3) 0.0509(12) Uani 1 1 d . . . . .
H31 H 0.5705 0.4552 0.9295 0.061 Uiso 1 1 calc R U . . .
C32 C 0.6456(4) 0.3780(3) 0.9997(3) 0.0647(16) Uani 1 1 d . . . . .
H32 H 0.6084 0.3662 1.0341 0.078 Uiso 1 1 calc R U . . .
C33 C 0.7232(4) 0.3420(3) 1.0094(3) 0.0622(15) Uani 1 1 d . . . . .
H33 H 0.7400 0.3065 1.0519 0.075 Uiso 1 1 calc R U . . .
C34 C 0.7764(4) 0.3578(3) 0.9568(3) 0.0514(12) Uani 1 1 d . . . . .
H34 H 0.8278 0.3306 0.9618 0.062 Uiso 1 1 calc R U . . .
C35 C 0.7531(3) 0.4155(2) 0.8949(2) 0.0325(8) Uani 1 1 d . . . . .
C36 C 0.8849(3) 0.4278(2) 0.8467(2) 0.0325(8) Uani 1 1 d . . . . .
C37 C 0.9406(3) 0.4295(3) 0.9189(3) 0.0493(11) Uani 1 1 d . . . . .
H37 H 0.9198 0.4280 0.9661 0.059 Uiso 1 1 calc R U . . .
C38 C 1.0250(3) 0.4335(4) 0.9194(3) 0.0594(14) Uani 1 1 d . . . . .
H38 H 1.0615 0.4340 0.9670 0.071 Uiso 1 1 calc R U . . .
C39 C 1.0560(3) 0.4369(4) 0.8496(4) 0.0618(15) Uani 1 1 d . . . . .
H39 H 1.1131 0.4423 0.8492 0.074 Uiso 1 1 calc R U . . .
C40 C 1.0004(3) 0.4321(3) 0.7808(3) 0.0476(11) Uani 1 1 d . . . . .
H40 H 1.0211 0.4338 0.7335 0.057 Uiso 1 1 calc R U . . .
N1 N 0.5619(2) 0.4605(2) 0.7409(2) 0.0342(7) Uani 1 1 d . . . . .
N2 N 0.6204(2) 0.6217(2) 0.7084(2) 0.0333(7) Uani 1 1 d . . . . .
N3 N 0.7393(2) 0.6160(2) 0.85641(19) 0.0324(7) Uani 1 1 d . . . . .
N4 N 0.6770(2) 0.4535(2) 0.8871(2) 0.0357(7) Uani 1 1 d . . . . .
N5 N 0.67627(19) 0.38107(19) 0.72234(19) 0.0291(7) Uani 1 1 d . . . . .
N6 N 0.68881(19) 0.5246(2) 0.64236(18) 0.0292(7) Uani 1 1 d . . . . .
N7 N 0.81145(19) 0.57868(19) 0.75668(18) 0.0273(6) Uani 1 1 d . . . . .
N8 N 0.8000(2) 0.4347(2) 0.83764(19) 0.0310(7) Uani 1 1 d . . . . .
N9 N 0.7961(2) 0.3090(2) 0.70771(19) 0.0329(7) Uani 1 1 d . . . . .
N10 N 0.7534(2) 0.4222(2) 0.57908(19) 0.0323(7) Uani 1 1 d . . . . .
N11 N 0.87860(19) 0.5353(2) 0.65540(19) 0.0306(7) Uani 1 1 d . . . . .
N12 N 0.9166(2) 0.4250(2) 0.7784(2) 0.0337(7) Uani 1 1 d . . . . .
O1S O 0.2345(2) 0.4408(2) 0.7468(2) 0.0585(9) Uani 1 1 d . . . . .
Co1 Co 0.64056(3) 0.54452(3) 0.80465(3) 0.03249(14) Uani 1 1 d . . . . .
Co2 Co 0.74404(3) 0.47990(3) 0.74036(3) 0.02362(12) Uani 1 1 d . . . . .
Co3 Co 0.84302(3) 0.41766(3) 0.67436(3) 0.02889(13) Uani 1 1 d . . . . .
Br1 Br 0.52952(4) 0.61400(4) 0.87839(4) 0.06191(17) Uani 1 1 d . . . . .
Br2 Br 0.95184(4) 0.34147(4) 0.60355(4) 0.06466(18) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.353(5) . ?
C1 C2 1.361(8) . ?
C1 H1 0.9300 . ?
C1S C2S 1.478(10) . ?
C1S H1SA 0.9600 . ?
C1S H1SB 0.9600 . ?
C1S H1SC 0.9600 . ?
C2 C3 1.375(8) . ?
C2 H2 0.9300 . ?
C2S O1S 1.412(7) . ?
C2S H2SA 0.9700 . ?
C2S H2SB 0.9700 . ?
C3 C4 1.374(7) . ?
C3 H3 0.9300 . ?
C3S O1S 1.416(7) . ?
C3S C4S 1.489(10) . ?
C3S H3SA 0.9700 . ?
C3S H3SB 0.9700 . ?
C4 C5 1.403(6) . ?
C4 H4 0.9300 . ?
C4S H4SA 0.9600 . ?
C4S H4SB 0.9600 . ?
C4S H4SC 0.9600 . ?
C5 N5 1.359(5) . ?
C5 N1 1.367(5) . ?
C6 N9 1.362(5) . ?
C6 N5 1.368(5) . ?
C6 C7 1.407(6) . ?
C7 C8 1.354(7) . ?
C7 H7 0.9300 . ?
C8 C9 1.384(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.379(7) . ?
C9 H9 0.9300 . ?
C10 N9 1.343(5) . ?
C10 H10 0.9300 . ?
C11 N2 1.349(5) . ?
C11 C12 1.363(7) . ?
C11 H11 0.9300 . ?
C12 C13 1.376(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.359(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.413(6) . ?
C14 H14 0.9300 . ?
C15 N2 1.354(5) . ?
C15 N6 1.369(5) . ?
C16 N10 1.348(5) . ?
C16 N6 1.370(5) . ?
C16 C17 1.407(6) . ?
C17 C18 1.371(7) . ?
C17 H17 0.9300 . ?
C18 C19 1.375(8) . ?
C18 H18 0.9300 . ?
C19 C20 1.370(7) . ?
C19 H19 0.9300 . ?
C20 N10 1.347(5) . ?
C20 H20 0.9300 . ?
C21 C22 1.354(7) . ?
C21 N3 1.358(5) . ?
C21 H21 0.9300 . ?
C22 C23 1.378(7) . ?
C22 H22 0.9300 . ?
C23 C24 1.380(6) . ?
C23 H23 0.9300 . ?
C24 C25 1.405(6) . ?
C24 H24 0.9300 . ?
C25 N3 1.360(5) . ?
C25 N7 1.370(5) . ?
C26 N11 1.359(5) . ?
C26 N7 1.368(5) . ?
C26 C27 1.406(6) . ?
C27 C28 1.358(6) . ?
C27 H27 0.9300 . ?
C28 C29 1.385(7) . ?
C28 H28 0.9300 . ?
C29 C30 1.368(7) . ?
C29 H29 0.9300 . ?
C30 N11 1.349(5) . ?
C30 H30 0.9300 . ?
C31 N4 1.360(5) . ?
C31 C32 1.376(8) . ?
C31 H31 0.9300 . ?
C32 C33 1.368(9) . ?
C32 H32 0.9300 . ?
C33 C34 1.372(7) . ?
C33 H33 0.9300 . ?
C34 C35 1.412(6) . ?
C34 H34 0.9300 . ?
C35 N4 1.359(5) . ?
C35 N8 1.373(5) . ?
C36 N12 1.358(5) . ?
C36 N8 1.364(5) . ?
C36 C37 1.414(6) . ?
C37 C38 1.366(7) . ?
C37 H37 0.9300 . ?
C38 C39 1.377(8) . ?
C38 H38 0.9300 . ?
C39 C40 1.370(7) . ?
C39 H39 0.9300 . ?
C40 N12 1.355(5) . ?
C40 H40 0.9300 . ?
N1 Co1 2.042(4) . ?
N2 Co1 2.047(3) . ?
N3 Co1 2.046(3) . ?
N4 Co1 2.049(4) . ?
N5 Co2 1.916(3) . ?
N6 Co2 1.915(3) . ?
N7 Co2 1.910(3) . ?
N8 Co2 1.912(3) . ?
N9 Co3 2.011(3) . ?
N10 Co3 2.009(3) . ?
N11 Co3 2.003(3) . ?
N12 Co3 1.989(3) . ?
Co1 Co2 2.3862(7) . ?
Co1 Br1 2.6096(7) . ?
Co2 Co3 2.3308(7) . ?
Co3 Br2 2.6002(7) . ?

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
N1 C1 C2 123.4(5) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C2S C1S H1SA 109.5 . . ?
C2S C1S H1SB 109.5 . . ?
H1SA C1S H1SB 109.5 . . ?
C2S C1S H1SC 109.5 . . ?
H1SA C1S H1SC 109.5 . . ?
H1SB C1S H1SC 109.5 . . ?
C1 C2 C3 118.6(4) . . ?
C1 C2 H2 120.7 . . ?
C3 C2 H2 120.7 . . ?
O1S C2S C1S 108.8(6) . . ?
O1S C2S H2SA 109.9 . . ?
C1S C2S H2SA 109.9 . . ?
O1S C2S H2SB 109.9 . . ?
C1S C2S H2SB 109.9 . . ?
H2SA C2S H2SB 108.3 . . ?
C4 C3 C2 119.9(5) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
O1S C3S C4S 108.9(5) . . ?
O1S C3S H3SA 109.9 . . ?
C4S C3S H3SA 109.9 . . ?
O1S C3S H3SB 109.9 . . ?
C4S C3S H3SB 109.9 . . ?
H3SA C3S H3SB 108.3 . . ?
C3 C4 C5 119.7(5) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C3S C4S H4SA 109.5 . . ?
C3S C4S H4SB 109.5 . . ?
H4SA C4S H4SB 109.5 . . ?
C3S C4S H4SC 109.5 . . ?
H4SA C4S H4SC 109.5 . . ?
H4SB C4S H4SC 109.5 . . ?
N5 C5 N1 115.6(3) . . ?
N5 C5 C4 124.3(4) . . ?
N1 C5 C4 119.9(4) . . ?
N9 C6 N5 115.0(3) . . ?
N9 C6 C7 119.6(4) . . ?
N5 C6 C7 125.2(4) . . ?
C8 C7 C6 120.7(5) . . ?
C8 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
C7 C8 C9 119.4(5) . . ?
C7 C8 H8 120.3 . . ?
C9 C8 H8 120.3 . . ?
C10 C9 C8 118.4(4) . . ?
C10 C9 H9 120.8 . . ?
C8 C9 H9 120.8 . . ?
N9 C10 C9 123.0(5) . . ?
N9 C10 H10 118.5 . . ?
C9 C10 H10 118.5 . . ?
N2 C11 C12 123.8(5) . . ?
N2 C11 H11 118.1 . . ?
C12 C11 H11 118.1 . . ?
C11 C12 C13 118.5(4) . . ?
C11 C12 H12 120.7 . . ?
C13 C12 H12 120.7 . . ?
C14 C13 C12 119.3(5) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C13 C14 C15 120.2(5) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
N2 C15 N6 115.8(3) . . ?
N2 C15 C14 120.0(4) . . ?
N6 C15 C14 124.2(4) . . ?
N10 C16 N6 116.0(3) . . ?
N10 C16 C17 119.9(4) . . ?
N6 C16 C17 123.8(4) . . ?
C18 C17 C16 120.6(5) . . ?
C18 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
C17 C18 C19 118.7(5) . . ?
C17 C18 H18 120.6 . . ?
C19 C18 H18 120.6 . . ?
C20 C19 C18 118.7(4) . . ?
C20 C19 H19 120.6 . . ?
C18 C19 H19 120.6 . . ?
N10 C20 C19 123.6(5) . . ?
N10 C20 H20 118.2 . . ?
C19 C20 H20 118.2 . . ?
C22 C21 N3 124.0(4) . . ?
C22 C21 H21 118.0 . . ?
N3 C21 H21 118.0 . . ?
C21 C22 C23 118.6(4) . . ?
C21 C22 H22 120.7 . . ?
C23 C22 H22 120.7 . . ?
C22 C23 C24 119.3(4) . . ?
C22 C23 H23 120.3 . . ?
C24 C23 H23 120.3 . . ?
C23 C24 C25 119.9(4) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
N3 C25 N7 115.3(3) . . ?
N3 C25 C24 120.0(4) . . ?
N7 C25 C24 124.3(4) . . ?
N11 C26 N7 115.5(3) . . ?
N11 C26 C27 119.6(3) . . ?
N7 C26 C27 124.8(4) . . ?
C28 C27 C26 120.4(4) . . ?
C28 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
C27 C28 C29 119.6(4) . . ?
C27 C28 H28 120.2 . . ?
C29 C28 H28 120.2 . . ?
C30 C29 C28 118.2(4) . . ?
C30 C29 H29 120.9 . . ?
C28 C29 H29 120.9 . . ?
N11 C30 C29 123.3(4) . . ?
N11 C30 H30 118.4 . . ?
C29 C30 H30 118.4 . . ?
N4 C31 C32 123.1(5) . . ?
N4 C31 H31 118.4 . . ?
C32 C31 H31 118.4 . . ?
C33 C32 C31 118.2(5) . . ?
C33 C32 H32 120.9 . . ?
C31 C32 H32 120.9 . . ?
C32 C33 C34 120.3(5) . . ?
C32 C33 H33 119.9 . . ?
C34 C33 H33 119.9 . . ?
C33 C34 C35 119.9(5) . . ?
C33 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
N4 C35 N8 115.3(3) . . ?
N4 C35 C34 119.5(4) . . ?
N8 C35 C34 125.1(4) . . ?
N12 C36 N8 114.8(3) . . ?
N12 C36 C37 119.1(4) . . ?
N8 C36 C37 125.9(4) . . ?
C38 C37 C36 120.1(5) . . ?
C38 C37 H37 119.9 . . ?
C36 C37 H37 119.9 . . ?
C37 C38 C39 120.1(5) . . ?
C37 C38 H38 120.0 . . ?
C39 C38 H38 120.0 . . ?
C40 C39 C38 118.2(5) . . ?
C40 C39 H39 120.9 . . ?
C38 C39 H39 120.9 . . ?
N12 C40 C39 123.0(5) . . ?
N12 C40 H40 118.5 . . ?
C39 C40 H40 118.5 . . ?
C1 N1 C5 118.5(4) . . ?
C1 N1 Co1 119.9(3) . . ?
C5 N1 Co1 121.5(3) . . ?
C11 N2 C15 118.0(4) . . ?
C11 N2 Co1 121.4(3) . . ?
C15 N2 Co1 120.5(3) . . ?
C21 N3 C25 118.0(4) . . ?
C21 N3 Co1 120.2(3) . . ?
C25 N3 Co1 121.6(3) . . ?
C35 N4 C31 118.8(4) . . ?
C35 N4 Co1 122.6(3) . . ?
C31 N4 Co1 118.6(3) . . ?
C5 N5 C6 123.6(3) . . ?
C5 N5 Co2 118.4(3) . . ?
C6 N5 Co2 118.0(3) . . ?
C15 N6 C16 122.5(3) . . ?
C15 N6 Co2 120.6(3) . . ?
C16 N6 Co2 116.6(3) . . ?
C26 N7 C25 122.9(3) . . ?
C26 N7 Co2 119.1(3) . . ?
C25 N7 Co2 117.9(2) . . ?
C36 N8 C35 124.4(3) . . ?
C36 N8 Co2 117.2(3) . . ?
C35 N8 Co2 118.4(3) . . ?
C10 N9 C6 118.8(4) . . ?
C10 N9 Co3 120.9(3) . . ?
C6 N9 Co3 120.3(3) . . ?
C20 N10 C16 118.5(4) . . ?
C20 N10 Co3 121.1(3) . . ?
C16 N10 Co3 120.1(3) . . ?
C30 N11 C26 118.8(4) . . ?
C30 N11 Co3 120.4(3) . . ?
C26 N11 Co3 120.6(2) . . ?
C40 N12 C36 119.2(4) . . ?
C40 N12 Co3 118.9(3) . . ?
C36 N12 Co3 121.8(3) . . ?
C2S O1S C3S 112.6(5) . . ?
N1 Co1 N3 167.14(13) . . ?
N1 Co1 N2 87.40(14) . . ?
N3 Co1 N2 91.68(13) . . ?
N1 Co1 N4 89.60(14) . . ?
N3 Co1 N4 88.56(14) . . ?
N2 Co1 N4 167.58(13) . . ?
N1 Co1 Co2 83.73(9) . . ?
N3 Co1 Co2 83.40(9) . . ?
N2 Co1 Co2 85.13(9) . . ?
N4 Co1 Co2 82.56(9) . . ?
N1 Co1 Br1 96.97(9) . . ?
N3 Co1 Br1 95.88(9) . . ?
N2 Co1 Br1 96.17(9) . . ?
N4 Co1 Br1 96.16(10) . . ?
Co2 Co1 Br1 178.54(3) . . ?
N7 Co2 N8 90.17(14) . . ?
N7 Co2 N6 89.87(14) . . ?
N8 Co2 N6 179.42(14) . . ?
N7 Co2 N5 179.15(13) . . ?
N8 Co2 N5 90.58(14) . . ?
N6 Co2 N5 89.38(14) . . ?
N7 Co2 Co3 90.05(9) . . ?
N8 Co2 Co3 90.10(10) . . ?
N6 Co2 Co3 89.32(10) . . ?
N5 Co2 Co3 89.55(9) . . ?
N7 Co2 Co1 90.19(9) . . ?
N8 Co2 Co1 91.40(10) . . ?
N6 Co2 Co1 89.19(10) . . ?
N5 Co2 Co1 90.19(9) . . ?
Co3 Co2 Co1 178.49(3) . . ?
N12 Co3 N11 86.89(14) . . ?
N12 Co3 N10 169.34(13) . . ?
N11 Co3 N10 91.24(13) . . ?
N12 Co3 N9 89.55(14) . . ?
N11 Co3 N9 169.69(13) . . ?
N10 Co3 N9 90.48(14) . . ?
N12 Co3 Co2 83.95(10) . . ?
N11 Co3 Co2 85.41(9) . . ?
N10 Co3 Co2 85.44(9) . . ?
N9 Co3 Co2 84.60(9) . . ?
N12 Co3 Br2 95.58(10) . . ?
N11 Co3 Br2 97.23(9) . . ?
N10 Co3 Br2 95.06(10) . . ?
N9 Co3 Br2 92.74(9) . . ?
Co2 Co3 Br2 177.30(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
N1 C1 C2 C3 -1.5(8) . . . . ?
C1 C2 C3 C4 0.3(7) . . . . ?
C2 C3 C4 C5 1.0(7) . . . . ?
C3 C4 C5 N5 -175.9(4) . . . . ?
C3 C4 C5 N1 -1.2(6) . . . . ?
N9 C6 C7 C8 1.3(7) . . . . ?
N5 C6 C7 C8 -173.3(5) . . . . ?
C6 C7 C8 C9 2.5(8) . . . . ?
C7 C8 C9 C10 -3.3(8) . . . . ?
C8 C9 C10 N9 0.4(8) . . . . ?
N2 C11 C12 C13 -3.6(8) . . . . ?
C11 C12 C13 C14 1.3(8) . . . . ?
C12 C13 C14 C15 2.2(8) . . . . ?
C13 C14 C15 N2 -3.7(7) . . . . ?
C13 C14 C15 N6 179.0(4) . . . . ?
N10 C16 C17 C18 -0.1(7) . . . . ?
N6 C16 C17 C18 -173.4(4) . . . . ?
C16 C17 C18 C19 -2.0(8) . . . . ?
C17 C18 C19 C20 2.2(8) . . . . ?
C18 C19 C20 N10 -0.4(8) . . . . ?
N3 C21 C22 C23 -2.5(8) . . . . ?
C21 C22 C23 C24 0.7(8) . . . . ?
C22 C23 C24 C25 1.7(8) . . . . ?
C23 C24 C25 N3 -2.6(6) . . . . ?
C23 C24 C25 N7 -176.4(4) . . . . ?
N11 C26 C27 C28 -3.2(7) . . . . ?
N7 C26 C27 C28 -178.7(4) . . . . ?
C26 C27 C28 C29 2.9(8) . . . . ?
C27 C28 C29 C30 0.3(8) . . . . ?
C28 C29 C30 N11 -3.5(8) . . . . ?
N4 C31 C32 C33 -2.3(8) . . . . ?
C31 C32 C33 C34 -2.0(9) . . . . ?
C32 C33 C34 C35 3.9(8) . . . . ?
C33 C34 C35 N4 -1.5(7) . . . . ?
C33 C34 C35 N8 -178.1(5) . . . . ?
N12 C36 C37 C38 3.9(7) . . . . ?
N8 C36 C37 C38 -171.0(5) . . . . ?
C36 C37 C38 C39 0.8(8) . . . . ?
C37 C38 C39 C40 -3.0(9) . . . . ?
C38 C39 C40 N12 0.6(9) . . . . ?
C2 C1 N1 C5 1.3(7) . . . . ?
C2 C1 N1 Co1 177.4(4) . . . . ?
N5 C5 N1 C1 175.2(4) . . . . ?
C4 C5 N1 C1 0.1(6) . . . . ?
N5 C5 N1 Co1 -0.9(5) . . . . ?
C4 C5 N1 Co1 -176.0(3) . . . . ?
C12 C11 N2 C15 2.1(7) . . . . ?
C12 C11 N2 Co1 -174.2(4) . . . . ?
N6 C15 N2 C11 179.1(4) . . . . ?
C14 C15 N2 C11 1.5(6) . . . . ?
N6 C15 N2 Co1 -4.6(4) . . . . ?
C14 C15 N2 Co1 177.9(3) . . . . ?
C22 C21 N3 C25 1.6(7) . . . . ?
C22 C21 N3 Co1 177.8(4) . . . . ?
N7 C25 N3 C21 175.3(4) . . . . ?
C24 C25 N3 C21 1.0(6) . . . . ?
N7 C25 N3 Co1 -0.8(4) . . . . ?
C24 C25 N3 Co1 -175.1(3) . . . . ?
N8 C35 N4 C31 174.3(4) . . . . ?
C34 C35 N4 C31 -2.6(6) . . . . ?
N8 C35 N4 Co1 -7.8(5) . . . . ?
C34 C35 N4 Co1 175.3(3) . . . . ?
C32 C31 N4 C35 4.6(7) . . . . ?
C32 C31 N4 Co1 -173.4(4) . . . . ?
N1 C5 N5 C6 155.2(4) . . . . ?
C4 C5 N5 C6 -29.9(6) . . . . ?
N1 C5 N5 Co2 -25.9(4) . . . . ?
C4 C5 N5 Co2 149.0(3) . . . . ?
N9 C6 N5 C5 157.3(4) . . . . ?
C7 C6 N5 C5 -27.9(6) . . . . ?
N9 C6 N5 Co2 -21.6(4) . . . . ?
C7 C6 N5 Co2 153.2(4) . . . . ?
N2 C15 N6 C16 151.9(4) . . . . ?
C14 C15 N6 C16 -30.7(6) . . . . ?
N2 C15 N6 Co2 -21.0(4) . . . . ?
C14 C15 N6 Co2 156.4(3) . . . . ?
N10 C16 N6 C15 157.5(3) . . . . ?
C17 C16 N6 C15 -29.0(6) . . . . ?
N10 C16 N6 Co2 -29.3(4) . . . . ?
C17 C16 N6 Co2 144.2(4) . . . . ?
N11 C26 N7 C25 157.5(3) . . . . ?
C27 C26 N7 C25 -26.8(6) . . . . ?
N11 C26 N7 Co2 -18.1(4) . . . . ?
C27 C26 N7 Co2 157.5(3) . . . . ?
N3 C25 N7 C26 157.3(3) . . . . ?
C24 C25 N7 C26 -28.7(6) . . . . ?
N3 C25 N7 Co2 -27.0(4) . . . . ?
C24 C25 N7 Co2 147.0(3) . . . . ?
N12 C36 N8 C35 161.1(4) . . . . ?
C37 C36 N8 C35 -23.8(6) . . . . ?
N12 C36 N8 Co2 -22.4(4) . . . . ?
C37 C36 N8 Co2 152.7(4) . . . . ?
N4 C35 N8 C36 157.1(4) . . . . ?
C34 C35 N8 C36 -26.1(6) . . . . ?
N4 C35 N8 Co2 -19.4(4) . . . . ?
C34 C35 N8 Co2 157.4(4) . . . . ?
C9 C10 N9 C6 3.4(7) . . . . ?
C9 C10 N9 Co3 -177.2(4) . . . . ?
N5 C6 N9 C10 171.0(4) . . . . ?
C7 C6 N9 C10 -4.2(6) . . . . ?
N5 C6 N9 Co3 -8.4(4) . . . . ?
C7 C6 N9 Co3 176.5(3) . . . . ?
C19 C20 N10 C16 -1.7(7) . . . . ?
C19 C20 N10 Co3 172.4(4) . . . . ?
N6 C16 N10 C20 175.7(4) . . . . ?
C17 C16 N10 C20 1.9(6) . . . . ?
N6 C16 N10 Co3 1.5(5) . . . . ?
C17 C16 N10 Co3 -172.3(3) . . . . ?
C29 C30 N11 C26 3.2(7) . . . . ?
C29 C30 N11 Co3 -172.4(4) . . . . ?
N7 C26 N11 C30 176.1(4) . . . . ?
C27 C26 N11 C30 0.2(6) . . . . ?
N7 C26 N11 Co3 -8.3(4) . . . . ?
C27 C26 N11 Co3 175.8(3) . . . . ?
C39 C40 N12 C36 4.1(7) . . . . ?
C39 C40 N12 Co3 -179.5(4) . . . . ?
N8 C36 N12 C40 169.2(4) . . . . ?
C37 C36 N12 C40 -6.3(6) . . . . ?
N8 C36 N12 Co3 -7.0(5) . . . . ?
C37 C36 N12 Co3 177.5(3) . . . . ?
C1S C2S O1S C3S -173.0(6) . . . . ?
C4S C3S O1S C2S 177.8(5) . . . . ?

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
C1 H1 Br1 0.93 2.78 3.429(6) 128.2 .
C2 H2 O1S 0.93 2.66 3.432(6) 141.1 .
C4 H4 Br1 0.93 3.11 3.735(4) 125.9 2_646
C10 H10 Br2 0.93 2.66 3.269(5) 123.6 .
C11 H11 Br1 0.93 2.73 3.389(5) 128.3 .
C20 H20 Br2 0.93 2.66 3.337(5) 130.4 .
C21 H21 Br1 0.93 2.72 3.387(5) 129.3 .
C29 H29 Br2 0.93 2.95 3.842(5) 162.5 3_766
C30 H30 Br2 0.93 2.76 3.380(5) 125.4 .
C31 H31 Br1 0.93 2.73 3.357(5) 125.9 .
C32 H32 Br1 0.93 2.91 3.793(5) 160.0 3_667
C40 H40 Br2 0.93 2.76 3.354(5) 122.5 .

_refine_diff_density_max         0.756
_refine_diff_density_min         -1.718
_refine_diff_density_rms         0.106

####################################################################### 
# 
# 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_4-Et2O-85K
_database_code_depnum_ccdc_archive 'CCDC 1865593'
_audit_update_record             
;
2018-09-03 deposited with the CCDC.
2018-11-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C40 H32 Co3 I2 N12, C4 H10 O'
_chemical_formula_sum            'C44 H42 Co3 I2 N12 O'
_chemical_formula_weight         1185.48

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

_cell_length_a                   37.112(3)
_cell_length_b                   12.6154(9)
_cell_length_c                   18.8581(14)
_cell_angle_alpha                90
_cell_angle_beta                 91.526(4)
_cell_angle_gamma                90
_cell_volume                     8825.8(11)
_cell_formula_units_Z            8
_cell_measurement_temperature    85(2)
_cell_measurement_reflns_used    9072
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      30.51

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_F_000             4680
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.087
_exptl_absorpt_coefficient_mu    2.564
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.67333
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   '(SADABS; Bruker, 2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      85(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            197985
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.011
_diffrn_reflns_theta_max         30.563
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             13501
_reflns_number_gt                11803
_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       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_structure_solution    'SHELXS2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_publication_material  'SHELXL-2016/4 (Sheldrick, 2016)'
_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)+(0.0181P)²+20.7854P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13501
_refine_ls_number_parameters     561
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0231
_refine_ls_wR_factor_ref         0.0524
_refine_ls_wR_factor_gt          0.0499
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.002
_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
C1 C 0.05763(5) 0.77276(15) 0.15921(10) 0.0202(4) Uani 1 1 d . . . . .
H1 H 0.058992 0.839736 0.136410 0.024 Uiso 1 1 calc R U . . .
C2 C 0.03730(5) 0.69469(17) 0.12660(11) 0.0234(4) Uani 1 1 d . . . . .
H2 H 0.024624 0.707601 0.083029 0.028 Uiso 1 1 calc R U . . .
C3 C 0.03595(5) 0.59619(16) 0.15960(11) 0.0208(4) Uani 1 1 d . . . . .
H3 H 0.022833 0.539731 0.137814 0.025 Uiso 1 1 calc R U . . .
C4 C 0.05362(5) 0.58063(15) 0.22384(10) 0.0173(3) Uani 1 1 d . . . . .
H4 H 0.052252 0.514073 0.247184 0.021 Uiso 1 1 calc R U . . .
C5 C 0.07373(4) 0.66396(13) 0.25465(9) 0.0132(3) Uani 1 1 d . . . . .
C6 C 0.08972(4) 0.58335(13) 0.36808(9) 0.0119(3) Uani 1 1 d . . . . .
C7 C 0.05533(5) 0.55069(15) 0.38962(10) 0.0183(4) Uani 1 1 d . . . . .
H7 H 0.034469 0.569431 0.362140 0.022 Uiso 1 1 calc R U . . .
C8 C 0.05204(5) 0.49159(16) 0.45053(11) 0.0212(4) Uani 1 1 d . . . . .
H8 H 0.028967 0.468925 0.465050 0.025 Uiso 1 1 calc R U . . .
C9 C 0.08283(5) 0.46530(15) 0.49070(10) 0.0194(4) Uani 1 1 d . . . . .
H9 H 0.081117 0.425810 0.533372 0.023 Uiso 1 1 calc R U . . .
C10 C 0.11587(5) 0.49811(14) 0.46688(9) 0.0148(3) Uani 1 1 d . . . . .
H10 H 0.136806 0.481249 0.494692 0.018 Uiso 1 1 calc R U . . .
C11 C 0.15777(5) 0.92135(14) 0.13701(10) 0.0173(3) Uani 1 1 d . . . . .
H11 H 0.148346 0.990955 0.141654 0.021 Uiso 1 1 calc R U . . .
C12 C 0.18231(5) 0.90320(15) 0.08467(10) 0.0210(4) Uani 1 1 d . . . . .
H12 H 0.189520 0.958738 0.054120 0.025 Uiso 1 1 calc R U . . .
C13 C 0.19625(5) 0.80124(15) 0.07782(10) 0.0192(4) Uani 1 1 d . . . . .
H13 H 0.213028 0.785915 0.042046 0.023 Uiso 1 1 calc R U . . .
C14 C 0.18543(5) 0.72296(14) 0.12347(9) 0.0155(3) Uani 1 1 d . . . . .
H14 H 0.194688 0.653100 0.119294 0.019 Uiso 1 1 calc R U . . .
C15 C 0.16056(4) 0.74675(13) 0.17645(9) 0.0108(3) Uani 1 1 d . . . . .
C16 C 0.15146(4) 0.56977(13) 0.22148(9) 0.0109(3) Uani 1 1 d . . . . .
C17 C 0.14325(5) 0.51649(14) 0.15721(9) 0.0148(3) Uani 1 1 d . . . . .
H17 H 0.141735 0.554987 0.113938 0.018 Uiso 1 1 calc R U . . .
C18 C 0.13746(5) 0.40892(14) 0.15733(10) 0.0180(3) Uani 1 1 d . . . . .
H18 H 0.132102 0.372565 0.114209 0.022 Uiso 1 1 calc R U . . .
C19 C 0.13954(5) 0.35354(14) 0.22139(10) 0.0179(4) Uani 1 1 d . . . . .
H19 H 0.134572 0.279711 0.222978 0.021 Uiso 1 1 calc R U . . .
C20 C 0.14895(4) 0.40848(13) 0.28228(10) 0.0136(3) Uani 1 1 d . . . . .
H20 H 0.150556 0.370584 0.325778 0.016 Uiso 1 1 calc R U . . .
C21 C 0.14642(5) 1.07090(14) 0.33630(10) 0.0177(3) Uani 1 1 d . . . . .
H21 H 0.124796 1.106320 0.322244 0.021 Uiso 1 1 calc R U . . .
C22 C 0.17179(5) 1.12651(14) 0.37544(10) 0.0203(4) Uani 1 1 d . . . . .
H22 H 0.167712 1.198283 0.388184 0.024 Uiso 1 1 calc R U . . .
C23 C 0.20374(5) 1.07515(14) 0.39609(10) 0.0179(4) Uani 1 1 d . . . . .
H23 H 0.221929 1.111878 0.422613 0.022 Uiso 1 1 calc R U . . .
C24 C 0.20853(5) 0.97061(14) 0.37751(9) 0.0147(3) Uani 1 1 d . . . . .
H24 H 0.230110 0.934641 0.391176 0.018 Uiso 1 1 calc R U . . .
C25 C 0.18122(4) 0.91707(12) 0.33802(9) 0.0110(3) Uani 1 1 d . . . . .
C26 C 0.21287(4) 0.75596(12) 0.31166(8) 0.0098(3) Uani 1 1 d . . . . .
C27 C 0.24232(4) 0.79936(14) 0.27564(9) 0.0133(3) Uani 1 1 d . . . . .
H27 H 0.242884 0.872982 0.265134 0.016 Uiso 1 1 calc R U . . .
C28 C 0.27016(5) 0.73481(14) 0.25581(9) 0.0149(3) Uani 1 1 d . . . . .
H28 H 0.289866 0.763086 0.230807 0.018 Uiso 1 1 calc R U . . .
C29 C 0.26911(5) 0.62720(14) 0.27291(9) 0.0144(3) Uani 1 1 d . . . . .
H29 H 0.288197 0.581256 0.260404 0.017 Uiso 1 1 calc R U . . .
C30 C 0.23978(4) 0.58898(13) 0.30831(9) 0.0117(3) Uani 1 1 d . . . . .
H30 H 0.239020 0.515469 0.319115 0.014 Uiso 1 1 calc R U . . .
C31 C 0.04552(5) 0.92136(14) 0.35130(11) 0.0191(4) Uani 1 1 d . . . . .
H31 H 0.036482 0.951640 0.308270 0.023 Uiso 1 1 calc R U . . .
C32 C 0.02349(5) 0.92065(15) 0.40862(12) 0.0225(4) Uani 1 1 d . . . . .
H32 H 0.000184 0.951734 0.405607 0.027 Uiso 1 1 calc R U . . .
C33 C 0.03605(5) 0.87332(16) 0.47138(11) 0.0217(4) Uani 1 1 d . . . . .
H33 H 0.021346 0.871003 0.511823 0.026 Uiso 1 1 calc R U . . .
C34 C 0.07025(5) 0.82983(15) 0.47378(10) 0.0176(3) Uani 1 1 d . . . . .
H34 H 0.079122 0.796802 0.516018 0.021 Uiso 1 1 calc R U . . .
C35 C 0.09201(4) 0.83436(13) 0.41370(9) 0.0125(3) Uani 1 1 d . . . . .
C36 C 0.14861(4) 0.76843(12) 0.46420(9) 0.0103(3) Uani 1 1 d . . . . .
C37 C 0.15040(5) 0.83004(13) 0.52676(9) 0.0146(3) Uani 1 1 d . . . . .
H37 H 0.132165 0.880738 0.535818 0.017 Uiso 1 1 calc R U . . .
C38 C 0.17867(5) 0.81627(14) 0.57445(9) 0.0159(3) Uani 1 1 d . . . . .
H38 H 0.179792 0.856495 0.617043 0.019 Uiso 1 1 calc R U . . .
C39 C 0.20570(5) 0.74305(14) 0.56015(10) 0.0162(3) Uani 1 1 d . . . . .
H39 H 0.226004 0.735021 0.591451 0.019 Uiso 1 1 calc R U . . .
C40 C 0.20220(4) 0.68280(13) 0.49957(9) 0.0129(3) Uani 1 1 d . . . . .
H40 H 0.220680 0.633329 0.489547 0.015 Uiso 1 1 calc R U . . .
C41 C -0.02380(8) 0.3053(2) 0.36934(16) 0.0450(7) Uani 1 1 d . . . . .
H41A H -0.038294 0.242893 0.380545 0.068 Uiso 1 1 calc R U . . .
H41B H -0.034255 0.340787 0.327374 0.068 Uiso 1 1 calc R U . . .
H41C H -0.023581 0.354365 0.409653 0.068 Uiso 1 1 calc R U . . .
C42 C 0.01419(8) 0.2714(2) 0.35464(13) 0.0421(6) Uani 1 1 d . . . . .
H42A H 0.013920 0.213990 0.318873 0.051 Uiso 1 1 calc R U . . .
H42B H 0.027911 0.331968 0.335665 0.051 Uiso 1 1 calc R U . . .
C43 C 0.06666(7) 0.1978(2) 0.40855(13) 0.0372(6) Uani 1 1 d . . . . .
H43A H 0.081886 0.256601 0.391663 0.045 Uiso 1 1 calc R U . . .
H43B H 0.066347 0.141206 0.372180 0.045 Uiso 1 1 calc R U . . .
C44 C 0.08190(7) 0.1554(2) 0.47751(14) 0.0405(6) Uani 1 1 d . . . . .
H44A H 0.083657 0.212968 0.512349 0.061 Uiso 1 1 calc R U . . .
H44B H 0.105932 0.125938 0.470023 0.061 Uiso 1 1 calc R U . . .
H44C H 0.066056 0.099738 0.495146 0.061 Uiso 1 1 calc R U . . .
N1 N 0.07581(4) 0.75997(12) 0.22180(8) 0.0145(3) Uani 1 1 d . . . . .
N2 N 0.14637(4) 0.84602(11) 0.18196(8) 0.0125(3) Uani 1 1 d . . . . .
N3 N 0.15049(4) 0.96804(11) 0.31653(8) 0.0134(3) Uani 1 1 d . . . . .
N4 N 0.07953(4) 0.88124(11) 0.35257(8) 0.0141(3) Uani 1 1 d . . . . .
N5 N 0.09546(4) 0.65244(11) 0.31410(8) 0.0113(3) Uani 1 1 d . . . . .
N6 N 0.15153(4) 0.67732(11) 0.22899(7) 0.0100(3) Uani 1 1 d . . . . .
N7 N 0.18196(4) 0.81084(10) 0.32411(7) 0.0095(2) Uani 1 1 d . . . . .
N8 N 0.12499(4) 0.78525(11) 0.40884(7) 0.0103(3) Uani 1 1 d . . . . .
N9 N 0.11999(4) 0.55294(11) 0.40608(8) 0.0109(3) Uani 1 1 d . . . . .
N10 N 0.15605(4) 0.51409(11) 0.28319(8) 0.0105(3) Uani 1 1 d . . . . .
N11 N 0.21199(4) 0.65073(11) 0.32852(7) 0.0094(2) Uani 1 1 d . . . . .
N12 N 0.17364(4) 0.69059(11) 0.45343(7) 0.0098(2) Uani 1 1 d . . . . .
O1 O 0.03092(4) 0.23495(13) 0.41911(8) 0.0319(3) Uani 1 1 d . . . . .
CO1 Co 0.11009(2) 0.88421(2) 0.26088(2) 0.01471(5) Uani 1 1 d . . . . .
CO2 Co 0.13835(2) 0.73240(2) 0.31887(2) 0.00850(4) Uani 1 1 d . . . . .
CO3 Co 0.16804(2) 0.59263(2) 0.37186(2) 0.00831(4) Uani 1 1 d . . . . .
I1 I 0.07703(2) 1.05423(2) 0.19240(2) 0.01939(3) Uani 1 1 d . . . . .
I2 I 0.20541(2) 0.41939(2) 0.43859(2) 0.01549(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.353(2) . ?
C1 C2 1.376(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.391(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.376(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.406(2) . ?
C4 H4 0.9500 . ?
C5 N1 1.364(2) . ?
C5 N5 1.371(2) . ?
C6 N5 1.361(2) . ?
C6 N9 1.371(2) . ?
C6 C7 1.411(2) . ?
C7 C8 1.378(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.394(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.381(2) . ?
C9 H9 0.9500 . ?
C10 N9 1.351(2) . ?
C10 H10 0.9500 . ?
C11 N2 1.349(2) . ?
C11 C12 1.380(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.394(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.377(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.410(2) . ?
C14 H14 0.9500 . ?
C15 N2 1.364(2) . ?
C15 N6 1.371(2) . ?
C16 N6 1.364(2) . ?
C16 N10 1.366(2) . ?
C16 C17 1.412(2) . ?
C17 C18 1.374(2) . ?
C17 H17 0.9500 . ?
C18 C19 1.396(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.378(2) . ?
C19 H19 0.9500 . ?
C20 N10 1.358(2) . ?
C20 H20 0.9500 . ?
C21 N3 1.360(2) . ?
C21 C22 1.373(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.397(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.377(2) . ?
C23 H23 0.9500 . ?
C24 C25 1.414(2) . ?
C24 H24 0.9500 . ?
C25 N3 1.361(2) . ?
C25 N7 1.366(2) . ?
C26 N7 1.366(2) . ?
C26 N11 1.366(2) . ?
C26 C27 1.412(2) . ?
C27 C28 1.375(2) . ?
C27 H27 0.9500 . ?
C28 C29 1.396(2) . ?
C28 H28 0.9500 . ?
C29 C30 1.379(2) . ?
C29 H29 0.9500 . ?
C30 N11 1.355(2) . ?
C30 H30 0.9500 . ?
C31 N4 1.359(2) . ?
C31 C32 1.373(3) . ?
C31 H31 0.9500 . ?
C32 C33 1.395(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.382(2) . ?
C33 H33 0.9500 . ?
C34 C35 1.410(3) . ?
C34 H34 0.9500 . ?
C35 N4 1.366(2) . ?
C35 N8 1.377(2) . ?
C36 N8 1.362(2) . ?
C36 N12 1.371(2) . ?
C36 C37 1.413(2) . ?
C37 C38 1.374(2) . ?
C37 H37 0.9500 . ?
C38 C39 1.395(2) . ?
C38 H38 0.9500 . ?
C39 C40 1.375(2) . ?
C39 H39 0.9500 . ?
C40 N12 1.357(2) . ?
C40 H40 0.9500 . ?
C41 C42 1.506(4) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 O1 1.427(3) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 O1 1.426(3) . ?
C43 C44 1.503(4) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
N1 CO1 2.1372(15) . ?
N2 CO1 2.0896(15) . ?
N3 CO1 2.0939(15) . ?
N4 CO1 2.0933(16) . ?
N5 CO2 1.8845(14) . ?
N6 CO2 1.9077(14) . ?
N7 CO2 1.8974(13) . ?
N8 CO2 1.9010(14) . ?
N9 CO3 1.9768(14) . ?
N10 CO3 1.9838(14) . ?
N11 CO3 1.9840(14) . ?
N12 CO3 1.9799(14) . ?
CO1 CO2 2.4295(3) . ?
CO1 I1 2.7728(3) . ?
CO2 CO3 2.2942(3) . ?
CO3 I2 2.8620(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 124.00(18) . . ?
N1 C1 H1 118.0 . . ?
C2 C1 H1 118.0 . . ?
C1 C2 C3 117.73(18) . . ?
C1 C2 H2 121.1 . . ?
C3 C2 H2 121.1 . . ?
C4 C3 C2 119.94(18) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 119.49(18) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
N1 C5 N5 115.23(15) . . ?
N1 C5 C4 120.83(16) . . ?
N5 C5 C4 123.56(16) . . ?
N5 C6 N9 115.33(14) . . ?
N5 C6 C7 124.25(16) . . ?
N9 C6 C7 120.18(16) . . ?
C8 C7 C6 119.93(17) . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C7 C8 C9 119.50(17) . . ?
C7 C8 H8 120.3 . . ?
C9 C8 H8 120.3 . . ?
C10 C9 C8 118.30(17) . . ?
C10 C9 H9 120.9 . . ?
C8 C9 H9 120.9 . . ?
N9 C10 C9 123.45(16) . . ?
N9 C10 H10 118.3 . . ?
C9 C10 H10 118.3 . . ?
N2 C11 C12 123.82(16) . . ?
N2 C11 H11 118.1 . . ?
C12 C11 H11 118.1 . . ?
C11 C12 C13 118.24(17) . . ?
C11 C12 H12 120.9 . . ?
C13 C12 H12 120.9 . . ?
C14 C13 C12 119.26(17) . . ?
C14 C13 H13 120.4 . . ?
C12 C13 H13 120.4 . . ?
C13 C14 C15 119.84(16) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
N2 C15 N6 115.43(14) . . ?
N2 C15 C14 120.72(15) . . ?
N6 C15 C14 123.59(15) . . ?
N6 C16 N10 115.04(14) . . ?
N6 C16 C17 124.21(15) . . ?
N10 C16 C17 120.38(15) . . ?
C18 C17 C16 119.93(17) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C17 C18 C19 119.39(17) . . ?
C17 C18 H18 120.3 . . ?
C19 C18 H18 120.3 . . ?
C20 C19 C18 118.44(16) . . ?
C20 C19 H19 120.8 . . ?
C18 C19 H19 120.8 . . ?
N10 C20 C19 123.28(16) . . ?
N10 C20 H20 118.4 . . ?
C19 C20 H20 118.4 . . ?
N3 C21 C22 123.72(17) . . ?
N3 C21 H21 118.1 . . ?
C22 C21 H21 118.1 . . ?
C21 C22 C23 118.52(16) . . ?
C21 C22 H22 120.7 . . ?
C23 C22 H22 120.7 . . ?
C24 C23 C22 119.17(17) . . ?
C24 C23 H23 120.4 . . ?
C22 C23 H23 120.4 . . ?
C23 C24 C25 119.73(17) . . ?
C23 C24 H24 120.1 . . ?
C25 C24 H24 120.1 . . ?
N3 C25 N7 115.29(15) . . ?
N3 C25 C24 120.95(15) . . ?
N7 C25 C24 123.52(15) . . ?
N7 C26 N11 115.29(14) . . ?
N7 C26 C27 123.40(15) . . ?
N11 C26 C27 120.84(15) . . ?
C28 C27 C26 119.86(16) . . ?
C28 C27 H27 120.1 . . ?
C26 C27 H27 120.1 . . ?
C27 C28 C29 119.14(16) . . ?
C27 C28 H28 120.4 . . ?
C29 C28 H28 120.4 . . ?
C30 C29 C28 118.64(16) . . ?
C30 C29 H29 120.7 . . ?
C28 C29 H29 120.7 . . ?
N11 C30 C29 123.47(15) . . ?
N11 C30 H30 118.3 . . ?
C29 C30 H30 118.3 . . ?
N4 C31 C32 123.77(18) . . ?
N4 C31 H31 118.1 . . ?
C32 C31 H31 118.1 . . ?
C31 C32 C33 118.58(17) . . ?
C31 C32 H32 120.7 . . ?
C33 C32 H32 120.7 . . ?
C34 C33 C32 118.91(18) . . ?
C34 C33 H33 120.5 . . ?
C32 C33 H33 120.5 . . ?
C33 C34 C35 120.17(18) . . ?
C33 C34 H34 119.9 . . ?
C35 C34 H34 119.9 . . ?
N4 C35 N8 114.88(15) . . ?
N4 C35 C34 120.49(15) . . ?
N8 C35 C34 124.36(16) . . ?
N8 C36 N12 115.02(14) . . ?
N8 C36 C37 124.71(15) . . ?
N12 C36 C37 120.05(15) . . ?
C38 C37 C36 119.67(16) . . ?
C38 C37 H37 120.2 . . ?
C36 C37 H37 120.2 . . ?
C37 C38 C39 119.83(16) . . ?
C37 C38 H38 120.1 . . ?
C39 C38 H38 120.1 . . ?
C40 C39 C38 118.28(16) . . ?
C40 C39 H39 120.9 . . ?
C38 C39 H39 120.9 . . ?
N12 C40 C39 123.20(16) . . ?
N12 C40 H40 118.4 . . ?
C39 C40 H40 118.4 . . ?
C42 C41 H41A 109.5 . . ?
C42 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C42 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O1 C42 C41 108.9(2) . . ?
O1 C42 H42A 109.9 . . ?
C41 C42 H42A 109.9 . . ?
O1 C42 H42B 109.9 . . ?
C41 C42 H42B 109.9 . . ?
H42A C42 H42B 108.3 . . ?
O1 C43 C44 109.03(19) . . ?
O1 C43 H43A 109.9 . . ?
C44 C43 H43A 109.9 . . ?
O1 C43 H43B 109.9 . . ?
C44 C43 H43B 109.9 . . ?
H43A C43 H43B 108.3 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C1 N1 C5 117.97(16) . . ?
C1 N1 CO1 119.45(13) . . ?
C5 N1 CO1 122.36(11) . . ?
C11 N2 C15 118.09(15) . . ?
C11 N2 CO1 120.26(12) . . ?
C15 N2 CO1 121.57(11) . . ?
C21 N3 C25 117.88(16) . . ?
C21 N3 CO1 122.41(12) . . ?
C25 N3 CO1 119.58(11) . . ?
C31 N4 C35 118.03(16) . . ?
C31 N4 CO1 120.13(13) . . ?
C35 N4 CO1 121.74(11) . . ?
C6 N5 C5 125.39(14) . . ?
C6 N5 CO2 117.11(11) . . ?
C5 N5 CO2 117.38(11) . . ?
C16 N6 C15 124.08(14) . . ?
C16 N6 CO2 117.04(11) . . ?
C15 N6 CO2 118.88(11) . . ?
C26 N7 C25 123.47(14) . . ?
C26 N7 CO2 116.49(10) . . ?
C25 N7 CO2 120.02(11) . . ?
C36 N8 C35 125.04(14) . . ?
C36 N8 CO2 116.86(11) . . ?
C35 N8 CO2 118.07(11) . . ?
C10 N9 C6 118.49(14) . . ?
C10 N9 CO3 122.02(11) . . ?
C6 N9 CO3 119.48(11) . . ?
C20 N10 C16 118.28(14) . . ?
C20 N10 CO3 122.66(12) . . ?
C16 N10 CO3 118.77(11) . . ?
C30 N11 C26 118.03(14) . . ?
C30 N11 CO3 122.93(11) . . ?
C26 N11 CO3 118.70(11) . . ?
C40 N12 C36 118.54(14) . . ?
C40 N12 CO3 121.15(11) . . ?
C36 N12 CO3 120.31(11) . . ?
C43 O1 C42 111.86(19) . . ?
N2 CO1 N4 163.28(6) . . ?
N2 CO1 N3 90.40(6) . . ?
N4 CO1 N3 89.52(6) . . ?
N2 CO1 N1 88.52(6) . . ?
N4 CO1 N1 86.63(6) . . ?
N3 CO1 N1 162.72(6) . . ?
N2 CO1 CO2 81.96(4) . . ?
N4 CO1 CO2 81.43(4) . . ?
N3 CO1 CO2 82.98(4) . . ?
N1 CO1 CO2 79.80(4) . . ?
N2 CO1 I1 97.59(4) . . ?
N4 CO1 I1 98.97(4) . . ?
N3 CO1 I1 98.32(4) . . ?
N1 CO1 I1 98.91(4) . . ?
CO2 CO1 I1 178.635(12) . . ?
N5 CO2 N7 179.05(6) . . ?
N5 CO2 N8 89.45(6) . . ?
N7 CO2 N8 90.74(6) . . ?
N5 CO2 N6 89.94(6) . . ?
N7 CO2 N6 89.87(6) . . ?
N8 CO2 N6 179.15(6) . . ?
N5 CO2 CO3 90.27(4) . . ?
N7 CO2 CO3 88.79(4) . . ?
N8 CO2 CO3 90.83(4) . . ?
N6 CO2 CO3 88.59(4) . . ?
N5 CO2 CO1 92.67(4) . . ?
N7 CO2 CO1 88.27(4) . . ?
N8 CO2 CO1 90.32(4) . . ?
N6 CO2 CO1 90.29(4) . . ?
CO3 CO2 CO1 176.858(13) . . ?
N9 CO3 N12 88.93(6) . . ?
N9 CO3 N10 87.98(6) . . ?
N12 CO3 N10 169.47(6) . . ?
N9 CO3 N11 170.61(6) . . ?
N12 CO3 N11 91.09(6) . . ?
N10 CO3 N11 90.32(6) . . ?
N9 CO3 CO2 84.83(4) . . ?
N12 CO3 CO2 84.15(4) . . ?
N10 CO3 CO2 85.55(4) . . ?
N11 CO3 CO2 85.83(4) . . ?
N9 CO3 I2 95.39(4) . . ?
N12 CO3 I2 95.47(4) . . ?
N10 CO3 I2 94.84(4) . . ?
N11 CO3 I2 93.96(4) . . ?
CO2 CO3 I2 179.555(12) . . ?

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
N1 C1 C2 C3 -1.1(3) . . . . ?
C1 C2 C3 C4 2.1(3) . . . . ?
C2 C3 C4 C5 -1.7(3) . . . . ?
C3 C4 C5 N1 0.2(3) . . . . ?
C3 C4 C5 N5 -172.31(17) . . . . ?
N5 C6 C7 C8 -171.48(17) . . . . ?
N9 C6 C7 C8 2.6(3) . . . . ?
C6 C7 C8 C9 0.5(3) . . . . ?
C7 C8 C9 C10 -1.3(3) . . . . ?
C8 C9 C10 N9 -1.1(3) . . . . ?
N2 C11 C12 C13 -0.1(3) . . . . ?
C11 C12 C13 C14 -0.6(3) . . . . ?
C12 C13 C14 C15 -0.1(3) . . . . ?
C13 C14 C15 N2 1.6(3) . . . . ?
C13 C14 C15 N6 -172.22(17) . . . . ?
N6 C16 C17 C18 -168.20(17) . . . . ?
N10 C16 C17 C18 4.4(3) . . . . ?
C16 C17 C18 C19 0.4(3) . . . . ?
C17 C18 C19 C20 -2.8(3) . . . . ?
C18 C19 C20 N10 0.5(3) . . . . ?
N3 C21 C22 C23 0.3(3) . . . . ?
C21 C22 C23 C24 -0.9(3) . . . . ?
C22 C23 C24 C25 0.0(3) . . . . ?
C23 C24 C25 N3 1.6(3) . . . . ?
C23 C24 C25 N7 -172.50(16) . . . . ?
N7 C26 C27 C28 -170.27(16) . . . . ?
N11 C26 C27 C28 1.4(2) . . . . ?
C26 C27 C28 C29 -1.1(3) . . . . ?
C27 C28 C29 C30 0.9(3) . . . . ?
C28 C29 C30 N11 -1.0(3) . . . . ?
N4 C31 C32 C33 -2.1(3) . . . . ?
C31 C32 C33 C34 0.6(3) . . . . ?
C32 C33 C34 C35 0.5(3) . . . . ?
C33 C34 C35 N4 -0.3(3) . . . . ?
C33 C34 C35 N8 -173.92(17) . . . . ?
N8 C36 C37 C38 -170.23(16) . . . . ?
N12 C36 C37 C38 4.3(2) . . . . ?
C36 C37 C38 C39 1.2(3) . . . . ?
C37 C38 C39 C40 -3.0(3) . . . . ?
C38 C39 C40 N12 -0.5(3) . . . . ?
C2 C1 N1 C5 -0.3(3) . . . . ?
C2 C1 N1 CO1 174.41(15) . . . . ?
N5 C5 N1 C1 173.87(15) . . . . ?
C4 C5 N1 C1 0.8(2) . . . . ?
N5 C5 N1 CO1 -0.7(2) . . . . ?
C4 C5 N1 CO1 -173.77(12) . . . . ?
C12 C11 N2 C15 1.6(3) . . . . ?
C12 C11 N2 CO1 178.38(15) . . . . ?
N6 C15 N2 C11 172.01(15) . . . . ?
C14 C15 N2 C11 -2.3(2) . . . . ?
N6 C15 N2 CO1 -4.72(19) . . . . ?
C14 C15 N2 CO1 -179.04(12) . . . . ?
C22 C21 N3 C25 1.3(3) . . . . ?
C22 C21 N3 CO1 177.09(14) . . . . ?
N7 C25 N3 C21 172.37(15) . . . . ?
C24 C25 N3 C21 -2.2(2) . . . . ?
N7 C25 N3 CO1 -3.6(2) . . . . ?
C24 C25 N3 CO1 -178.10(12) . . . . ?
C32 C31 N4 C35 2.3(3) . . . . ?
C32 C31 N4 CO1 178.71(14) . . . . ?
N8 C35 N4 C31 173.14(15) . . . . ?
C34 C35 N4 C31 -1.1(2) . . . . ?
N8 C35 N4 CO1 -3.21(19) . . . . ?
C34 C35 N4 CO1 -177.45(13) . . . . ?
N9 C6 N5 C5 154.50(16) . . . . ?
C7 C6 N5 C5 -31.2(3) . . . . ?
N9 C6 N5 CO2 -21.35(19) . . . . ?
C7 C6 N5 CO2 152.96(14) . . . . ?
N1 C5 N5 C6 155.97(16) . . . . ?
C4 C5 N5 C6 -31.1(3) . . . . ?
N1 C5 N5 CO2 -28.19(19) . . . . ?
C4 C5 N5 CO2 144.71(14) . . . . ?
N10 C16 N6 C15 154.95(15) . . . . ?
C17 C16 N6 C15 -32.1(2) . . . . ?
N10 C16 N6 CO2 -24.75(18) . . . . ?
C17 C16 N6 CO2 148.17(14) . . . . ?
N2 C15 N6 C16 155.58(15) . . . . ?
C14 C15 N6 C16 -30.3(2) . . . . ?
N2 C15 N6 CO2 -24.73(19) . . . . ?
C14 C15 N6 CO2 149.41(14) . . . . ?
N11 C26 N7 C25 153.11(15) . . . . ?
C27 C26 N7 C25 -34.8(2) . . . . ?
N11 C26 N7 CO2 -28.50(18) . . . . ?
C27 C26 N7 CO2 143.60(14) . . . . ?
N3 C25 N7 C26 150.06(15) . . . . ?
C24 C25 N7 C26 -35.6(2) . . . . ?
N3 C25 N7 CO2 -28.27(19) . . . . ?
C24 C25 N7 CO2 146.10(14) . . . . ?
N12 C36 N8 C35 159.84(15) . . . . ?
C37 C36 N8 C35 -25.4(3) . . . . ?
N12 C36 N8 CO2 -18.07(18) . . . . ?
C37 C36 N8 CO2 156.66(13) . . . . ?
N4 C35 N8 C36 154.43(15) . . . . ?
C34 C35 N8 C36 -31.6(3) . . . . ?
N4 C35 N8 CO2 -27.68(18) . . . . ?
C34 C35 N8 CO2 146.30(14) . . . . ?
C9 C10 N9 C6 4.1(3) . . . . ?
C9 C10 N9 CO3 -177.16(14) . . . . ?
N5 C6 N9 C10 169.78(15) . . . . ?
C7 C6 N9 C10 -4.8(2) . . . . ?
N5 C6 N9 CO3 -8.97(19) . . . . ?
C7 C6 N9 CO3 176.47(13) . . . . ?
C19 C20 N10 C16 4.2(2) . . . . ?
C19 C20 N10 CO3 177.99(13) . . . . ?
N6 C16 N10 C20 166.65(14) . . . . ?
C17 C16 N10 C20 -6.6(2) . . . . ?
N6 C16 N10 CO3 -7.39(19) . . . . ?
C17 C16 N10 CO3 179.39(12) . . . . ?
C29 C30 N11 C26 1.2(2) . . . . ?
C29 C30 N11 CO3 174.48(13) . . . . ?
N7 C26 N11 C30 170.91(14) . . . . ?
C27 C26 N11 C30 -1.4(2) . . . . ?
N7 C26 N11 CO3 -2.62(19) . . . . ?
C27 C26 N11 CO3 -174.94(12) . . . . ?
C39 C40 N12 C36 5.9(2) . . . . ?
C39 C40 N12 CO3 -174.39(14) . . . . ?
N8 C36 N12 C40 167.34(14) . . . . ?
C37 C36 N12 C40 -7.7(2) . . . . ?
N8 C36 N12 CO3 -12.38(19) . . . . ?
C37 C36 N12 CO3 172.63(12) . . . . ?
C44 C43 O1 C42 -177.0(2) . . . . ?
C41 C42 O1 C43 177.84(19) . . . . ?
C6 N5 CO2 N8 -56.74(12) . . . . ?
C5 N5 CO2 N8 127.08(13) . . . . ?
C6 N5 CO2 N6 122.68(12) . . . . ?
C5 N5 CO2 N6 -53.50(13) . . . . ?
C6 N5 CO2 CO3 34.09(12) . . . . ?
C5 N5 CO2 CO3 -142.09(12) . . . . ?
C6 N5 CO2 CO1 -147.03(12) . . . . ?
C5 N5 CO2 CO1 36.79(12) . . . . ?
C26 N7 CO2 N8 129.21(12) . . . . ?
C25 N7 CO2 N8 -52.35(13) . . . . ?
C26 N7 CO2 N6 -50.20(12) . . . . ?
C25 N7 CO2 N6 128.24(13) . . . . ?
C26 N7 CO2 CO3 38.39(11) . . . . ?
C25 N7 CO2 CO3 -143.16(12) . . . . ?
C26 N7 CO2 CO1 -140.50(11) . . . . ?
C25 N7 CO2 CO1 37.95(12) . . . . ?

_refine_diff_density_max         0.693
_refine_diff_density_min         -0.718
_refine_diff_density_rms         0.086


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile, ether'
_exptl_crystal_preparation       'Magnetic properties'
