# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2018

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1818142'
_audit_update_record             
;
2018-01-19 deposited with the CCDC.
2018-03-28 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         ?
_chemical_formula_sum            'C62 H60 Cl2 Fe2 N8 O14 S2'
_chemical_formula_weight         1387.90

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'
Fe Fe 0.3463 0.8444 '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'
S S 0.1246 0.1234 '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                   10.2821(9)
_cell_length_b                   12.1907(15)
_cell_length_c                   13.1148(12)
_cell_angle_alpha                82.243(9)
_cell_angle_beta                 84.962(7)
_cell_angle_gamma                72.071(9)
_cell_volume                     1547.9(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3812
_cell_measurement_theta_min      2.6190
_cell_measurement_theta_max      22.8430

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_F_000             718
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    0.695
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.96184
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
'Mon Jun 01 16:31:43 2015'
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  
'Saxi-CrysAlisPro-abstract goniometer imported S'
_diffrn_measurement_method       'ω and π scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19959
_diffrn_reflns_av_unetI/netI     0.0884
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.293
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             6152
_reflns_number_gt                3834
_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       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'CysAlisPro 171.37.34b'
_computing_data_reduction        'CysAlisPro 171.37.34b'
_computing_structure_solution    'SuperFlip (Palatinus & Chapius, 2007)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0845P)²+0.5375P] 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     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0058(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         6152
_refine_ls_number_parameters     407
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1057
_refine_ls_R_factor_gt           0.0644
_refine_ls_wR_factor_ref         0.1906
_refine_ls_wR_factor_gt          0.1598
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.040
_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 -0.0739(4) 0.0284(3) 0.4825(3) 0.0359(9) Uani 1 1 d . . . . .
O1 O 0.1673(2) -0.0077(2) 0.45931(19) 0.0410(7) Uani 1 1 d . . . . .
O2 O -0.0868(2) 0.0907(2) 0.3976(2) 0.0425(7) Uani 1 1 d . . . . .
C2 C -0.1477(4) 0.3493(5) 0.4404(4) 0.0668(14) Uani 1 1 d . . . . .
H2A H -0.2108 0.3989 0.4854 0.100 Uiso 1 1 calc R U . . .
H2B H -0.1484 0.3897 0.3723 0.100 Uiso 1 1 calc R U . . .
H2C H -0.1744 0.2807 0.4385 0.100 Uiso 1 1 calc R U . . .
C3 C -0.0066(4) 0.3157(4) 0.4795(3) 0.0510(11) Uani 1 1 d . . . . .
C4 C 0.0177(5) 0.3568(4) 0.5683(4) 0.0630(13) Uani 1 1 d . . . . .
H4 H -0.0554 0.4034 0.6049 0.076 Uiso 1 1 calc R U . . .
C5 C 0.1447(5) 0.3302(5) 0.6017(3) 0.0623(13) Uani 1 1 d . . . . .
H5 H 0.1590 0.3567 0.6619 0.075 Uiso 1 1 calc R U . . .
C6 C 0.2555(4) 0.2625(4) 0.5456(3) 0.0487(11) Uani 1 1 d . . . . .
C7 C 0.3942(5) 0.2361(4) 0.5723(4) 0.0597(13) Uani 1 1 d . . . . .
H7 H 0.4133 0.2606 0.6319 0.072 Uiso 1 1 calc R U . . .
C8 C 0.4982(5) 0.1761(4) 0.5125(4) 0.0612(13) Uani 1 1 d . . . . .
H8 H 0.5879 0.1604 0.5309 0.073 Uiso 1 1 calc R U . . .
C9 C 0.4717(4) 0.1367(4) 0.4212(3) 0.0460(10) Uani 1 1 d . . . . .
C10 C 0.5764(4) 0.0796(4) 0.3535(4) 0.0580(12) Uani 1 1 d . . . . .
H10 H 0.6677 0.0622 0.3689 0.070 Uiso 1 1 calc R U . . .
C11 C 0.5434(4) 0.0503(4) 0.2662(4) 0.0576(12) Uani 1 1 d . . . . .
H11 H 0.6126 0.0129 0.2210 0.069 Uiso 1 1 calc R U . . .
C12 C 0.4073(4) 0.0750(4) 0.2424(3) 0.0457(10) Uani 1 1 d . . . . .
C13 C 0.3717(5) 0.0501(5) 0.1417(3) 0.0605(13) Uani 1 1 d . . . . .
H13A H 0.4542 0.0159 0.1024 0.091 Uiso 1 1 calc R U . . .
H13B H 0.3180 -0.0028 0.1538 0.091 Uiso 1 1 calc R U . . .
H13C H 0.3202 0.1211 0.1041 0.091 Uiso 1 1 calc R U . . .
C14 C 0.3368(4) 0.1573(3) 0.3949(3) 0.0389(9) Uani 1 1 d . . . . .
N1 N 0.0972(3) 0.2458(3) 0.4267(2) 0.0409(8) Uani 1 1 d . . . . .
N2 N 0.3052(3) 0.1226(3) 0.3071(2) 0.0404(8) Uani 1 1 d . . . . .
C15 C 0.2265(4) 0.2228(4) 0.4581(3) 0.0406(9) Uani 1 1 d . . . . .
C16 C 0.0466(6) 0.3931(5) 0.1883(4) 0.0789(16) Uani 1 1 d . U . . .
H16A H 0.0127 0.4729 0.1599 0.118 Uiso 1 1 calc R U . . .
H16B H 0.0408 0.3883 0.2622 0.118 Uiso 1 1 calc R U . . .
H16C H 0.1404 0.3618 0.1649 0.118 Uiso 1 1 calc R U . . .
C17 C -0.0365(5) 0.3260(4) 0.1543(4) 0.0605(12) Uani 1 1 d . U . . .
C18 C -0.1331(6) 0.3762(5) 0.0789(4) 0.0759(16) Uani 1 1 d . . . . .
H18 H -0.1474 0.4534 0.0520 0.091 Uiso 1 1 calc R U . . .
C19 C -0.2055(6) 0.3142(6) 0.0448(4) 0.0824(18) Uani 1 1 d . . . . .
H19 H -0.2763 0.3512 0.0009 0.099 Uiso 1 1 calc R U . . .
C20 C -0.1748(4) 0.1945(5) 0.0749(4) 0.0619(14) Uani 1 1 d . . . . .
C21 C -0.2398(5) 0.1231(7) 0.0358(4) 0.0755(17) Uani 1 1 d . . . . .
H21 H -0.3126 0.1565 -0.0070 0.091 Uiso 1 1 calc R U . . .
C22 C -0.1970(6) 0.0073(7) 0.0600(4) 0.0773(17) Uani 1 1 d . . . . .
H22 H -0.2406 -0.0386 0.0339 0.093 Uiso 1 1 calc R U . . .
C23 C -0.0856(5) -0.0458(5) 0.1252(4) 0.0599(13) Uani 1 1 d . . . . .
C24 C -0.0307(6) -0.1660(5) 0.1469(4) 0.0713(16) Uani 1 1 d . . . . .
H24 H -0.0719 -0.2150 0.1231 0.086 Uiso 1 1 calc R U . . .
C25 C 0.0806(6) -0.2104(5) 0.2017(4) 0.0696(14) Uani 1 1 d . . . . .
H25 H 0.1209 -0.2903 0.2116 0.084 Uiso 1 1 calc R U . . .
C26 C 0.1368(5) -0.1372(4) 0.2444(4) 0.0576(12) Uani 1 1 d . . . . .
C27 C 0.2681(5) -0.1899(5) 0.2976(4) 0.0702(14) Uani 1 1 d . . . . .
H27A H 0.2917 -0.2730 0.3026 0.105 Uiso 1 1 calc R U . . .
H27B H 0.3393 -0.1646 0.2589 0.105 Uiso 1 1 calc R U . . .
H27C H 0.2575 -0.1661 0.3655 0.105 Uiso 1 1 calc R U . . .
C28 C -0.0231(4) 0.0226(4) 0.1682(3) 0.0483(11) Uani 1 1 d . . . . .
C29 C -0.0703(4) 0.1465(4) 0.1440(3) 0.0517(11) Uani 1 1 d . . . . .
N3 N -0.0039(3) 0.2133(3) 0.1865(3) 0.0476(9) Uani 1 1 d . . . . .
N4 N 0.0861(3) -0.0230(3) 0.2298(2) 0.0450(8) Uani 1 1 d . . . . .
Fe1 Fe 0.09760(5) 0.11408(5) 0.32290(4) 0.0396(2) Uani 1 1 d . . . . .
O3 O 0.6291(8) 0.8042(5) 0.1424(6) 0.190(3) Uani 1 1 d . . . . .
O4 O 0.6930(6) 0.6141(5) 0.1954(4) 0.1318(19) Uani 1 1 d . . . . .
O5 O 0.5456(7) 0.6812(9) 0.0745(6) 0.222(4) Uani 1 1 d . . . . .
O6 O 0.7621(6) 0.6797(5) 0.0361(4) 0.138(2) Uani 1 1 d . . . . .
Cl1 Cl 0.65516(13) 0.69594(12) 0.11068(10) 0.0653(4) Uani 1 1 d . . . . .
C30 C 0.4418(11) 0.4148(9) 0.1594(8) 0.171(4) Uiso 1 1 d . . . . .
H30A H 0.5187 0.3465 0.1554 0.257 Uiso 1 1 calc R U . A 1
H30B H 0.3726 0.4128 0.1157 0.257 Uiso 1 1 calc R U . A 1
H30C H 0.4706 0.4825 0.1374 0.257 Uiso 1 1 calc R U . A 1
C31 C 0.5169(11) 0.4422(10) 0.3359(8) 0.178(4) Uiso 1 1 d . . . . .
H31A H 0.5959 0.3760 0.3298 0.267 Uiso 1 1 calc R U . B 1
H31B H 0.5354 0.5100 0.2995 0.267 Uiso 1 1 calc R U . B 1
H31C H 0.4955 0.4530 0.4072 0.267 Uiso 1 1 calc R U . B 1
O7 O 0.2643(6) 0.5181(6) 0.2933(7) 0.187(3) Uani 1 1 d . . . . .
S1A S 0.3773(2) 0.4197(3) 0.28288(19) 0.0827(11) Uani 0.747(7) 1 d . . P C 1
S1B S 0.3726(11) 0.5069(11) 0.2461(12) 0.145(5) Uani 0.253(7) 1 d . . P C 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 O1 1.240(4) 2_556 ?
C1 O2 1.252(5) . ?
C1 C1 1.545(7) 2_556 ?
O1 C1 1.240(4) 2_556 ?
O1 Fe1 2.184(3) . ?
O2 Fe1 2.138(3) . ?
C2 C3 1.498(6) . ?
C3 N1 1.347(5) . ?
C3 C4 1.399(6) . ?
C4 C5 1.343(7) . ?
C5 C6 1.400(6) . ?
C6 C15 1.393(5) . ?
C6 C7 1.426(6) . ?
C7 C8 1.348(6) . ?
C8 C9 1.425(6) . ?
C9 C14 1.397(5) . ?
C9 C10 1.404(6) . ?
C10 C11 1.344(6) . ?
C11 C12 1.392(6) . ?
C12 N2 1.327(5) . ?
C12 C13 1.494(6) . ?
C14 N2 1.375(5) . ?
C14 C15 1.437(5) . ?
N1 C15 1.361(5) . ?
N1 Fe1 2.240(3) . ?
N2 Fe1 2.160(3) . ?
C16 C17 1.482(7) . ?
C17 N3 1.328(6) . ?
C17 C18 1.406(7) . ?
C18 C19 1.350(8) . ?
C19 C20 1.403(8) . ?
C20 C29 1.400(6) . ?
C20 C21 1.417(8) . ?
C21 C22 1.344(8) . ?
C22 C23 1.424(7) . ?
C23 C28 1.395(6) . ?
C23 C24 1.398(8) . ?
C24 C25 1.333(8) . ?
C25 C26 1.398(6) . ?
C26 N4 1.322(6) . ?
C26 C27 1.493(6) . ?
C28 N4 1.369(5) . ?
C28 C29 1.436(7) . ?
C29 N3 1.404(6) . ?
N3 Fe1 2.172(3) . ?
N4 Fe1 2.235(3) . ?
O3 Cl1 1.378(5) . ?
O4 Cl1 1.385(5) . ?
O5 Cl1 1.330(5) . ?
O6 Cl1 1.392(5) . ?
C30 S1B 1.664(14) . ?
C30 S1A 1.696(10) . ?
C31 S1A 1.757(10) . ?
C31 S1B 1.882(15) . ?
O7 S1B 1.204(13) . ?
O7 S1A 1.402(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
O1 C1 O2 126.6(3) 2_556 . ?
O1 C1 C1 117.0(4) 2_556 2_556 ?
O2 C1 C1 116.4(4) . 2_556 ?
C1 O1 Fe1 114.4(2) 2_556 . ?
C1 O2 Fe1 115.9(2) . . ?
N1 C3 C4 120.4(4) . . ?
N1 C3 C2 118.7(4) . . ?
C4 C3 C2 120.9(4) . . ?
C5 C4 C3 121.2(4) . . ?
C4 C5 C6 119.6(4) . . ?
C15 C6 C5 117.2(4) . . ?
C15 C6 C7 119.5(4) . . ?
C5 C6 C7 123.2(4) . . ?
C8 C7 C6 121.1(4) . . ?
C7 C8 C9 120.5(4) . . ?
C14 C9 C10 117.4(4) . . ?
C14 C9 C8 119.8(4) . . ?
C10 C9 C8 122.7(4) . . ?
C11 C10 C9 119.3(4) . . ?
C10 C11 C12 121.1(4) . . ?
N2 C12 C11 121.5(4) . . ?
N2 C12 C13 117.8(3) . . ?
C11 C12 C13 120.7(4) . . ?
N2 C14 C9 122.4(4) . . ?
N2 C14 C15 118.3(3) . . ?
C9 C14 C15 119.3(3) . . ?
C3 N1 C15 118.3(3) . . ?
C3 N1 Fe1 130.6(3) . . ?
C15 N1 Fe1 108.3(2) . . ?
C12 N2 C14 118.1(3) . . ?
C12 N2 Fe1 129.8(3) . . ?
C14 N2 Fe1 109.7(2) . . ?
N1 C15 C6 123.0(4) . . ?
N1 C15 C14 117.3(3) . . ?
C6 C15 C14 119.6(3) . . ?
N3 C17 C18 120.8(5) . . ?
N3 C17 C16 117.8(4) . . ?
C18 C17 C16 120.7(5) . . ?
C19 C18 C17 121.0(5) . . ?
C18 C19 C20 120.5(5) . . ?
C29 C20 C19 116.1(5) . . ?
C29 C20 C21 120.5(6) . . ?
C19 C20 C21 123.3(5) . . ?
C22 C21 C20 120.5(5) . . ?
C21 C22 C23 120.7(5) . . ?
C28 C23 C24 116.8(5) . . ?
C28 C23 C22 120.1(5) . . ?
C24 C23 C22 123.1(5) . . ?
C25 C24 C23 120.1(5) . . ?
C24 C25 C26 120.2(5) . . ?
N4 C26 C25 122.2(4) . . ?
N4 C26 C27 119.1(4) . . ?
C25 C26 C27 118.3(5) . . ?
N4 C28 C23 123.0(5) . . ?
N4 C28 C29 117.7(4) . . ?
C23 C28 C29 119.3(4) . . ?
C20 C29 N3 123.0(5) . . ?
C20 C29 C28 118.7(4) . . ?
N3 C29 C28 118.2(4) . . ?
C17 N3 C29 118.0(4) . . ?
C17 N3 Fe1 131.0(3) . . ?
C29 N3 Fe1 109.1(3) . . ?
C26 N4 C28 117.5(4) . . ?
C26 N4 Fe1 131.1(3) . . ?
C28 N4 Fe1 108.4(3) . . ?
O2 Fe1 N2 158.30(11) . . ?
O2 Fe1 N3 93.65(11) . . ?
N2 Fe1 N3 106.67(12) . . ?
O2 Fe1 O1 76.11(10) . . ?
N2 Fe1 O1 84.65(11) . . ?
N3 Fe1 O1 167.14(12) . . ?
O2 Fe1 N4 83.89(11) . . ?
N2 Fe1 N4 107.77(12) . . ?
N3 Fe1 N4 76.73(14) . . ?
O1 Fe1 N4 94.21(12) . . ?
O2 Fe1 N1 91.43(11) . . ?
N2 Fe1 N1 76.11(12) . . ?
N3 Fe1 N1 105.44(13) . . ?
O1 Fe1 N1 82.90(11) . . ?
N4 Fe1 N1 174.99(12) . . ?
O5 Cl1 O3 112.5(6) . . ?
O5 Cl1 O4 107.4(5) . . ?
O3 Cl1 O4 107.9(4) . . ?
O5 Cl1 O6 110.4(5) . . ?
O3 Cl1 O6 108.9(4) . . ?
O4 Cl1 O6 109.6(4) . . ?
O7 S1A C30 111.9(5) . . ?
O7 S1A C31 107.6(5) . . ?
C30 S1A C31 97.5(5) . . ?
O7 S1B C30 126.8(10) . . ?
O7 S1B C31 110.1(12) . . ?
C30 S1B C31 93.9(7) . . ?

_refine_diff_density_max         0.711
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.079



####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1818145'
_audit_update_record             
;
2018-01-19 deposited with the CCDC.
2018-03-28 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         ?
_chemical_formula_sum            'C62 H60 Cl2 N8 O14 S2 Zn2'
_chemical_formula_weight         1406.94

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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                   10.2879(6)
_cell_length_b                   12.2402(11)
_cell_length_c                   13.0862(11)
_cell_angle_alpha                81.993(7)
_cell_angle_beta                 84.845(6)
_cell_angle_gamma                71.976(7)
_cell_volume                     1549.8(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    3000
_cell_measurement_theta_min      2.6300
_cell_measurement_theta_max      22.9410

_exptl_crystal_description       Tabular
_exptl_crystal_colour            Colorles
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_F_000             726
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    1.000
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.95738
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
'Thu Jun 18 14:59:54 2015'
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  
'Saxi-CrysAlisPro-abstract goniometer imported S'
_diffrn_measurement_method       'ω and π scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16336
_diffrn_reflns_av_unetI/netI     0.0580
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.289
_diffrn_reflns_theta_max         26.372
_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             6314
_reflns_number_gt                4444
_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       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'CysAlisPro 171.37.34b'
_computing_data_reduction        'CysAlisPro 171.37.34b'
_computing_structure_solution    'SuperFlip (Palatinus & Chapius, 2007)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0991P)²+0.7487P] 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         6314
_refine_ls_number_parameters     416
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0605
_refine_ls_wR_factor_ref         0.1769
_refine_ls_wR_factor_gt          0.1536
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_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 -0.0738(3) 0.0292(3) 0.9825(3) 0.0345(8) Uani 1 1 d . . . . .
C2 C 0.2712(5) -0.1920(5) 0.7987(4) 0.0709(14) Uani 1 1 d . . . . .
H2A H 0.2928 -0.2747 0.8053 0.106 Uiso 1 1 calc R U . . .
H2B H 0.3418 -0.1687 0.7569 0.106 Uiso 1 1 calc R U . . .
H2C H 0.2648 -0.1673 0.8660 0.106 Uiso 1 1 calc R U . . .
C3 C 0.1366(5) -0.1377(4) 0.7486(4) 0.0630(13) Uani 1 1 d . . . . .
C4 C 0.0807(6) -0.2116(5) 0.7031(4) 0.0688(14) Uani 1 1 d . . . . .
H4 H 0.1219 -0.2913 0.7115 0.083 Uiso 1 1 calc R U . . .
C5 C -0.0301(6) -0.1664(5) 0.6489(4) 0.0697(14) Uani 1 1 d . . . . .
H5 H -0.0715 -0.2148 0.6248 0.084 Uiso 1 1 calc R U . . .
C6 C -0.0855(5) -0.0459(5) 0.6277(4) 0.0613(13) Uani 1 1 d . . . . .
C7 C -0.1962(5) 0.0088(7) 0.5617(4) 0.0759(17) Uani 1 1 d . . . . .
H7 H -0.2395 -0.0364 0.5346 0.091 Uiso 1 1 calc R U . . .
C8 C -0.2390(5) 0.1236(6) 0.5381(4) 0.0739(16) Uani 1 1 d . . . . .
H8 H -0.3123 0.1575 0.4957 0.089 Uiso 1 1 calc R U . . .
C9 C -0.1728(4) 0.1944(5) 0.5775(4) 0.0659(14) Uani 1 1 d . . . . .
C10 C -0.2032(6) 0.3141(6) 0.5468(4) 0.0859(18) Uani 1 1 d . . . . .
H10 H -0.2737 0.3508 0.5026 0.103 Uiso 1 1 calc R U . . .
C11 C -0.1311(6) 0.3763(5) 0.5809(4) 0.0771(16) Uani 1 1 d . . . . .
H11 H -0.1459 0.4535 0.5545 0.092 Uiso 1 1 calc R U . . .
C12 C -0.0320(5) 0.3238(4) 0.6575(4) 0.0652(13) Uani 1 1 d . . . . .
C13 C 0.0502(6) 0.3911(5) 0.6905(5) 0.0778(15) Uani 1 1 d . . . . .
H13A H 0.0166 0.4702 0.6607 0.117 Uiso 1 1 calc R U . . .
H13B H 0.0433 0.3875 0.7645 0.117 Uiso 1 1 calc R U . . .
H13C H 0.1442 0.3593 0.6679 0.117 Uiso 1 1 calc R U . . .
C14 C -0.0692(4) 0.1462(4) 0.6468(3) 0.0525(11) Uani 1 1 d . . . . .
C15 C -0.0220(4) 0.0218(4) 0.6711(3) 0.0508(11) Uani 1 1 d . . . . .
C16 C 0.3695(5) 0.0476(5) 0.6408(3) 0.0612(12) Uani 1 1 d . . . . .
H16A H 0.4520 0.0132 0.6017 0.092 Uiso 1 1 calc R U . . .
H16B H 0.3153 -0.0047 0.6531 0.092 Uiso 1 1 calc R U . . .
H16C H 0.3183 0.1185 0.6028 0.092 Uiso 1 1 calc R U . . .
C17 C 0.4049(4) 0.0723(4) 0.7422(3) 0.0468(10) Uani 1 1 d . . . . .
C18 C 0.5420(4) 0.0489(4) 0.7641(4) 0.0570(11) Uani 1 1 d . . . . .
H18 H 0.6109 0.0135 0.7177 0.068 Uiso 1 1 calc R U . . .
C19 C 0.5753(4) 0.0775(4) 0.8530(4) 0.0564(11) Uani 1 1 d . . . . .
H19 H 0.6665 0.0589 0.8689 0.068 Uiso 1 1 calc R U . . .
C20 C 0.4711(4) 0.1353(4) 0.9202(3) 0.0457(10) Uani 1 1 d . . . . .
C21 C 0.4975(5) 0.1747(4) 1.0120(4) 0.0593(12) Uani 1 1 d . . . . .
H21 H 0.5873 0.1579 1.0309 0.071 Uiso 1 1 calc R U . . .
C22 C 0.3952(5) 0.2352(4) 1.0709(4) 0.0586(12) Uani 1 1 d . . . . .
H22 H 0.4150 0.2606 1.1298 0.070 Uiso 1 1 calc R U . . .
C23 C 0.2552(4) 0.2620(4) 1.0450(3) 0.0494(10) Uani 1 1 d . . . . .
C24 C 0.1444(5) 0.3301(4) 1.1017(4) 0.0612(12) Uani 1 1 d . . . . .
H24 H 0.1589 0.3562 1.1618 0.073 Uiso 1 1 calc R U . . .
C25 C 0.0162(5) 0.3574(4) 1.0679(4) 0.0627(12) Uani 1 1 d . . . . .
H25 H -0.0569 0.4051 1.1035 0.075 Uiso 1 1 calc R U . . .
C26 C -0.0067(4) 0.3144(4) 0.9801(3) 0.0522(10) Uani 1 1 d . . . . .
C27 C -0.1489(4) 0.3488(4) 0.9401(4) 0.0676(14) Uani 1 1 d . . . . .
H27A H -0.2120 0.3987 0.9847 0.101 Uiso 1 1 calc R U . . .
H27B H -0.1490 0.3887 0.8715 0.101 Uiso 1 1 calc R U . . .
H27C H -0.1761 0.2807 0.9387 0.101 Uiso 1 1 calc R U . . .
C28 C 0.2250(4) 0.2207(3) 0.9582(3) 0.0404(9) Uani 1 1 d . . . . .
C29 C 0.3353(3) 0.1553(3) 0.8944(3) 0.0374(8) Uani 1 1 d . . . . .
N1 N 0.0871(3) -0.0232(3) 0.7320(3) 0.0458(8) Uani 1 1 d . . . . .
N2 N -0.0032(3) 0.2120(3) 0.6898(3) 0.0484(8) Uani 1 1 d . . . . .
N3 N 0.3032(3) 0.1204(3) 0.8075(2) 0.0396(7) Uani 1 1 d . . . . .
N4 N 0.0957(3) 0.2442(3) 0.9272(3) 0.0420(8) Uani 1 1 d . . . . .
O1 O -0.0878(2) 0.0931(2) 0.8979(2) 0.0436(6) Uani 1 1 d . . . . .
O2 O 0.1681(2) -0.0099(2) 0.9584(2) 0.0414(6) Uani 1 1 d . . . . .
Zn2 Zn 0.09873(4) 0.11321(4) 0.82344(3) 0.04179(18) Uani 1 1 d . . . . .
Cl02 Cl -0.34321(13) -0.30378(11) 0.61048(10) 0.0652(3) Uani 1 1 d . . . . .
O3 O -0.3074(7) -0.3871(5) 0.6962(4) 0.135(2) Uani 1 1 d . . . . .
O4 O -0.3659(8) -0.1955(5) 0.6422(6) 0.182(3) Uani 1 1 d . . . . .
O5 O -0.2366(6) -0.3210(5) 0.5366(5) 0.142(2) Uani 1 1 d . . . . .
O6 O -0.4546(8) -0.3131(10) 0.5739(7) 0.227(4) Uani 1 1 d . . . . .
O7 O 0.2656(6) 0.5183(6) 0.7914(7) 0.171(3) Uani 1 1 d . . . . .
S1 S 0.37771(18) 0.4184(3) 0.78271(19) 0.0827(10) Uani 0.784(8) 1 d . . P A 1
S2 S 0.3764(10) 0.5030(13) 0.7496(12) 0.122(5) Uani 0.216(8) 1 d . . P A 2
C30 C 0.4429(11) 0.4185(12) 0.6578(8) 0.187(5) Uani 1 1 d . . . . .
H30A H 0.5193 0.3503 0.6520 0.280 Uiso 1 1 calc R U . A 1
H30B H 0.3735 0.4194 0.6130 0.280 Uiso 1 1 calc R U . A 1
H30C H 0.4724 0.4860 0.6382 0.280 Uiso 1 1 calc R U . A 1
C31 C 0.5212(11) 0.4379(11) 0.8347(10) 0.200(6) Uani 1 1 d . . . . .
H31A H 0.5986 0.3702 0.8293 0.300 Uiso 1 1 calc R U . A 1
H31B H 0.5421 0.5040 0.7970 0.300 Uiso 1 1 calc R U . A 1
H31C H 0.5008 0.4499 0.9061 0.300 Uiso 1 1 calc R U . A 1


_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 O2 1.246(4) 2_557 ?
C1 O1 1.256(4) . ?
C1 C1 1.545(6) 2_557 ?
C2 C3 1.504(6) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 N1 1.328(6) . ?
C3 C4 1.427(6) . ?
C4 C5 1.324(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.404(8) . ?
C5 H5 0.9300 . ?
C6 C15 1.404(6) . ?
C6 C7 1.426(7) . ?
C7 C8 1.336(8) . ?
C7 H7 0.9300 . ?
C8 C9 1.427(8) . ?
C8 H8 0.9300 . ?
C9 C14 1.394(6) . ?
C9 C10 1.407(9) . ?
C10 C11 1.355(9) . ?
C10 H10 0.9300 . ?
C11 C12 1.434(7) . ?
C11 H11 0.9300 . ?
C12 N2 1.322(6) . ?
C12 C13 1.476(7) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 N2 1.400(6) . ?
C14 C15 1.445(7) . ?
C15 N1 1.361(5) . ?
C16 C17 1.501(6) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 N3 1.330(5) . ?
C17 C18 1.398(6) . ?
C18 C19 1.361(6) . ?
C18 H18 0.9300 . ?
C19 C20 1.399(6) . ?
C19 H19 0.9300 . ?
C20 C29 1.405(5) . ?
C20 C21 1.433(6) . ?
C21 C22 1.334(7) . ?
C21 H21 0.9300 . ?
C22 C23 1.436(6) . ?
C22 H22 0.9300 . ?
C23 C28 1.401(6) . ?
C23 C24 1.406(7) . ?
C24 C25 1.355(7) . ?
C24 H24 0.9300 . ?
C25 C26 1.396(7) . ?
C25 H25 0.9300 . ?
C26 N4 1.343(5) . ?
C26 C27 1.512(6) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 N4 1.358(5) . ?
C28 C29 1.442(5) . ?
C29 N3 1.369(5) . ?
N1 Zn2 2.223(3) . ?
N2 Zn2 2.139(3) . ?
N3 Zn2 2.123(3) . ?
N4 Zn2 2.232(3) . ?
O1 Zn2 2.141(3) . ?
O2 C1 1.246(4) 2_557 ?
O2 Zn2 2.172(3) . ?
Cl02 O6 1.323(6) . ?
Cl02 O5 1.380(5) . ?
Cl02 O4 1.388(6) . ?
Cl02 O3 1.399(5) . ?
O7 S2 1.191(13) . ?
O7 S1 1.408(6) . ?
S1 C30 1.710(10) . ?
S1 C31 1.773(8) . ?
S2 C30 1.655(15) . ?
S2 C31 1.847(14) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 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
O2 C1 O1 125.9(3) 2_557 . ?
O2 C1 C1 117.0(4) 2_557 2_557 ?
O1 C1 C1 117.1(4) . 2_557 ?
C3 C2 H2A 109.5 . . ?
C3 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C3 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N1 C3 C4 121.9(4) . . ?
N1 C3 C2 119.5(4) . . ?
C4 C3 C2 117.5(5) . . ?
C5 C4 C3 119.7(5) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 120.5(5) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C15 C6 C5 116.6(4) . . ?
C15 C6 C7 119.7(5) . . ?
C5 C6 C7 123.6(5) . . ?
C8 C7 C6 121.3(5) . . ?
C8 C7 H7 119.3 . . ?
C6 C7 H7 119.3 . . ?
C7 C8 C9 120.3(4) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 H8 119.9 . . ?
C14 C9 C10 116.3(5) . . ?
C14 C9 C8 120.8(5) . . ?
C10 C9 C8 122.9(5) . . ?
C11 C10 C9 120.8(5) . . ?
C11 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
C10 C11 C12 120.3(5) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
N2 C12 C11 120.2(5) . . ?
N2 C12 C13 119.7(4) . . ?
C11 C12 C13 119.7(5) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C9 C14 N2 123.1(5) . . ?
C9 C14 C15 118.6(4) . . ?
N2 C14 C15 118.2(3) . . ?
N1 C15 C6 123.6(5) . . ?
N1 C15 C14 117.2(4) . . ?
C6 C15 C14 119.1(4) . . ?
C17 C16 H16A 109.5 . . ?
C17 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C17 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N3 C17 C18 121.8(4) . . ?
N3 C17 C16 118.3(3) . . ?
C18 C17 C16 119.8(4) . . ?
C19 C18 C17 120.4(4) . . ?
C19 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
C18 C19 C20 119.4(4) . . ?
C18 C19 H19 120.3 . . ?
C20 C19 H19 120.3 . . ?
C19 C20 C29 117.4(4) . . ?
C19 C20 C21 122.9(4) . . ?
C29 C20 C21 119.7(4) . . ?
C22 C21 C20 120.9(4) . . ?
C22 C21 H21 119.5 . . ?
C20 C21 H21 119.5 . . ?
C21 C22 C23 121.2(4) . . ?
C21 C22 H22 119.4 . . ?
C23 C22 H22 119.4 . . ?
C28 C23 C24 117.1(4) . . ?
C28 C23 C22 119.4(4) . . ?
C24 C23 C22 123.4(4) . . ?
C25 C24 C23 119.5(4) . . ?
C25 C24 H24 120.3 . . ?
C23 C24 H24 120.3 . . ?
C24 C25 C26 120.4(4) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
N4 C26 C25 121.7(4) . . ?
N4 C26 C27 118.0(4) . . ?
C25 C26 C27 120.3(4) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N4 C28 C23 123.1(4) . . ?
N4 C28 C29 117.4(3) . . ?
C23 C28 C29 119.4(3) . . ?
N3 C29 C20 122.5(4) . . ?
N3 C29 C28 118.2(3) . . ?
C20 C29 C28 119.2(3) . . ?
C3 N1 C15 117.3(4) . . ?
C3 N1 Zn2 130.9(3) . . ?
C15 N1 Zn2 108.3(3) . . ?
C12 N2 C14 118.9(4) . . ?
C12 N2 Zn2 130.4(3) . . ?
C14 N2 Zn2 109.3(3) . . ?
C17 N3 C29 118.2(3) . . ?
C17 N3 Zn2 129.6(3) . . ?
C29 N3 Zn2 110.0(2) . . ?
C26 N4 C28 118.0(3) . . ?
C26 N4 Zn2 132.0(3) . . ?
C28 N4 Zn2 107.5(2) . . ?
C1 O1 Zn2 114.7(2) . . ?
C1 O2 Zn2 114.1(2) 2_557 . ?
N3 Zn2 N2 107.20(12) . . ?
N3 Zn2 O1 158.74(11) . . ?
N2 Zn2 O1 92.42(11) . . ?
N3 Zn2 O2 84.72(10) . . ?
N2 Zn2 O2 166.46(11) . . ?
O1 Zn2 O2 76.89(9) . . ?
N3 Zn2 N1 107.64(12) . . ?
N2 Zn2 N1 77.46(13) . . ?
O1 Zn2 N1 84.15(11) . . ?
O2 Zn2 N1 93.01(11) . . ?
N3 Zn2 N4 77.03(12) . . ?
N2 Zn2 N4 104.80(13) . . ?
O1 Zn2 N4 90.33(11) . . ?
O2 Zn2 N4 83.82(11) . . ?
N1 Zn2 N4 174.14(12) . . ?
O6 Cl02 O5 110.9(5) . . ?
O6 Cl02 O4 111.4(6) . . ?
O5 Cl02 O4 108.3(4) . . ?
O6 Cl02 O3 108.1(5) . . ?
O5 Cl02 O3 109.8(4) . . ?
O4 Cl02 O3 108.3(4) . . ?
O7 S1 C30 109.6(6) . . ?
O7 S1 C31 108.6(6) . . ?
C30 S1 C31 95.7(6) . . ?
O7 S2 C30 126.8(11) . . ?
O7 S2 C31 115.4(12) . . ?
C30 S2 C31 94.9(8) . . ?
S1 C30 H30A 109.5 . . ?
S1 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
S1 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
S1 C31 H31A 109.5 . . ?
S1 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
S1 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 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 C3 C4 C5 -5.2(8) . . . . ?
C2 C3 C4 C5 -173.1(5) . . . . ?
C3 C4 C5 C6 6.0(8) . . . . ?
C4 C5 C6 C15 -3.3(7) . . . . ?
C4 C5 C6 C7 173.7(5) . . . . ?
C15 C6 C7 C8 1.7(8) . . . . ?
C5 C6 C7 C8 -175.2(5) . . . . ?
C6 C7 C8 C9 1.0(8) . . . . ?
C7 C8 C9 C14 -4.5(8) . . . . ?
C7 C8 C9 C10 173.0(5) . . . . ?
C14 C9 C10 C11 2.3(8) . . . . ?
C8 C9 C10 C11 -175.4(5) . . . . ?
C9 C10 C11 C12 -6.6(9) . . . . ?
C10 C11 C12 N2 4.9(9) . . . . ?
C10 C11 C12 C13 177.3(6) . . . . ?
C10 C9 C14 N2 3.9(7) . . . . ?
C8 C9 C14 N2 -178.4(4) . . . . ?
C10 C9 C14 C15 -172.4(4) . . . . ?
C8 C9 C14 C15 5.2(7) . . . . ?
C5 C6 C15 N1 -0.6(7) . . . . ?
C7 C6 C15 N1 -177.7(4) . . . . ?
C5 C6 C15 C14 176.3(4) . . . . ?
C7 C6 C15 C14 -0.9(7) . . . . ?
C9 C14 C15 N1 174.5(4) . . . . ?
N2 C14 C15 N1 -2.1(6) . . . . ?
C9 C14 C15 C6 -2.6(6) . . . . ?
N2 C14 C15 C6 -179.1(4) . . . . ?
N3 C17 C18 C19 -1.5(7) . . . . ?
C16 C17 C18 C19 175.9(5) . . . . ?
C17 C18 C19 C20 -2.8(7) . . . . ?
C18 C19 C20 C29 3.3(7) . . . . ?
C18 C19 C20 C21 -176.1(5) . . . . ?
C19 C20 C21 C22 176.1(5) . . . . ?
C29 C20 C21 C22 -3.3(7) . . . . ?
C20 C21 C22 C23 0.6(8) . . . . ?
C21 C22 C23 C28 2.0(7) . . . . ?
C21 C22 C23 C24 -176.8(5) . . . . ?
C28 C23 C24 C25 -3.2(7) . . . . ?
C22 C23 C24 C25 175.7(5) . . . . ?
C23 C24 C25 C26 2.7(8) . . . . ?
C24 C25 C26 N4 0.8(7) . . . . ?
C24 C25 C26 C27 -177.6(5) . . . . ?
C24 C23 C28 N4 0.4(6) . . . . ?
C22 C23 C28 N4 -178.5(4) . . . . ?
C24 C23 C28 C29 176.9(4) . . . . ?
C22 C23 C28 C29 -2.0(6) . . . . ?
C19 C20 C29 N3 0.2(6) . . . . ?
C21 C20 C29 N3 179.6(4) . . . . ?
C19 C20 C29 C28 -176.3(4) . . . . ?
C21 C20 C29 C28 3.2(6) . . . . ?
N4 C28 C29 N3 -0.5(5) . . . . ?
C23 C28 C29 N3 -177.2(4) . . . . ?
N4 C28 C29 C20 176.1(4) . . . . ?
C23 C28 C29 C20 -0.6(6) . . . . ?
C4 C3 N1 C15 1.4(7) . . . . ?
C2 C3 N1 C15 169.1(5) . . . . ?
C4 C3 N1 Zn2 157.6(4) . . . . ?
C2 C3 N1 Zn2 -34.7(7) . . . . ?
C6 C15 N1 C3 1.4(6) . . . . ?
C14 C15 N1 C3 -175.5(4) . . . . ?
C6 C15 N1 Zn2 -159.9(4) . . . . ?
C14 C15 N1 Zn2 23.3(4) . . . . ?
C11 C12 N2 C14 1.1(7) . . . . ?
C13 C12 N2 C14 -171.3(5) . . . . ?
C11 C12 N2 Zn2 -163.8(4) . . . . ?
C13 C12 N2 Zn2 23.8(7) . . . . ?
C9 C14 N2 C12 -5.6(7) . . . . ?
C15 C14 N2 C12 170.8(4) . . . . ?
C9 C14 N2 Zn2 162.3(4) . . . . ?
C15 C14 N2 Zn2 -21.4(4) . . . . ?
C18 C17 N3 C29 5.0(6) . . . . ?
C16 C17 N3 C29 -172.5(4) . . . . ?
C18 C17 N3 Zn2 -156.1(3) . . . . ?
C16 C17 N3 Zn2 26.4(6) . . . . ?
C20 C29 N3 C17 -4.4(6) . . . . ?
C28 C29 N3 C17 172.1(4) . . . . ?
C20 C29 N3 Zn2 160.3(3) . . . . ?
C28 C29 N3 Zn2 -23.3(4) . . . . ?
C25 C26 N4 C28 -3.6(6) . . . . ?
C27 C26 N4 C28 174.8(4) . . . . ?
C25 C26 N4 Zn2 155.8(4) . . . . ?
C27 C26 N4 Zn2 -25.8(6) . . . . ?
C23 C28 N4 C26 3.0(6) . . . . ?
C29 C28 N4 C26 -173.6(4) . . . . ?
C23 C28 N4 Zn2 -161.1(3) . . . . ?
C29 C28 N4 Zn2 22.3(4) . . . . ?
O2 C1 O1 Zn2 176.2(3) 2_557 . . . ?
C1 C1 O1 Zn2 -2.8(5) 2_557 . . . ?

_refine_diff_density_max         1.066
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.080



####################################################################### 
# 
# 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_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1818143'
_audit_update_record             
;
2018-01-19 deposited with the CCDC.
2018-03-28 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         ?
_chemical_formula_sum            'C62 H60 Cl2 Co2 N8 O14 S2'
_chemical_formula_weight         1394.06

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      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                   10.3328(10)
_cell_length_b                   12.2165(12)
_cell_length_c                   13.0629(12)
_cell_angle_alpha                82.207(8)
_cell_angle_beta                 84.709(8)
_cell_angle_gamma                71.837(9)
_cell_volume                     1550.1(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    4987
_cell_measurement_theta_min      2.3460
_cell_measurement_theta_max      22.4790

_exptl_crystal_description       
;
'Thu Jun 18 12:11:23 2015'
;
_exptl_crystal_colour            Plate
_exptl_crystal_density_meas      Pink
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_F_000             720
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    0.761
_shelx_estimated_absorpt_T_min   0.863
_shelx_estimated_absorpt_T_max   0.942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.92458
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
'Thu Jun 18 12:11:23 2015'
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  
'Saxi-CrysAlisPro-abstract goniometer imported S'
_diffrn_measurement_method       'ω and π scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            43439
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.282
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6331
_reflns_number_gt                4523
_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       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'CysAlisPro 171.37.34b'
_computing_data_reduction        'CysAlisPro 171.37.34b'
_computing_structure_solution    'SuperFlip (Palatinus & Chapius, 2007)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0611P)²+1.3647P] 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         6331
_refine_ls_number_parameters     422
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0506
_refine_ls_wR_factor_ref         0.1409
_refine_ls_wR_factor_gt          0.1205
_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 0.4267(3) 0.5278(3) 0.4812(2) 0.0302(6) Uani 1 1 d . . . . .
C2 C 0.5562(5) 0.8915(4) 0.1930(3) 0.0679(11) Uani 1 1 d . . . . .
H2A H 0.6265 0.8404 0.2353 0.102 Uiso 1 1 calc R U . . .
H2B H 0.4976 0.9502 0.2326 0.102 Uiso 1 1 calc R U . . .
H2C H 0.5968 0.9274 0.1342 0.102 Uiso 1 1 calc R U . . .
C3 C 0.4750(4) 0.8241(3) 0.1569(3) 0.0514(9) Uani 1 1 d . . . . .
C4 C 0.3753(5) 0.8785(4) 0.0828(3) 0.0681(12) Uani 1 1 d . . . . .
H4 H 0.3594 0.9565 0.0587 0.082 Uiso 1 1 calc R U . . .
C5 C 0.3031(4) 0.8170(4) 0.0471(3) 0.0727(13) Uani 1 1 d . . . . .
H5 H 0.2343 0.8542 0.0018 0.087 Uiso 1 1 calc R U . . .
C6 C 0.3316(3) 0.6990(4) 0.0778(3) 0.0552(10) Uani 1 1 d . . . . .
C7 C 0.2667(4) 0.6266(5) 0.0384(3) 0.0654(12) Uani 1 1 d . . . . .
H7 H 0.1948 0.6604 -0.0049 0.078 Uiso 1 1 calc R U . . .
C8 C 0.3070(4) 0.5120(5) 0.0625(3) 0.0658(12) Uani 1 1 d . . . . .
H8 H 0.2626 0.4674 0.0358 0.079 Uiso 1 1 calc R U . . .
C9 C 0.4174(4) 0.4562(4) 0.1286(3) 0.0507(9) Uani 1 1 d . . . . .
C10 C 0.4705(4) 0.3361(4) 0.1500(3) 0.0612(11) Uani 1 1 d . . . . .
H10 H 0.4291 0.2878 0.1258 0.073 Uiso 1 1 calc R U . . .
C11 C 0.5823(5) 0.2902(4) 0.2060(3) 0.0593(10) Uani 1 1 d . . . . .
H11 H 0.6208 0.2102 0.2170 0.071 Uiso 1 1 calc R U . . .
C12 C 0.6408(4) 0.3630(3) 0.2477(3) 0.0475(8) Uani 1 1 d . . . . .
C13 C 0.7714(4) 0.3103(3) 0.3018(3) 0.0618(11) Uani 1 1 d . . . . .
H13A H 0.7978 0.3703 0.3266 0.093 Uiso 1 1 calc R U . . .
H13B H 0.8416 0.2710 0.2543 0.093 Uiso 1 1 calc R U . . .
H13C H 0.7585 0.2559 0.3591 0.093 Uiso 1 1 calc R U . . .
C14 C 0.4796(3) 0.5246(3) 0.1728(2) 0.0406(8) Uani 1 1 d . . . . .
C15 C 0.4346(3) 0.6478(3) 0.1478(2) 0.0429(8) Uani 1 1 d . . . . .
C16 C 0.8685(4) 0.5467(4) 0.1388(3) 0.0531(9) Uani 1 1 d . . . . .
H16A H 0.7737 0.5517 0.1423 0.080 Uiso 1 1 calc R U . . .
H16B H 0.9228 0.4701 0.1250 0.080 Uiso 1 1 calc R U . . .
H16C H 0.8858 0.6024 0.0843 0.080 Uiso 1 1 calc R U . . .
C17 C 0.9047(3) 0.5714(3) 0.2393(2) 0.0397(7) Uani 1 1 d . . . . .
C18 C 1.0419(3) 0.5473(3) 0.2615(3) 0.0507(9) Uani 1 1 d . . . . .
H18 H 1.1104 0.5107 0.2151 0.061 Uiso 1 1 calc R U . . .
C19 C 1.0754(3) 0.5765(3) 0.3492(3) 0.0502(9) Uani 1 1 d . . . . .
H19 H 1.1664 0.5583 0.3643 0.060 Uiso 1 1 calc R U . . .
C20 C 0.9712(3) 0.6349(3) 0.4177(3) 0.0409(8) Uani 1 1 d . . . . .
C21 C 0.9980(4) 0.6746(4) 0.5091(3) 0.0548(10) Uani 1 1 d . . . . .
H21 H 1.0876 0.6585 0.5271 0.066 Uiso 1 1 calc R U . . .
C22 C 0.8953(4) 0.7349(4) 0.5694(3) 0.0543(10) Uani 1 1 d . . . . .
H22 H 0.9149 0.7596 0.6288 0.065 Uiso 1 1 calc R U . . .
C23 C 0.7559(4) 0.7618(3) 0.5438(3) 0.0438(8) Uani 1 1 d . . . . .
C24 C 0.6450(4) 0.8303(3) 0.5999(3) 0.0556(10) Uani 1 1 d . . . . .
H24 H 0.6594 0.8572 0.6598 0.067 Uiso 1 1 calc R U . . .
C25 C 0.5174(4) 0.8574(3) 0.5673(3) 0.0555(10) Uani 1 1 d . . . . .
H25 H 0.4447 0.9055 0.6032 0.067 Uiso 1 1 calc R U . . .
C26 C 0.4941(3) 0.8130(3) 0.4791(3) 0.0458(8) Uani 1 1 d . . . . .
C27 C 0.3533(4) 0.8480(4) 0.4394(3) 0.0616(11) Uani 1 1 d . . . . .
H27A H 0.3441 0.9105 0.3848 0.092 Uiso 1 1 calc R U . . .
H27B H 0.2869 0.8727 0.4947 0.092 Uiso 1 1 calc R U . . .
H27C H 0.3390 0.7830 0.4134 0.092 Uiso 1 1 calc R U . . .
C28 C 0.7262(3) 0.7200(3) 0.4571(2) 0.0343(7) Uani 1 1 d . . . . .
C29 C 0.8363(3) 0.6549(3) 0.3924(2) 0.0332(7) Uani 1 1 d . . . . .
N1 N 0.5884(3) 0.4784(2) 0.23375(19) 0.0375(6) Uani 1 1 d . . . . .
N2 N 0.5010(3) 0.7125(3) 0.1908(2) 0.0415(6) Uani 1 1 d . . . . .
N3 N 0.8039(2) 0.6197(2) 0.30541(19) 0.0347(6) Uani 1 1 d . . . . .
N4 N 0.5970(2) 0.7427(2) 0.42612(19) 0.0358(6) Uani 1 1 d . . . . .
O1 O 0.66691(19) 0.49490(19) 0.46078(15) 0.0361(5) Uani 1 1 d . . . . .
O2 O 0.4139(2) 0.59026(19) 0.39599(16) 0.0371(5) Uani 1 1 d . . . . .
Co1 Co 0.59968(4) 0.61265(4) 0.32512(3) 0.03432(15) Uani 1 1 d . . . . .
Cl1 Cl 0.15677(10) 0.19726(9) 0.11127(8) 0.0593(3) Uani 1 1 d . . . . .
O3 O 0.1921(5) 0.1133(4) 0.1972(3) 0.1245(16) Uani 1 1 d . . . . .
O4 O 0.0434(7) 0.1909(8) 0.0754(6) 0.222(4) Uani 1 1 d . . . . .
O5 O 0.1369(6) 0.3052(4) 0.1449(5) 0.159(2) Uani 1 1 d . . . . .
O6 O 0.2630(5) 0.1799(4) 0.0358(4) 0.1393(19) Uani 1 1 d . . . . .
O7 O 0.7689(5) 1.0200(5) 0.2951(5) 0.164(2) Uani 1 1 d . . . . .
S1A S 0.88038(15) 0.91905(19) 0.28383(15) 0.0759(8) Uani 0.775(6) 1 d . . P A 1
S1B S 0.8806(9) 1.0039(10) 0.2473(11) 0.137(5) Uani 0.225(6) 1 d . . P A 2
C30 C 0.9446(9) 0.9192(9) 0.1586(6) 0.173(4) Uani 1 1 d . . . . .
H30A H 1.0416 0.9038 0.1571 0.260 Uiso 1 1 calc R U . A 1
H30B H 0.9041 0.9935 0.1210 0.260 Uiso 1 1 calc R U . A 1
H30C H 0.9240 0.8603 0.1272 0.260 Uiso 1 1 calc R U . A 1
C31 C 1.0212(9) 0.9408(9) 0.3373(7) 0.191(5) Uani 1 1 d . . . . .
H31A H 1.0358 1.0114 0.3042 0.286 Uiso 1 1 calc R U . A 1
H31B H 1.1014 0.8769 0.3264 0.286 Uiso 1 1 calc R U . A 1
H31C H 1.0026 0.9459 0.4101 0.286 Uiso 1 1 calc R U . A 1


_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 O1 1.250(3) 2_666 ?
C1 O2 1.254(4) . ?
C1 C1 1.550(5) 2_666 ?
C2 C3 1.487(6) . ?
C3 N2 1.325(5) . ?
C3 C4 1.422(5) . ?
C4 C5 1.359(7) . ?
C5 C6 1.388(6) . ?
C6 C15 1.405(5) . ?
C6 C7 1.433(6) . ?
C7 C8 1.332(7) . ?
C8 C9 1.431(6) . ?
C9 C10 1.396(6) . ?
C9 C14 1.407(5) . ?
C10 C11 1.350(6) . ?
C11 C12 1.407(5) . ?
C12 N1 1.337(4) . ?
C12 C13 1.499(5) . ?
C14 N1 1.366(4) . ?
C14 C15 1.430(5) . ?
C15 N2 1.394(4) . ?
C16 C17 1.491(5) . ?
C17 N3 1.330(4) . ?
C17 C18 1.404(5) . ?
C18 C19 1.350(5) . ?
C19 C20 1.409(5) . ?
C20 C29 1.401(4) . ?
C20 C21 1.428(5) . ?
C21 C22 1.343(5) . ?
C22 C23 1.434(5) . ?
C23 C28 1.399(4) . ?
C23 C24 1.401(5) . ?
C24 C25 1.350(5) . ?
C25 C26 1.407(5) . ?
C26 N4 1.343(4) . ?
C26 C27 1.504(5) . ?
C28 N4 1.364(4) . ?
C28 C29 1.443(4) . ?
C29 N3 1.371(4) . ?
N1 Co1 2.192(3) . ?
N2 Co1 2.140(3) . ?
N3 Co1 2.129(2) . ?
N4 Co1 2.190(3) . ?
O1 C1 1.250(3) 2_666 ?
O1 Co1 2.146(2) . ?
O2 Co1 2.133(2) . ?
Cl1 O4 1.329(5) . ?
Cl1 O6 1.391(4) . ?
Cl1 O5 1.395(4) . ?
Cl1 O3 1.405(4) . ?
O7 S1B 1.233(11) . ?
O7 S1A 1.415(5) . ?
S1A C30 1.708(8) . ?
S1A C31 1.777(7) . ?
S1B C30 1.615(13) . ?
S1B C31 1.859(12) . ?

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
O1 C1 O2 126.7(3) 2_666 . ?
O1 C1 C1 116.2(3) 2_666 2_666 ?
O2 C1 C1 117.1(3) . 2_666 ?
N2 C3 C4 120.8(4) . . ?
N2 C3 C2 119.4(3) . . ?
C4 C3 C2 119.7(4) . . ?
C5 C4 C3 120.3(4) . . ?
C4 C5 C6 120.4(4) . . ?
C5 C6 C15 117.4(4) . . ?
C5 C6 C7 123.8(4) . . ?
C15 C6 C7 118.8(4) . . ?
C8 C7 C6 121.5(4) . . ?
C7 C8 C9 121.2(4) . . ?
C10 C9 C14 117.3(3) . . ?
C10 C9 C8 123.6(4) . . ?
C14 C9 C8 119.1(4) . . ?
C11 C10 C9 119.8(3) . . ?
C10 C11 C12 120.3(4) . . ?
N1 C12 C11 121.7(3) . . ?
N1 C12 C13 119.0(3) . . ?
C11 C12 C13 119.1(4) . . ?
N1 C14 C9 122.9(3) . . ?
N1 C14 C15 117.5(3) . . ?
C9 C14 C15 119.4(3) . . ?
N2 C15 C6 122.2(4) . . ?
N2 C15 C14 117.9(3) . . ?
C6 C15 C14 119.9(3) . . ?
N3 C17 C18 121.3(3) . . ?
N3 C17 C16 118.2(3) . . ?
C18 C17 C16 120.4(3) . . ?
C19 C18 C17 120.8(3) . . ?
C18 C19 C20 119.4(3) . . ?
C29 C20 C19 117.2(3) . . ?
C29 C20 C21 119.9(3) . . ?
C19 C20 C21 122.9(3) . . ?
C22 C21 C20 120.7(3) . . ?
C21 C22 C23 121.2(3) . . ?
C28 C23 C24 116.8(3) . . ?
C28 C23 C22 119.3(3) . . ?
C24 C23 C22 123.9(3) . . ?
C25 C24 C23 120.3(3) . . ?
C24 C25 C26 120.2(3) . . ?
N4 C26 C25 121.2(3) . . ?
N4 C26 C27 118.4(3) . . ?
C25 C26 C27 120.3(3) . . ?
N4 C28 C23 123.4(3) . . ?
N4 C28 C29 117.0(3) . . ?
C23 C28 C29 119.6(3) . . ?
N3 C29 C20 122.6(3) . . ?
N3 C29 C28 118.1(2) . . ?
C20 C29 C28 119.2(3) . . ?
C12 N1 C14 117.8(3) . . ?
C12 N1 Co1 131.3(2) . . ?
C14 N1 Co1 108.1(2) . . ?
C3 N2 C15 118.6(3) . . ?
C3 N2 Co1 131.2(2) . . ?
C15 N2 Co1 109.0(2) . . ?
C17 N3 C29 118.4(3) . . ?
C17 N3 Co1 130.2(2) . . ?
C29 N3 Co1 109.08(18) . . ?
C26 N4 C28 118.0(3) . . ?
C26 N4 Co1 131.4(2) . . ?
C28 N4 Co1 107.95(19) . . ?
C1 O1 Co1 114.69(18) 2_666 . ?
C1 O2 Co1 114.48(17) . . ?
N3 Co1 O2 161.19(9) . . ?
N3 Co1 N2 105.25(10) . . ?
O2 Co1 N2 92.54(9) . . ?
N3 Co1 O1 85.52(9) . . ?
O2 Co1 O1 77.36(8) . . ?
N2 Co1 O1 168.16(9) . . ?
N3 Co1 N4 77.61(10) . . ?
O2 Co1 N4 92.37(9) . . ?
N2 Co1 N4 104.10(10) . . ?
O1 Co1 N4 82.73(9) . . ?
N3 Co1 N1 106.79(10) . . ?
O2 Co1 N1 82.65(9) . . ?
N2 Co1 N1 77.55(10) . . ?
O1 Co1 N1 94.84(9) . . ?
N4 Co1 N1 174.85(9) . . ?
O4 Cl1 O6 111.4(4) . . ?
O4 Cl1 O5 111.2(5) . . ?
O6 Cl1 O5 108.0(3) . . ?
O4 Cl1 O3 108.5(4) . . ?
O6 Cl1 O3 110.3(3) . . ?
O5 Cl1 O3 107.4(3) . . ?
O7 S1A C30 110.3(5) . . ?
O7 S1A C31 106.5(5) . . ?
C30 S1A C31 96.8(5) . . ?
O7 S1B C30 128.3(9) . . ?
O7 S1B C31 110.5(10) . . ?
C30 S1B C31 96.9(7) . . ?

_refine_diff_density_max         0.567
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.071



####################################################################### 
# 
# 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_shelx_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1818144'
_audit_update_record             
;
2018-01-19 deposited with the CCDC.
2018-03-28 downloaded from the CCDC.
;

_vrf_PLAT430_shelx               
;
PROBLEM: Short Inter D...A Contact O100 ..O101 . 1.89 Ang.
RESPONSE: Disodered water molecules.
;
_vrf_PLAT602_shelx               
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! Info
RESPONSE: SQUEEZE techinique aplied to treat the disodered water 
molecules problem.
;
_vrf_PLAT306_shelx               
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O110 Check
RESPONSE: Disodered water molecules.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C186 H144 N24 Nb2 Ni6 O52.19'
_chemical_formula_weight         4088.42

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'
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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'

_cell_length_a                   35.7961(16)
_cell_length_b                   33.5952(13)
_cell_length_c                   33.0784(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     39779(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    22433
_cell_measurement_theta_min      2.4820
_cell_measurement_theta_max      22.0200

_exptl_crystal_description       Block
_exptl_crystal_colour            'Light Blue'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_F_000             16764
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    0.750
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.96016
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
'Tue Mar 31 18:37:32 2015'
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  
'Saxi-CrysAlisPro-abstract goniometer imported S'
_diffrn_measurement_method       'ω and π scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            121551
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_theta_min         1.676
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             19513
_reflns_number_gt                15692
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.965
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'CysAlisPro 171.37.34b'
_computing_data_reduction        'CysAlisPro 171.37.34b'
_computing_structure_solution    'SuperFlip (Palatinus & Chapius, 2007)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
'Refined as a 2-component inversion twin.,SQUEEZE'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1213P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.000116(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.427(17)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         19513
_refine_ls_number_parameters     1198
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0640
_refine_ls_wR_factor_ref         0.1769
_refine_ls_wR_factor_gt          0.1644
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_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 0.2137(2) 0.0233(3) 0.1187(3) 0.0481(19) Uani 1 1 d . . . . .
C2 C 0.1957(2) -0.0178(2) 0.1284(2) 0.0382(16) Uani 1 1 d . . . . .
C3 C 0.2187(2) -0.0502(2) 0.2732(3) 0.0443(18) Uani 1 1 d . . . . .
C4 C 0.2483(2) -0.0205(2) 0.2903(3) 0.050(2) Uani 1 1 d . . . . .
C5 C 0.3030(3) 0.0431(3) 0.1962(3) 0.065(3) Uani 1 1 d . . . . .
C6 C 0.3058(3) 0.0002(3) 0.1795(3) 0.057(2) Uani 1 1 d . . . . .
C7 C 0.0000 0.0000 0.1992(3) 0.041(2) Uani 1 2 d S T P . .
C8 C 0.0000 0.0000 0.1523(4) 0.046(3) Uani 1 2 d S T P . .
C9 C -0.0841(3) 0.0506(4) 0.1340(4) 0.084(4) Uani 1 1 d . . . . .
H9A H -0.1076 0.0386 0.1273 0.127 Uiso 1 1 calc R U . . .
H9B H -0.0802 0.0736 0.1173 0.127 Uiso 1 1 calc R U . . .
H9C H -0.0643 0.0319 0.1296 0.127 Uiso 1 1 calc R U . . .
C10 C -0.0845(2) 0.0629(3) 0.1776(3) 0.059(2) Uani 1 1 d . . . . .
C11 C -0.1187(3) 0.0585(3) 0.2022(5) 0.081(4) Uani 1 1 d . . . . .
H11 H -0.1398 0.0470 0.1909 0.097 Uiso 1 1 calc R U . . .
C12 C -0.1195(3) 0.0706(4) 0.2392(5) 0.083(4) Uani 1 1 d . . . . .
H12 H -0.1405 0.0658 0.2549 0.099 Uiso 1 1 calc R U . . .
C13 C -0.0899(3) 0.0900(3) 0.2554(3) 0.069(3) Uani 1 1 d . . . . .
C14 C -0.0900(4) 0.1083(4) 0.2965(5) 0.097(5) Uani 1 1 d . . . . .
H14 H -0.1108 0.1048 0.3129 0.117 Uiso 1 1 calc R U . . .
C15 C -0.0614(4) 0.1295(4) 0.3105(4) 0.076(3) Uani 1 1 d . . . . .
H15 H -0.0625 0.1405 0.3363 0.091 Uiso 1 1 calc R U . . .
C16 C -0.0294(3) 0.1352(4) 0.2865(3) 0.070(3) Uani 1 1 d . . . . .
C17 C 0.0009(3) 0.1593(3) 0.2974(3) 0.068(3) Uani 1 1 d . . . . .
H17 H 0.0012 0.1705 0.3231 0.082 Uiso 1 1 calc R U . . .
C18 C 0.0286(3) 0.1667(3) 0.2732(4) 0.071(3) Uani 1 1 d . . . . .
H18 H 0.0475 0.1838 0.2813 0.086 Uiso 1 1 calc R U . . .
C19 C 0.0300(3) 0.1485(3) 0.2335(3) 0.061(2) Uani 1 1 d . . . . .
C20 C 0.0595(3) 0.1586(3) 0.2045(4) 0.074(3) Uani 1 1 d . . . . .
H20A H 0.0763 0.1775 0.2166 0.112 Uiso 1 1 calc R U . . .
H20B H 0.0731 0.1350 0.1973 0.112 Uiso 1 1 calc R U . . .
H20C H 0.0485 0.1700 0.1807 0.112 Uiso 1 1 calc R U . . .
C21 C -0.0269(2) 0.1168(2) 0.2474(3) 0.0466(19) Uani 1 1 d . . . . .
C22 C -0.0571(2) 0.0939(3) 0.2330(3) 0.052(2) Uani 1 1 d . . . . .
C23 C -0.0567(3) 0.1589(3) 0.1441(4) 0.081(3) Uani 1 1 d . . . . .
H23A H -0.0738 0.1768 0.1310 0.121 Uiso 1 1 calc R U . . .
H23B H -0.0699 0.1357 0.1530 0.121 Uiso 1 1 calc R U . . .
H23C H -0.0457 0.1720 0.1670 0.121 Uiso 1 1 calc R U . . .
C24 C -0.0260(3) 0.1468(3) 0.1144(3) 0.054(2) Uani 1 1 d . . . . .
C25 C -0.0253(3) 0.1638(3) 0.0768(3) 0.066(3) Uani 1 1 d . . . . .
H25 H -0.0443 0.1809 0.0688 0.079 Uiso 1 1 calc R U . . .
C26 C 0.0041(3) 0.1554(3) 0.0504(3) 0.069(3) Uani 1 1 d . . . . .
H26 H 0.0039 0.1653 0.0241 0.083 Uiso 1 1 calc R U . . .
C27 C 0.0340(3) 0.1317(3) 0.0640(3) 0.057(2) Uani 1 1 d . . . . .
C28 C 0.0667(4) 0.1251(3) 0.0409(3) 0.072(3) Uani 1 1 d . . . . .
H28 H 0.0684 0.1361 0.0152 0.086 Uiso 1 1 calc R U . . .
C29 C 0.0944(3) 0.1043(4) 0.0548(3) 0.072(3) Uani 1 1 d . . . . .
H29 H 0.1151 0.0999 0.0384 0.087 Uiso 1 1 calc R U . . .
C30 C 0.0936(3) 0.0875(3) 0.0956(3) 0.061(2) Uani 1 1 d . . . . .
C31 C 0.1228(3) 0.0670(3) 0.1130(4) 0.073(3) Uani 1 1 d . . . . .
H31 H 0.1442 0.0617 0.0980 0.088 Uiso 1 1 calc R U . . .
C32 C 0.1204(3) 0.0545(3) 0.1521(4) 0.068(3) Uani 1 1 d . . . . .
H32 H 0.1405 0.0413 0.1638 0.081 Uiso 1 1 calc R U . . .
C33 C 0.0886(3) 0.0612(3) 0.1746(4) 0.069(3) Uani 1 1 d . . . . .
C35 C 0.0870(3) 0.0503(4) 0.2179(3) 0.081(3) Uani 1 1 d . . . . .
H35A H 0.1102 0.0382 0.2258 0.122 Uiso 1 1 calc R U . . .
H35B H 0.0829 0.0738 0.2339 0.122 Uiso 1 1 calc R U . . .
H35C H 0.0670 0.0318 0.2223 0.122 Uiso 1 1 calc R U . . .
C36 C 0.0617(2) 0.0928(2) 0.1186(3) 0.0460(19) Uani 1 1 d . . . . .
C37 C 0.0304(2) 0.1154(2) 0.1027(3) 0.0457(19) Uani 1 1 d . . . . .
C38 C 0.2500 0.2500 0.1157(3) 0.032(2) Uani 1 2 d S T P . .
C39 C 0.2500 0.2500 0.1617(3) 0.036(2) Uani 1 2 d S T P . .
C40 C 0.3927(3) 0.1724(3) 0.1725(4) 0.077(3) Uani 1 1 d . . . . .
H40A H 0.4086 0.1535 0.1859 0.115 Uiso 1 1 calc R U . . .
H40B H 0.3696 0.1598 0.1653 0.115 Uiso 1 1 calc R U . . .
H40C H 0.4049 0.1820 0.1485 0.115 Uiso 1 1 calc R U . . .
C41 C 0.3849(2) 0.2073(3) 0.2008(3) 0.054(2) Uani 1 1 d . . . . .
C42 C 0.4025(3) 0.2083(3) 0.2386(4) 0.075(3) Uani 1 1 d . . . . .
H42 H 0.4187 0.1881 0.2465 0.089 Uiso 1 1 calc R U . . .
C43 C 0.3953(4) 0.2389(4) 0.2626(4) 0.082(4) Uani 1 1 d . . . . .
H43 H 0.4053 0.2389 0.2886 0.099 Uiso 1 1 calc R U . . .
C44 C 0.3733(3) 0.2709(4) 0.2506(3) 0.070(3) Uani 1 1 d . . . . .
C45 C 0.3659(5) 0.3060(5) 0.2726(5) 0.100(5) Uani 1 1 d . . . . .
H45 H 0.3750 0.3079 0.2988 0.120 Uiso 1 1 calc R U . . .
C46 C 0.3467(4) 0.3367(4) 0.2580(5) 0.091(5) Uani 1 1 d . . . . .
H46 H 0.3409 0.3583 0.2744 0.109 Uiso 1 1 calc R U . . .
C47 C 0.3355(3) 0.3360(3) 0.2188(5) 0.082(4) Uani 1 1 d . . . . .
C48 C 0.3193(3) 0.3688(3) 0.1993(7) 0.106(6) Uani 1 1 d . . . . .
H48 H 0.3143 0.3918 0.2141 0.127 Uiso 1 1 calc R U . . .
C49 C 0.3103(3) 0.3676(3) 0.1568(7) 0.108(6) Uani 1 1 d . . . . .
H49 H 0.3002 0.3898 0.1440 0.130 Uiso 1 1 calc R U . . .
C50 C 0.3172(2) 0.3320(2) 0.1348(4) 0.067(3) Uani 1 1 d . . . . .
C51 C 0.3110(4) 0.3311(4) 0.0910(5) 0.106(5) Uani 1 1 d . . . . .
H51A H 0.3016 0.3564 0.0822 0.159 Uiso 1 1 calc R U . . .
H51B H 0.3342 0.3255 0.0775 0.159 Uiso 1 1 calc R U . . .
H51C H 0.2932 0.3106 0.0846 0.159 Uiso 1 1 calc R U . . .
C52 C 0.3402(2) 0.3027(2) 0.1933(3) 0.052(2) Uani 1 1 d . . . . .
C53 C 0.3582(2) 0.2687(2) 0.2112(3) 0.0435(18) Uani 1 1 d . . . . .
C54 C 0.2867(3) 0.1556(3) 0.1878(3) 0.060(2) Uani 1 1 d . . . . .
H54A H 0.2726 0.1331 0.1972 0.091 Uiso 1 1 calc R U . . .
H54B H 0.3096 0.1575 0.2028 0.091 Uiso 1 1 calc R U . . .
H54C H 0.2724 0.1795 0.1917 0.091 Uiso 1 1 calc R U . . .
C55 C 0.2951(2) 0.1507(2) 0.1448(3) 0.0459(18) Uani 1 1 d . . . . .
C56 C 0.2818(3) 0.1169(2) 0.1241(3) 0.056(2) Uani 1 1 d . . . . .
H56 H 0.2674 0.0983 0.1380 0.067 Uiso 1 1 calc R U . . .
C57 C 0.2893(3) 0.1108(3) 0.0845(3) 0.061(2) Uani 1 1 d . . . . .
H57 H 0.2802 0.0884 0.0712 0.073 Uiso 1 1 calc R U . . .
C58 C 0.3110(3) 0.1385(3) 0.0639(3) 0.056(2) Uani 1 1 d . . . . .
C59 C 0.3221(3) 0.1338(4) 0.0217(3) 0.072(3) Uani 1 1 d . . . . .
H59 H 0.3127 0.1130 0.0063 0.086 Uiso 1 1 calc R U . . .
C60 C 0.3460(4) 0.1597(4) 0.0058(3) 0.085(4) Uani 1 1 d . . . . .
H60 H 0.3538 0.1556 -0.0207 0.102 Uiso 1 1 calc R U . . .
C61 C 0.3602(3) 0.1928(3) 0.0264(3) 0.065(3) Uani 1 1 d . . . . .
C62 C 0.3863(3) 0.2198(4) 0.0112(4) 0.082(3) Uani 1 1 d . . . . .
H62 H 0.3939 0.2176 -0.0155 0.099 Uiso 1 1 calc R U . . .
C63 C 0.4001(3) 0.2477(4) 0.0334(4) 0.077(3) Uani 1 1 d . . . . .
H63 H 0.4182 0.2644 0.0226 0.093 Uiso 1 1 calc R U . . .
C64 C 0.3882(3) 0.2534(3) 0.0745(3) 0.057(2) Uani 1 1 d . . . . .
C66 C 0.4057(3) 0.2840(3) 0.1013(4) 0.069(3) Uani 1 1 d . . . . .
H66A H 0.4246 0.2981 0.0865 0.104 Uiso 1 1 calc R U . . .
H66B H 0.3869 0.3024 0.1102 0.104 Uiso 1 1 calc R U . . .
H66C H 0.4167 0.2712 0.1243 0.104 Uiso 1 1 calc R U . . .
C67 C 0.3483(2) 0.1996(2) 0.0669(2) 0.0435(18) Uani 1 1 d . . . . .
C68 C 0.3235(2) 0.1716(2) 0.0859(3) 0.0402(16) Uani 1 1 d . . . . .
C69 C 0.7500 0.2500 0.1864(3) 0.027(2) Uani 1 2 d S T P . .
C70 C 0.7500 0.2500 0.2342(3) 0.040(3) Uani 1 2 d S T P . .
C71 C 0.6054(3) 0.1766(3) 0.1717(4) 0.072(3) Uani 1 1 d . . . . .
H71A H 0.5891 0.1593 0.1569 0.108 Uiso 1 1 calc R U . . .
H71B H 0.6278 0.1625 0.1788 0.108 Uiso 1 1 calc R U . . .
H71C H 0.5931 0.1854 0.1959 0.108 Uiso 1 1 calc R U . . .
C72 C 0.6151(3) 0.2115(2) 0.1465(3) 0.057(2) Uani 1 1 d . . . . .
C73 C 0.5996(3) 0.2149(4) 0.1070(4) 0.078(3) Uani 1 1 d . . . . .
H73 H 0.5842 0.1948 0.0972 0.094 Uiso 1 1 calc R U . . .
C74 C 0.6069(3) 0.2466(4) 0.0837(4) 0.076(3) Uani 1 1 d . . . . .
H74 H 0.5974 0.2479 0.0576 0.091 Uiso 1 1 calc R U . . .
C75 C 0.6286(3) 0.2772(3) 0.0984(3) 0.063(3) Uani 1 1 d . . . . .
C76 C 0.6351(4) 0.3132(4) 0.0769(3) 0.081(4) Uani 1 1 d . . . . .
H76 H 0.6268 0.3154 0.0504 0.097 Uiso 1 1 calc R U . . .
C77 C 0.6532(4) 0.3446(5) 0.0944(5) 0.094(5) Uani 1 1 d . . . . .
H77 H 0.6568 0.3679 0.0797 0.112 Uiso 1 1 calc R U . . .
C78 C 0.6672(3) 0.3418(3) 0.1361(4) 0.066(3) Uani 1 1 d . . . . .
C79 C 0.6839(3) 0.3735(3) 0.1582(5) 0.076(3) Uani 1 1 d . . . . .
H79 H 0.6899 0.3971 0.1451 0.092 Uiso 1 1 calc R U . . .
C80 C 0.6908(3) 0.3694(3) 0.1961(5) 0.075(3) Uani 1 1 d . . . . .
H80 H 0.6995 0.3912 0.2106 0.090 Uiso 1 1 calc R U . . .
C81 C 0.6856(3) 0.3334(2) 0.2160(3) 0.058(3) Uani 1 1 d . . . . .
C82 C 0.6935(4) 0.3303(3) 0.2606(4) 0.083(4) Uani 1 1 d . . . . .
H82A H 0.7029 0.3553 0.2703 0.124 Uiso 1 1 calc R U . . .
H82B H 0.6709 0.3237 0.2747 0.124 Uiso 1 1 calc R U . . .
H82C H 0.7118 0.3099 0.2652 0.124 Uiso 1 1 calc R U . . .
C83 C 0.6619(2) 0.3063(2) 0.1575(3) 0.047(2) Uani 1 1 d . . . . .
C84 C 0.6426(2) 0.2735(3) 0.1378(3) 0.0492(19) Uani 1 1 d . . . . .
C85 C 0.5954(3) 0.2894(3) 0.2439(4) 0.083(4) Uani 1 1 d . . . . .
H85A H 0.5764 0.3042 0.2577 0.125 Uiso 1 1 calc R U . . .
H85B H 0.6156 0.3069 0.2369 0.125 Uiso 1 1 calc R U . . .
H85C H 0.5852 0.2779 0.2198 0.125 Uiso 1 1 calc R U . . .
C86 C 0.6099(3) 0.2562(3) 0.2716(3) 0.061(3) Uani 1 1 d . . . . .
C87 C 0.5952(4) 0.2512(4) 0.3111(5) 0.090(4) Uani 1 1 d . . . . .
H87 H 0.5775 0.2689 0.3211 0.108 Uiso 1 1 calc R U . . .
C88 C 0.6066(4) 0.2217(5) 0.3329(4) 0.095(4) Uani 1 1 d . . . . .
H88 H 0.5967 0.2185 0.3587 0.113 Uiso 1 1 calc R U . . .
C89 C 0.6341(4) 0.1936(4) 0.3187(3) 0.079(3) Uani 1 1 d . . . . .
C90 C 0.6448(5) 0.1595(5) 0.3396(4) 0.105(5) Uani 1 1 d . . . . .
H90 H 0.6360 0.1553 0.3656 0.126 Uiso 1 1 calc R U . . .
C91 C 0.6677(4) 0.1324(4) 0.3227(4) 0.093(4) Uani 1 1 d . . . . .
H91 H 0.6748 0.1099 0.3372 0.111 Uiso 1 1 calc R U . . .
C92 C 0.6805(3) 0.1383(3) 0.2838(4) 0.071(3) Uani 1 1 d . . . . .
C93 C 0.7010(4) 0.1095(4) 0.2632(6) 0.098(5) Uani 1 1 d . . . . .
H93 H 0.7088 0.0868 0.2769 0.118 Uiso 1 1 calc R U . . .
C94 C 0.7099(4) 0.1140(3) 0.2235(6) 0.095(5) Uani 1 1 d . . . . .
H94 H 0.7218 0.0937 0.2095 0.113 Uiso 1 1 calc R U . . .
C95 C 0.7007(3) 0.1503(2) 0.2037(4) 0.061(2) Uani 1 1 d . . . . .
C96 C 0.7096(3) 0.1558(3) 0.1602(3) 0.078(3) Uani 1 1 d . . . . .
H96A H 0.7232 0.1330 0.1505 0.116 Uiso 1 1 calc R U . . .
H96B H 0.6869 0.1586 0.1450 0.116 Uiso 1 1 calc R U . . .
H96C H 0.7246 0.1792 0.1568 0.116 Uiso 1 1 calc R U . . .
C97 C 0.6715(3) 0.1725(3) 0.2620(3) 0.052(2) Uani 1 1 d . . . . .
C98 C 0.6472(2) 0.2009(3) 0.2802(3) 0.049(2) Uani 1 1 d . . . . .
N1 N -0.05506(17) 0.0803(2) 0.1943(2) 0.0481(17) Uani 1 1 d . . . . .
N2 N 0.00332(18) 0.12252(19) 0.2233(2) 0.0441(15) Uani 1 1 d . . . . .
N3 N 0.00119(18) 0.1213(2) 0.1273(2) 0.0460(16) Uani 1 1 d . . . . .
N4 N 0.0582(2) 0.07885(19) 0.1579(2) 0.0470(16) Uani 1 1 d . . . . .
N5 N 0.36316(18) 0.23633(18) 0.1869(2) 0.0403(14) Uani 1 1 d . . . . .
N6 N 0.33021(19) 0.29969(19) 0.1529(3) 0.0512(19) Uani 1 1 d . . . . .
N7 N 0.31435(16) 0.17808(17) 0.12521(18) 0.0340(13) Uani 1 1 d . . . . .
N8 N 0.36097(18) 0.23048(19) 0.0896(2) 0.0426(15) Uani 1 1 d . . . . .
N9 N 0.6373(2) 0.23963(18) 0.1607(2) 0.0446(16) Uani 1 1 d . . . . .
N10 N 0.67237(18) 0.30195(18) 0.1965(2) 0.0417(15) Uani 1 1 d . . . . .
N11 N 0.6365(2) 0.2329(2) 0.2570(2) 0.0460(16) Uani 1 1 d . . . . .
N12 N 0.6817(2) 0.17882(19) 0.2230(2) 0.0474(17) Uani 1 1 d . . . . .
O1 O 0.19316(18) 0.04045(17) 0.2264(2) 0.0604(16) Uani 1 1 d . . . . .
O2 O 0.22707(18) 0.03933(16) 0.1498(2) 0.0574(16) Uani 1 1 d . . . . .
O3 O 0.2125(3) 0.0372(2) 0.0851(2) 0.081(2) Uani 1 1 d . . . . .
O4 O 0.1811(2) -0.03850(18) 0.1028(2) 0.0659(18) Uani 1 1 d . . . . .
O5 O 0.19750(16) -0.02612(15) 0.16587(17) 0.0478(13) Uani 1 1 d . . . . .
O6 O 0.20940(16) -0.04208(15) 0.23756(17) 0.0471(13) Uani 1 1 d . . . . .
O7 O 0.20703(18) -0.07716(16) 0.29401(18) 0.0543(14) Uani 1 1 d . . . . .
O8 O 0.25654(19) 0.00644(16) 0.2640(2) 0.0549(15) Uani 1 1 d . . . . .
O9 O 0.2610(3) -0.0233(3) 0.3236(2) 0.093(3) Uani 1 1 d . . . . .
O10 O 0.27038(17) 0.05243(15) 0.2074(2) 0.0560(14) Uani 1 1 d . . . . .
O11 O 0.3294(2) 0.0654(3) 0.1957(3) 0.100(3) Uani 1 1 d . . . . .
O12 O 0.27670(19) -0.0209(2) 0.1832(2) 0.0633(16) Uani 1 1 d . . . . .
O13 O 0.3369(2) -0.0119(3) 0.1668(3) 0.087(3) Uani 1 1 d . . . . .
O14 O 0.00353(17) 0.03335(16) 0.21602(17) 0.0494(14) Uani 1 1 d . . . . .
O15 O -0.00103(17) 0.03316(16) 0.13568(18) 0.0512(14) Uani 1 1 d . . . . .
O16 O 0.28110(15) 0.24678(16) 0.09743(16) 0.0412(12) Uani 1 1 d . . . . .
O17 O 0.28084(14) 0.24387(14) 0.17855(16) 0.0365(11) Uani 1 1 d . . . . .
O18 O 0.71954(17) 0.24377(16) 0.16968(17) 0.0446(13) Uani 1 1 d . . . . .
O19 O 0.71926(16) 0.24561(16) 0.25009(16) 0.0406(12) Uani 1 1 d . . . . .
O100 O 0.2378(4) 0.2153(4) 0.2724(4) 0.082(6) Uiso 0.60(3) 1 d . . P . .
O101 O 0.2161(7) 0.2590(7) 0.2828(8) 0.234(9) Uiso 1 1 d . . . . .
O102 O 0.7165(5) 0.2389(5) 0.0677(6) 0.123(9) Uiso 0.67(4) 1 d . . P . .
O103 O 0.7393(6) 0.2871(6) 0.0730(6) 0.118(10) Uiso 0.57(4) 1 d . . P . .
O105 O 0.6371(4) 0.0842(4) 0.1429(5) 0.151(5) Uiso 1 1 d . . . . .
O108 O 0.4143(11) 0.0510(12) 0.1951(13) 0.370(18) Uiso 1 1 d . . . . .
O110 O 0.4474(16) 0.0805(17) 0.2291(16) 0.47(3) Uiso 1 1 d . . . . .
O111 O 0.7285(12) 0.2583(15) 0.3571(15) 0.43(3) Uiso 1 1 d . . . . .
O112 O 0.4366(12) 0.1169(13) 0.2473(13) 0.12(2) Uiso 0.27(4) 1 d . . P . .
Ni1 Ni 0.00171(3) 0.08098(2) 0.17568(3) 0.0421(2) Uani 1 1 d . . . . .
Ni2 Ni 0.32515(2) 0.23872(2) 0.13851(3) 0.0342(2) Uani 1 1 d . . . . .
Ni3 Ni 0.67450(3) 0.23977(2) 0.20945(3) 0.0363(2) Uani 1 1 d . . . . .
Nb1 Nb 0.22720(2) 0.00969(2) 0.20760(2) 0.03800(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 O3 1.205(11) . ?
C1 O2 1.256(10) . ?
C1 C2 1.558(11) . ?
C2 O4 1.213(9) . ?
C2 O5 1.272(9) . ?
C3 O7 1.212(10) . ?
C3 O6 1.254(10) . ?
C3 C4 1.560(11) . ?
C4 O9 1.196(11) . ?
C4 O8 1.289(11) . ?
C5 O11 1.206(12) . ?
C5 O10 1.265(12) . ?
C5 C6 1.547(15) . ?
C6 O13 1.257(12) . ?
C6 O12 1.267(11) . ?
C7 O14 1.257(8) . ?
C7 O14 1.257(8) 2 ?
C7 C8 1.551(14) . ?
C8 O15 1.243(8) . ?
C8 O15 1.243(8) 2 ?
C9 C10 1.500(17) . ?
C10 N1 1.323(11) . ?
C10 C11 1.478(17) . ?
C11 C12 1.288(19) . ?
C12 C13 1.354(18) . ?
C13 C22 1.395(13) . ?
C13 C14 1.49(2) . ?
C14 C15 1.33(2) . ?
C15 C16 1.408(16) . ?
C16 C17 1.401(15) . ?
C16 C21 1.436(14) . ?
C17 C18 1.297(16) . ?
C18 C19 1.448(15) . ?
C19 N2 1.337(11) . ?
C19 C20 1.467(15) . ?
C21 N2 1.359(11) . ?
C21 C22 1.410(12) . ?
C22 N1 1.360(12) . ?
C23 C24 1.529(15) . ?
C24 N3 1.366(11) . ?
C24 C25 1.370(14) . ?
C25 C26 1.396(15) . ?
C26 C27 1.406(14) . ?
C27 C37 1.397(13) . ?
C27 C28 1.417(15) . ?
C28 C29 1.296(17) . ?
C29 C30 1.462(16) . ?
C30 C31 1.378(15) . ?
C30 C36 1.382(13) . ?
C31 C32 1.362(17) . ?
C32 C33 1.378(16) . ?
C33 N4 1.359(11) . ?
C33 C35 1.479(16) . ?
C36 N4 1.388(11) . ?
C36 C37 1.454(12) . ?
C37 N3 1.340(11) . ?
C38 O16 1.271(8) 14 ?
C38 O16 1.271(8) . ?
C38 C39 1.520(15) . ?
C39 O17 1.254(7) . ?
C39 O17 1.254(7) 14 ?
C40 C41 1.527(15) . ?
C41 N5 1.330(11) . ?
C41 C42 1.398(15) . ?
C42 C43 1.326(18) . ?
C43 C44 1.390(18) . ?
C44 C45 1.412(18) . ?
C44 C53 1.414(15) . ?
C45 C46 1.33(2) . ?
C46 C47 1.36(2) . ?
C47 C48 1.40(2) . ?
C47 C52 1.411(14) . ?
C48 C49 1.44(2) . ?
C49 C50 1.421(18) . ?
C50 N6 1.325(11) . ?
C50 C51 1.47(2) . ?
C52 N6 1.390(12) . ?
C52 C53 1.438(13) . ?
C53 N5 1.363(10) . ?
C54 C55 1.465(13) . ?
C55 N7 1.320(10) . ?
C55 C56 1.409(12) . ?
C56 C57 1.354(14) . ?
C57 C58 1.389(14) . ?
C58 C68 1.400(12) . ?
C58 C59 1.461(14) . ?
C59 C60 1.329(18) . ?
C60 C61 1.399(17) . ?
C61 C62 1.397(16) . ?
C61 C67 1.425(12) . ?
C62 C63 1.289(18) . ?
C63 C64 1.437(16) . ?
C64 N8 1.339(11) . ?
C64 C66 1.496(15) . ?
C67 N8 1.357(11) . ?
C67 C68 1.438(11) . ?
C68 N7 1.360(10) . ?
C69 O18 1.241(7) . ?
C69 O18 1.241(7) 14_655 ?
C69 C70 1.581(14) . ?
C70 O19 1.228(7) . ?
C70 O19 1.228(7) 14_655 ?
C71 C72 1.479(14) . ?
C72 N9 1.322(11) . ?
C72 C73 1.424(15) . ?
C73 C74 1.339(19) . ?
C74 C75 1.377(17) . ?
C75 C84 1.402(14) . ?
C75 C76 1.423(16) . ?
C76 C77 1.37(2) . ?
C77 C78 1.470(19) . ?
C78 C83 1.401(12) . ?
C78 C79 1.421(17) . ?
C79 C80 1.287(18) . ?
C80 C81 1.390(15) . ?
C81 N10 1.325(11) . ?
C81 C82 1.504(16) . ?
C83 N10 1.353(11) . ?
C83 C84 1.454(12) . ?
C84 N9 1.379(11) . ?
C85 C86 1.534(16) . ?
C86 N11 1.323(12) . ?
C86 C87 1.420(17) . ?
C87 C88 1.29(2) . ?
C88 C89 1.44(2) . ?
C89 C98 1.377(14) . ?
C89 C90 1.39(2) . ?
C90 C91 1.35(2) . ?
C91 C92 1.381(19) . ?
C92 C93 1.390(19) . ?
C92 C97 1.394(13) . ?
C93 C94 1.36(2) . ?
C94 C95 1.423(15) . ?
C95 N12 1.336(11) . ?
C95 C96 1.486(16) . ?
C97 N12 1.361(12) . ?
C97 C98 1.425(13) . ?
C98 N11 1.375(12) . ?
N1 Ni1 2.124(7) . ?
N2 Ni1 2.106(7) . ?
N3 Ni1 2.096(7) . ?
N4 Ni1 2.106(7) . ?
N5 Ni2 2.103(7) . ?
N6 Ni2 2.110(7) . ?
N7 Ni2 2.120(6) . ?
N8 Ni2 2.083(6) . ?
N9 Ni3 2.091(7) . ?
N10 Ni3 2.134(6) . ?
N11 Ni3 2.093(7) . ?
N12 Ni3 2.112(6) . ?
O1 Nb1 1.714(6) . ?
O2 Nb1 2.156(6) . ?
O5 Nb1 2.117(5) . ?
O6 Nb1 2.101(5) . ?
O8 Nb1 2.144(6) . ?
O10 Nb1 2.110(5) . ?
O12 Nb1 2.202(6) . ?
O14 Ni1 2.085(6) . ?
O15 Ni1 2.083(6) . ?
O16 Ni2 2.099(5) . ?
O17 Ni2 2.073(5) . ?
O18 Ni3 2.085(6) . ?
O19 Ni3 2.101(6) . ?
O100 O101 1.70(3) . ?
O102 O103 1.82(3) 14_655 ?
O110 O112 1.41(6) . ?
O111 O111 1.63(8) 14_655 ?

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
O3 C1 O2 127.0(8) . . ?
O3 C1 C2 121.3(8) . . ?
O2 C1 C2 111.6(7) . . ?
O4 C2 O5 125.2(7) . . ?
O4 C2 C1 122.8(7) . . ?
O5 C2 C1 112.0(6) . . ?
O7 C3 O6 127.3(8) . . ?
O7 C3 C4 120.3(8) . . ?
O6 C3 C4 112.4(7) . . ?
O9 C4 O8 126.0(8) . . ?
O9 C4 C3 122.9(8) . . ?
O8 C4 C3 111.2(7) . . ?
O11 C5 O10 125.0(11) . . ?
O11 C5 C6 121.6(10) . . ?
O10 C5 C6 113.3(8) . . ?
O13 C6 O12 125.5(11) . . ?
O13 C6 C5 118.5(9) . . ?
O12 C6 C5 115.7(9) . . ?
O14 C7 O14 127.5(10) . 2 ?
O14 C7 C8 116.3(5) . . ?
O14 C7 C8 116.3(5) 2 . ?
O15 C8 O15 127.5(12) . 2 ?
O15 C8 C7 116.3(6) . . ?
O15 C8 C7 116.2(6) 2 . ?
N1 C10 C11 118.3(10) . . ?
N1 C10 C9 121.0(9) . . ?
C11 C10 C9 120.6(9) . . ?
C12 C11 C10 120.7(10) . . ?
C11 C12 C13 120.6(10) . . ?
C12 C13 C22 119.4(11) . . ?
C12 C13 C14 124.0(11) . . ?
C22 C13 C14 116.6(11) . . ?
C15 C14 C13 122.6(11) . . ?
C14 C15 C16 120.1(12) . . ?
C17 C16 C15 124.3(11) . . ?
C17 C16 C21 115.7(9) . . ?
C15 C16 C21 120.0(11) . . ?
C18 C17 C16 122.8(10) . . ?
C17 C18 C19 120.4(9) . . ?
N2 C19 C18 118.6(9) . . ?
N2 C19 C20 120.1(9) . . ?
C18 C19 C20 121.3(9) . . ?
N2 C21 C22 119.3(8) . . ?
N2 C21 C16 121.1(8) . . ?
C22 C21 C16 119.6(9) . . ?
N1 C22 C13 121.0(9) . . ?
N1 C22 C21 117.4(7) . . ?
C13 C22 C21 121.0(10) . . ?
N3 C24 C25 122.1(9) . . ?
N3 C24 C23 118.6(8) . . ?
C25 C24 C23 119.2(9) . . ?
C24 C25 C26 120.0(9) . . ?
C25 C26 C27 119.1(9) . . ?
C37 C27 C26 116.5(9) . . ?
C37 C27 C28 120.5(9) . . ?
C26 C27 C28 123.0(10) . . ?
C29 C28 C27 121.7(10) . . ?
C28 C29 C30 121.3(10) . . ?
C31 C30 C36 117.2(10) . . ?
C31 C30 C29 124.4(10) . . ?
C36 C30 C29 118.3(10) . . ?
C32 C31 C30 120.3(10) . . ?
C31 C32 C33 121.0(10) . . ?
N4 C33 C32 120.8(11) . . ?
N4 C33 C35 118.2(10) . . ?
C32 C33 C35 121.0(9) . . ?
C30 C36 N4 123.3(9) . . ?
C30 C36 C37 120.3(8) . . ?
N4 C36 C37 116.4(7) . . ?
N3 C37 C27 124.8(8) . . ?
N3 C37 C36 117.3(8) . . ?
C27 C37 C36 117.8(8) . . ?
O16 C38 O16 123.2(10) 14 . ?
O16 C38 C39 118.4(5) 14 . ?
O16 C38 C39 118.4(5) . . ?
O17 C39 O17 127.1(10) . 14 ?
O17 C39 C38 116.4(5) . . ?
O17 C39 C38 116.4(5) 14 . ?
N5 C41 C42 123.7(9) . . ?
N5 C41 C40 117.3(9) . . ?
C42 C41 C40 118.9(9) . . ?
C43 C42 C41 117.8(11) . . ?
C42 C43 C44 122.5(11) . . ?
C43 C44 C45 127.3(13) . . ?
C43 C44 C53 116.1(10) . . ?
C45 C44 C53 116.5(13) . . ?
C46 C45 C44 124.0(14) . . ?
C45 C46 C47 119.1(11) . . ?
C46 C47 C48 123.2(13) . . ?
C46 C47 C52 123.2(12) . . ?
C48 C47 C52 113.5(14) . . ?
C47 C48 C49 121.2(12) . . ?
C50 C49 C48 118.9(12) . . ?
N6 C50 C49 121.3(14) . . ?
N6 C50 C51 118.7(10) . . ?
C49 C50 C51 119.9(11) . . ?
N6 C52 C47 127.0(10) . . ?
N6 C52 C53 116.9(7) . . ?
C47 C52 C53 116.1(10) . . ?
N5 C53 C44 122.3(9) . . ?
N5 C53 C52 116.8(8) . . ?
C44 C53 C52 120.5(8) . . ?
N7 C55 C56 120.1(8) . . ?
N7 C55 C54 120.4(7) . . ?
C56 C55 C54 119.5(8) . . ?
C57 C56 C55 121.5(8) . . ?
C56 C57 C58 119.0(9) . . ?
C57 C58 C68 117.1(9) . . ?
C57 C58 C59 123.2(9) . . ?
C68 C58 C59 119.6(9) . . ?
C60 C59 C58 119.0(10) . . ?
C59 C60 C61 123.9(10) . . ?
C62 C61 C60 125.6(11) . . ?
C62 C61 C67 115.7(10) . . ?
C60 C61 C67 118.7(10) . . ?
C63 C62 C61 121.7(10) . . ?
C62 C63 C64 121.4(10) . . ?
N8 C64 C63 119.5(10) . . ?
N8 C64 C66 118.6(9) . . ?
C63 C64 C66 121.9(9) . . ?
N8 C67 C61 122.8(8) . . ?
N8 C67 C68 117.9(7) . . ?
C61 C67 C68 119.2(8) . . ?
N7 C68 C58 123.2(7) . . ?
N7 C68 C67 117.4(7) . . ?
C58 C68 C67 119.5(8) . . ?
O18 C69 O18 127.0(9) . 14_655 ?
O18 C69 C70 116.5(5) . . ?
O18 C69 C70 116.5(5) 14_655 . ?
O19 C70 O19 129.4(11) . 14_655 ?
O19 C70 C69 115.3(5) . . ?
O19 C70 C69 115.3(5) 14_655 . ?
N9 C72 C73 120.1(10) . . ?
N9 C72 C71 120.5(9) . . ?
C73 C72 C71 119.4(9) . . ?
C74 C73 C72 121.0(10) . . ?
C73 C74 C75 120.1(10) . . ?
C74 C75 C84 117.7(10) . . ?
C74 C75 C76 123.4(11) . . ?
C84 C75 C76 118.8(11) . . ?
C77 C76 C75 121.5(11) . . ?
C76 C77 C78 120.7(10) . . ?
C83 C78 C79 115.7(11) . . ?
C83 C78 C77 118.8(11) . . ?
C79 C78 C77 125.4(11) . . ?
C80 C79 C78 120.2(10) . . ?
C79 C80 C81 121.9(10) . . ?
N10 C81 C80 120.7(11) . . ?
N10 C81 C82 119.3(8) . . ?
C80 C81 C82 120.0(9) . . ?
N10 C83 C78 122.6(9) . . ?
N10 C83 C84 118.4(7) . . ?
C78 C83 C84 118.9(9) . . ?
N9 C84 C75 122.2(8) . . ?
N9 C84 C83 116.5(8) . . ?
C75 C84 C83 121.2(8) . . ?
N11 C86 C87 122.2(11) . . ?
N11 C86 C85 117.2(9) . . ?
C87 C86 C85 120.6(10) . . ?
C88 C87 C86 119.2(12) . . ?
C87 C88 C89 122.3(12) . . ?
C98 C89 C90 120.7(13) . . ?
C98 C89 C88 114.7(11) . . ?
C90 C89 C88 124.3(12) . . ?
C91 C90 C89 121.3(11) . . ?
C90 C91 C92 119.5(10) . . ?
C91 C92 C93 122.1(11) . . ?
C91 C92 C97 121.4(12) . . ?
C93 C92 C97 116.3(11) . . ?
C94 C93 C92 121.2(10) . . ?
C93 C94 C95 119.2(12) . . ?
N12 C95 C94 120.8(12) . . ?
N12 C95 C96 118.9(8) . . ?
C94 C95 C96 120.2(10) . . ?
N12 C97 C92 123.8(10) . . ?
N12 C97 C98 117.4(8) . . ?
C92 C97 C98 118.5(9) . . ?
N11 C98 C89 124.1(9) . . ?
N11 C98 C97 117.2(7) . . ?
C89 C98 C97 118.6(9) . . ?
C10 N1 C22 119.7(8) . . ?
C10 N1 Ni1 130.2(7) . . ?
C22 N1 Ni1 108.7(5) . . ?
C19 N2 C21 120.9(8) . . ?
C19 N2 Ni1 129.8(6) . . ?
C21 N2 Ni1 108.9(5) . . ?
C37 N3 C24 117.3(7) . . ?
C37 N3 Ni1 111.3(5) . . ?
C24 N3 Ni1 130.5(6) . . ?
C33 N4 C36 117.1(9) . . ?
C33 N4 Ni1 132.1(7) . . ?
C36 N4 Ni1 109.8(5) . . ?
C41 N5 C53 117.3(8) . . ?
C41 N5 Ni2 132.1(6) . . ?
C53 N5 Ni2 109.5(5) . . ?
C50 N6 C52 117.7(9) . . ?
C50 N6 Ni2 131.6(8) . . ?
C52 N6 Ni2 108.0(5) . . ?
C55 N7 C68 118.9(7) . . ?
C55 N7 Ni2 131.6(5) . . ?
C68 N7 Ni2 108.0(4) . . ?
C64 N8 C67 118.5(8) . . ?
C64 N8 Ni2 131.5(6) . . ?
C67 N8 Ni2 108.9(5) . . ?
C72 N9 C84 118.6(8) . . ?
C72 N9 Ni3 131.2(6) . . ?
C84 N9 Ni3 109.5(5) . . ?
C81 N10 C83 118.5(7) . . ?
C81 N10 Ni3 132.1(6) . . ?
C83 N10 Ni3 107.9(5) . . ?
C86 N11 C98 117.4(8) . . ?
C86 N11 Ni3 132.5(7) . . ?
C98 N11 Ni3 109.0(5) . . ?
C95 N12 C97 118.5(8) . . ?
C95 N12 Ni3 131.1(7) . . ?
C97 N12 Ni3 108.7(6) . . ?
C1 O2 Nb1 121.9(5) . . ?
C2 O5 Nb1 122.4(5) . . ?
C3 O6 Nb1 122.9(5) . . ?
C4 O8 Nb1 120.6(5) . . ?
C5 O10 Nb1 120.6(6) . . ?
C6 O12 Nb1 115.9(7) . . ?
C7 O14 Ni1 113.4(6) . . ?
C8 O15 Ni1 114.1(6) . . ?
C38 O16 Ni2 111.1(6) . . ?
C39 O17 Ni2 113.7(6) . . ?
C69 O18 Ni3 114.2(5) . . ?
C70 O19 Ni3 114.9(6) . . ?
O15 Ni1 O14 79.40(19) . . ?
O15 Ni1 N3 90.7(3) . . ?
O14 Ni1 N3 170.0(3) . . ?
O15 Ni1 N2 170.9(2) . . ?
O14 Ni1 N2 91.7(2) . . ?
N3 Ni1 N2 98.3(2) . . ?
O15 Ni1 N4 80.9(2) . . ?
O14 Ni1 N4 97.1(3) . . ?
N3 Ni1 N4 79.5(3) . . ?
N2 Ni1 N4 101.9(3) . . ?
O15 Ni1 N1 97.5(3) . . ?
O14 Ni1 N1 80.6(2) . . ?
N3 Ni1 N1 102.7(3) . . ?
N2 Ni1 N1 79.4(3) . . ?
N4 Ni1 N1 177.4(2) . . ?
O17 Ni2 N8 168.0(2) . . ?
O17 Ni2 O16 80.1(2) . . ?
N8 Ni2 O16 88.7(2) . . ?
O17 Ni2 N5 90.7(2) . . ?
N8 Ni2 N5 100.9(3) . . ?
O16 Ni2 N5 169.7(2) . . ?
O17 Ni2 N6 80.8(2) . . ?
N8 Ni2 N6 104.5(3) . . ?
O16 Ni2 N6 94.9(3) . . ?
N5 Ni2 N6 79.1(3) . . ?
O17 Ni2 N7 94.2(2) . . ?
N8 Ni2 N7 79.8(2) . . ?
O16 Ni2 N7 81.5(2) . . ?
N5 Ni2 N7 103.8(2) . . ?
N6 Ni2 N7 174.4(2) . . ?
O18 Ni3 N9 90.3(3) . . ?
O18 Ni3 N11 169.8(3) . . ?
N9 Ni3 N11 99.5(3) . . ?
O18 Ni3 O19 78.9(2) . . ?
N9 Ni3 O19 168.3(3) . . ?
N11 Ni3 O19 91.4(3) . . ?
O18 Ni3 N12 95.8(3) . . ?
N9 Ni3 N12 103.8(3) . . ?
N11 Ni3 N12 79.2(3) . . ?
O19 Ni3 N12 82.0(2) . . ?
O18 Ni3 N10 80.7(2) . . ?
N9 Ni3 N10 79.9(3) . . ?
N11 Ni3 N10 103.6(3) . . ?
O19 Ni3 N10 93.7(2) . . ?
N12 Ni3 N10 174.9(3) . . ?
O1 Nb1 O6 96.5(3) . . ?
O1 Nb1 O10 96.4(3) . . ?
O6 Nb1 O10 141.9(2) . . ?
O1 Nb1 O5 102.8(3) . . ?
O6 Nb1 O5 71.6(2) . . ?
O10 Nb1 O5 138.8(3) . . ?
O1 Nb1 O8 93.6(3) . . ?
O6 Nb1 O8 72.3(2) . . ?
O10 Nb1 O8 71.2(2) . . ?
O5 Nb1 O8 141.7(2) . . ?
O1 Nb1 O2 92.4(3) . . ?
O6 Nb1 O2 143.1(2) . . ?
O10 Nb1 O2 71.6(2) . . ?
O5 Nb1 O2 71.5(2) . . ?
O8 Nb1 O2 142.8(2) . . ?
O1 Nb1 O12 170.5(3) . . ?
O6 Nb1 O12 91.7(2) . . ?
O10 Nb1 O12 74.2(3) . . ?
O5 Nb1 O12 84.3(3) . . ?
O8 Nb1 O12 84.3(3) . . ?
O2 Nb1 O12 83.8(3) . . ?

_refine_diff_density_max         1.729
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.151


