# Supplementary Information (SI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2025

####################################################################### 
# 
# 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_Fe20V8
_database_code_depnum_ccdc_archive 'CCDC 2434503'
loop_
_audit_author_name
_audit_author_address
'Yanfeng Bi'
;Liaoning Petrochemical University
China
;
_audit_update_record             
;
2025-05-08 deposited with the CCDC.	2025-05-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/1
_shelx_SHELXL_version_number     2019/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C216 H260 Cl5 Fe20 O52 S20 V8, 12(C3 H7 N O)(C2 H6 O)'
_chemical_formula_sum            'C254 H351 Cl5 Fe20 N12 O65 S20 V8'
_chemical_formula_weight         6955.42

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'
Fe Fe 0.3463 0.8444 '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'
V V 0.3005 0.5294 '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      tetragonal
_space_group_IT_number           79
_space_group_name_H-M_alt        'I 4'
_space_group_name_Hall           'I 4'

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

_cell_length_a                   26.9722(13)
_cell_length_b                   26.9722(13)
_cell_length_c                   22.8711(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     16638.7(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9483
_cell_measurement_theta_min      2.3878
_cell_measurement_theta_max      25.0029

_exptl_crystal_description       Block
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_F_000             7176
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    1.285
_shelx_estimated_absorpt_T_min   0.811
_shelx_estimated_absorpt_T_max   0.821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6478
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            94058
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.434
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_full        25.026
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_point_group_measured_fraction_full 0.968
_reflns_number_total             14257
_reflns_number_gt                13241
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.890
_reflns_Friedel_fraction_max     0.938
_reflns_Friedel_fraction_full    0.938

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'Bruker Instrument Service vV6.2.3'
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_molecular_graphics    'Diamond 3.2K'
_computing_publication_material  'Adobe Photoshop CS6 and POV-Ray v3.7'
_refine_special_details          
'Refined as a 2-component inversion twin.,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)+(0.1005P)²+36.2742P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.41(2)
_chemical_absolute_configuration unk
_refine_ls_number_reflns         14257
_refine_ls_number_parameters     735
_refine_ls_number_restraints     95
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0459
_refine_ls_wR_factor_ref         0.1415
_refine_ls_wR_factor_gt          0.1372
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.053
_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
Fe1 Fe 0.50989(3) 0.68864(3) 0.35683(5) 0.02399(18) Uani 1 1 d . . . . .
Fe2 Fe 0.58466(4) 0.64635(3) 0.46234(4) 0.0240(2) Uani 1 1 d . . . . .
Fe3 Fe 0.65823(3) 0.60284(3) 0.35681(5) 0.02602(19) Uani 1 1 d . . . . .
Fe4 Fe 0.58317(4) 0.64521(4) 0.24926(5) 0.0297(3) Uani 1 1 d . . . . .
Fe5 Fe 0.42654(3) 0.54772(3) 0.56136(4) 0.0269(2) Uani 1 1 d . . . . .
V1 V 0.46071(4) 0.65053(4) 0.48919(5) 0.0221(3) Uani 1 1 d . . . . .
V2 V 0.46033(5) 0.65014(5) 0.22847(5) 0.0331(3) Uani 1 1 d . . . . .
Cl1 Cl 0.56117(4) 0.60599(4) 0.36002(8) 0.0243(3) Uani 1 1 d . . . . .
Cl2 Cl 0.500000 0.500000 0.50763(14) 0.0277(6) Uani 1 4 d S T P . .
S1 S 0.49618(5) 0.78279(5) 0.35597(10) 0.0307(3) Uani 1 1 d . . . . .
S2 S 0.62311(7) 0.71440(7) 0.52599(8) 0.0311(4) Uani 1 1 d . . . . .
S3 S 0.74548(5) 0.64002(5) 0.35591(10) 0.0324(3) Uani 1 1 d . . . . .
S4 S 0.62118(7) 0.71270(8) 0.18492(9) 0.0348(4) Uani 1 1 d . . . . .
S5 S 0.41925(6) 0.38116(6) 0.65195(9) 0.0349(4) Uani 1 1 d . . . . .
O1 O 0.55721(19) 0.70831(17) 0.4208(2) 0.0286(11) Uani 1 1 d . . . . .
O2 O 0.65243(19) 0.65108(18) 0.4245(2) 0.0291(11) Uani 1 1 d . . . . .
O3 O 0.65031(18) 0.6529(2) 0.2901(2) 0.0336(12) Uani 1 1 d . . . . .
O4 O 0.55667(19) 0.70799(17) 0.2903(2) 0.0299(11) Uani 1 1 d . . . . .
O5 O 0.42204(17) 0.48423(16) 0.6072(2) 0.0290(10) Uani 1 1 d . . . . .
O6 O 0.51914(17) 0.63085(18) 0.5048(2) 0.0271(10) Uani 1 1 d . . . . .
O7 O 0.45599(18) 0.66618(19) 0.4175(2) 0.0290(11) Uani 1 1 d . . . . .
O8 O 0.41826(17) 0.60487(17) 0.5055(2) 0.0251(10) Uani 1 1 d . . . . .
O9 O 0.4493(2) 0.7038(2) 0.5313(3) 0.0440(13) Uani 1 1 d D . . . .
O10 O 0.5162(2) 0.6294(3) 0.2155(3) 0.0494(16) Uani 1 1 d . . . . .
O11 O 0.45570(18) 0.66665(19) 0.3006(2) 0.0307(11) Uani 1 1 d . . . . .
O12 O 0.4209(3) 0.6064(3) 0.2141(3) 0.062(2) Uani 1 1 d . . . . .
O13 O 0.4498(4) 0.7010(4) 0.1856(4) 0.096(3) Uani 1 1 d D . . . .
C1 C 0.5611(3) 0.7537(3) 0.4428(4) 0.0288(16) Uani 1 1 d . . . . .
C2 C 0.5354(3) 0.7946(3) 0.4178(4) 0.0328(16) Uani 1 1 d . . . . .
C3 C 0.5381(3) 0.8417(3) 0.4417(4) 0.0400(19) Uani 1 1 d . . . . .
H3A H 0.520259 0.868059 0.424018 0.048 Uiso 1 1 calc R U . . .
C4 C 0.5667(3) 0.8510(3) 0.4912(5) 0.050(2) Uani 1 1 d . . . . .
C5 C 0.5915(3) 0.8120(3) 0.5151(4) 0.043(2) Uani 1 1 d . . . . .
H5A H 0.611060 0.817643 0.548995 0.051 Uiso 1 1 calc R U . . .
C6 C 0.5897(3) 0.7642(3) 0.4919(3) 0.0334(17) Uani 1 1 d . . . . .
C7 C 0.6884(3) 0.6813(3) 0.4425(3) 0.0248(14) Uani 1 1 d . . . . .
C8 C 0.6808(3) 0.7148(3) 0.4886(3) 0.0325(17) Uani 1 1 d . . . . .
C9 C 0.7197(3) 0.7463(3) 0.5052(4) 0.047(2) Uani 1 1 d . . . . .
H9A H 0.714123 0.768498 0.536793 0.056 Uiso 1 1 calc R U . . .
C10 C 0.7638(4) 0.7471(5) 0.4793(4) 0.062(3) Uani 1 1 d . . . . .
C11 C 0.7724(3) 0.7137(4) 0.4333(4) 0.048(2) Uani 1 1 d . . . . .
H11A H 0.803839 0.712876 0.414599 0.058 Uiso 1 1 calc R U . . .
C12 C 0.7350(3) 0.6818(3) 0.4151(4) 0.0332(17) Uani 1 1 d . . . . .
C13 C 0.6857(3) 0.6805(3) 0.2696(4) 0.0338(17) Uani 1 1 d . . . . .
C14 C 0.7339(3) 0.6799(3) 0.2951(3) 0.0297(16) Uani 1 1 d . . . . .
C15 C 0.7721(3) 0.7088(3) 0.2752(3) 0.0380(19) Uani 1 1 d . . . . .
H15A H 0.803636 0.706929 0.293627 0.046 Uiso 1 1 calc R U . . .
C16 C 0.7652(3) 0.7413(3) 0.2276(4) 0.0408(19) Uani 1 1 d . . . . .
C17 C 0.7180(3) 0.7420(3) 0.2012(3) 0.0346(17) Uani 1 1 d . . . . .
H17A H 0.712147 0.763287 0.168919 0.042 Uiso 1 1 calc R U . . .
C18 C 0.6801(3) 0.7120(3) 0.2218(3) 0.0296(15) Uani 1 1 d . . . . .
C19 C 0.5595(3) 0.7534(3) 0.2691(4) 0.0339(17) Uani 1 1 d . . . . .
C20 C 0.5887(3) 0.7631(3) 0.2187(4) 0.0362(18) Uani 1 1 d . . . . .
C21 C 0.5922(3) 0.8101(3) 0.1954(4) 0.041(2) Uani 1 1 d . . . . .
H21A H 0.612881 0.815779 0.162440 0.049 Uiso 1 1 calc R U . . .
C22 C 0.5655(3) 0.8498(3) 0.2197(4) 0.044(2) Uani 1 1 d . . . . .
C23 C 0.5392(3) 0.8407(3) 0.2703(4) 0.042(2) Uani 1 1 d . . . . .
H23A H 0.523130 0.867483 0.289343 0.051 Uiso 1 1 calc R U . . .
C24 C 0.5355(3) 0.7932(3) 0.2943(4) 0.0342(17) Uani 1 1 d . . . . .
C25 C 0.5673(4) 0.9027(4) 0.5204(6) 0.067(3) Uani 1 1 d . U . . .
C26 C 0.8075(5) 0.7803(5) 0.4994(6) 0.084(4) Uani 1 1 d . U . . .
C27 C 0.8107(4) 0.7699(4) 0.2043(4) 0.054(2) Uani 1 1 d . . . . .
C28 C 0.5681(4) 0.9013(4) 0.1903(5) 0.064(3) Uani 1 1 d . . . . .
C29 C 0.5513(9) 0.9427(6) 0.4750(10) 0.142(7) Uani 1 1 d . U . . .
H29A H 0.573496 0.941427 0.441113 0.213 Uiso 1 1 calc R U . . .
H29B H 0.517215 0.936333 0.462434 0.213 Uiso 1 1 calc R U . . .
H29C H 0.553275 0.975646 0.493063 0.213 Uiso 1 1 calc R U . . .
C30 C 0.5370(8) 0.9020(8) 0.5711(10) 0.144(7) Uani 1 1 d . U . . .
H30A H 0.503158 0.892595 0.560316 0.216 Uiso 1 1 calc R U . . .
H30B H 0.550279 0.878010 0.599202 0.216 Uiso 1 1 calc R U . . .
H30C H 0.536702 0.935106 0.588911 0.216 Uiso 1 1 calc R U . . .
C31 C 0.6179(5) 0.9168(4) 0.5368(7) 0.088(3) Uani 1 1 d . U . . .
H31A H 0.638901 0.917302 0.501901 0.133 Uiso 1 1 calc R U . . .
H31B H 0.617453 0.949866 0.554641 0.133 Uiso 1 1 calc R U . . .
H31C H 0.631030 0.892770 0.564932 0.133 Uiso 1 1 calc R U . . .
C32 C 0.7970(5) 0.8124(5) 0.5447(6) 0.075(4) Uani 1 1 d . . . . .
H32A H 0.776105 0.795592 0.573596 0.113 Uiso 1 1 calc R U . . .
H32B H 0.827950 0.823068 0.563215 0.113 Uiso 1 1 calc R U . . .
H32C H 0.779386 0.841448 0.529362 0.113 Uiso 1 1 calc R U . . .
C33 C 0.8491(5) 0.7407(7) 0.5278(7) 0.108(6) Uani 1 1 d . . . . .
H33A H 0.858676 0.716305 0.498127 0.163 Uiso 1 1 calc R U . . .
H33B H 0.878523 0.759116 0.540545 0.163 Uiso 1 1 calc R U . . .
H33C H 0.834453 0.723553 0.561427 0.163 Uiso 1 1 calc R U . . .
C34 C 0.8385(5) 0.7978(5) 0.4508(6) 0.084(4) Uani 1 1 d . . . . .
H34A H 0.842727 0.771099 0.422179 0.125 Uiso 1 1 calc R U . . .
H34B H 0.822465 0.826248 0.431934 0.125 Uiso 1 1 calc R U . . .
H34C H 0.871030 0.807868 0.465788 0.125 Uiso 1 1 calc R U . . .
C35 C 0.8369(5) 0.7948(5) 0.2557(5) 0.079(4) Uani 1 1 d . . . . .
H35A H 0.813790 0.817212 0.275596 0.119 Uiso 1 1 calc R U . . .
H35B H 0.848406 0.769465 0.283271 0.119 Uiso 1 1 calc R U . . .
H35C H 0.865397 0.813798 0.241305 0.119 Uiso 1 1 calc R U . . .
C36 C 0.8452(4) 0.7355(5) 0.1732(5) 0.071(3) Uani 1 1 d . . . . .
H36A H 0.856574 0.709722 0.200285 0.107 Uiso 1 1 calc R U . . .
H36B H 0.827847 0.719979 0.140268 0.107 Uiso 1 1 calc R U . . .
H36C H 0.873811 0.754134 0.158577 0.107 Uiso 1 1 calc R U . . .
C37 C 0.7948(4) 0.8083(4) 0.1601(5) 0.063(3) Uani 1 1 d . . . . .
H37A H 0.772013 0.831885 0.178583 0.095 Uiso 1 1 calc R U . . .
H37B H 0.824030 0.826124 0.145616 0.095 Uiso 1 1 calc R U . . .
H37C H 0.778065 0.791969 0.127307 0.095 Uiso 1 1 calc R U . . .
C38 C 0.6217(5) 0.9162(5) 0.1801(8) 0.100(5) Uani 1 1 d . . . . .
H38A H 0.638457 0.890272 0.157479 0.150 Uiso 1 1 calc R U . . .
H38B H 0.622729 0.947477 0.158419 0.150 Uiso 1 1 calc R U . . .
H38C H 0.638404 0.920315 0.217818 0.150 Uiso 1 1 calc R U . . .
C39 C 0.5396(8) 0.8962(6) 0.1287(7) 0.132(6) Uani 1 1 d D U . . .
H39A H 0.555984 0.870775 0.104814 0.199 Uiso 1 1 calc R U . . .
H39B H 0.505103 0.886544 0.135630 0.199 Uiso 1 1 calc R U . . .
H39C H 0.540540 0.927996 0.108068 0.199 Uiso 1 1 calc R U . . .
C40 C 0.5417(8) 0.9404(5) 0.2249(8) 0.132(6) Uani 1 1 d D U . . .
H40A H 0.507197 0.930299 0.231110 0.198 Uiso 1 1 calc R U . . .
H40B H 0.558152 0.944621 0.262730 0.198 Uiso 1 1 calc R U . . .
H40C H 0.542476 0.971783 0.203331 0.198 Uiso 1 1 calc R U . . .
C41 C 0.3975(2) 0.4801(2) 0.6585(3) 0.0290(14) Uani 1 1 d . . . . .
C42 C 0.3766(3) 0.5209(3) 0.6860(4) 0.0428(18) Uani 1 1 d . . . . .
C43 C 0.3545(5) 0.5171(4) 0.7408(5) 0.085(4) Uani 1 1 d . . . . .
H43A H 0.341635 0.546157 0.758753 0.102 Uiso 1 1 calc R U . . .
C44 C 0.3508(6) 0.4729(4) 0.7697(6) 0.101(5) Uani 1 1 d D . . . .
C45 C 0.3701(5) 0.4329(4) 0.7405(6) 0.093(5) Uani 1 1 d . . . . .
H45A H 0.367320 0.401385 0.758716 0.112 Uiso 1 1 calc R U . . .
C46 C 0.3935(3) 0.4350(3) 0.6865(4) 0.0425(18) Uiso 1 1 d . . . . .
C47 C 0.3139(8) 0.4688(8) 0.8184(9) 0.129(5) Uiso 0.588(16) 1 d D U P A 1
C48 C 0.2581(9) 0.4636(11) 0.8004(14) 0.140(6) Uiso 0.588(16) 1 d D U P A 1
H48A H 0.237553 0.461187 0.835651 0.211 Uiso 0.588(16) 1 calc R U P A 1
H48B H 0.248055 0.492640 0.777627 0.211 Uiso 0.588(16) 1 calc R U P A 1
H48C H 0.253773 0.433589 0.776737 0.211 Uiso 0.588(16) 1 calc R U P A 1
C49 C 0.3269(10) 0.4245(8) 0.8589(16) 0.119(5) Uiso 0.588(16) 1 d D U P A 1
H49A H 0.302487 0.422310 0.890454 0.178 Uiso 0.588(16) 1 calc R U P A 1
H49B H 0.326533 0.393692 0.836114 0.178 Uiso 0.588(16) 1 calc R U P A 1
H49C H 0.360014 0.429482 0.875555 0.178 Uiso 0.588(16) 1 calc R U P A 1
C50 C 0.3207(10) 0.5184(7) 0.8533(15) 0.125(5) Uiso 0.588(16) 1 d D U P A 1
H50A H 0.297711 0.519008 0.886475 0.187 Uiso 0.588(16) 1 calc R U P A 1
H50B H 0.354844 0.520651 0.867696 0.187 Uiso 0.588(16) 1 calc R U P A 1
H50C H 0.313790 0.546606 0.827508 0.187 Uiso 0.588(16) 1 calc R U P A 1
C47' C 0.3374(11) 0.4739(10) 0.8386(14) 0.122(5) Uiso 0.412(16) 1 d D U P A 2
C48' C 0.2815(11) 0.4871(14) 0.838(2) 0.130(5) Uiso 0.412(16) 1 d D U P A 2
H48D H 0.277398 0.521686 0.825273 0.195 Uiso 0.412(16) 1 calc R U P A 2
H48E H 0.264276 0.465303 0.809937 0.195 Uiso 0.412(16) 1 calc R U P A 2
H48F H 0.267470 0.482718 0.876721 0.195 Uiso 0.412(16) 1 calc R U P A 2
C49' C 0.3467(14) 0.4203(9) 0.857(3) 0.126(6) Uiso 0.412(16) 1 d D U P A 2
H49D H 0.326948 0.397898 0.832977 0.189 Uiso 0.412(16) 1 calc R U P A 2
H49E H 0.381929 0.412429 0.852933 0.189 Uiso 0.412(16) 1 calc R U P A 2
H49F H 0.337039 0.416178 0.898473 0.189 Uiso 0.412(16) 1 calc R U P A 2
C50' C 0.3669(13) 0.5119(12) 0.8747(19) 0.128(6) Uiso 0.412(16) 1 d D U P A 2
H50D H 0.359443 0.545399 0.860636 0.191 Uiso 0.412(16) 1 calc R U P A 2
H50E H 0.357553 0.509116 0.915955 0.191 Uiso 0.412(16) 1 calc R U P A 2
H50F H 0.402443 0.505367 0.870415 0.191 Uiso 0.412(16) 1 calc R U P A 2
O14 O 0.5703(6) 0.1401(5) 0.8668(8) 0.160(4) Uiso 1 1 d . U . . .
N1 N 0.6536(4) 0.1736(4) 0.8669(5) 0.092(3) Uiso 1 1 d . U . . .
C52 C 0.7024(4) 0.1696(4) 0.8555(7) 0.082(3) Uiso 1 1 d . U . . .
H52A H 0.719958 0.198102 0.872120 0.123 Uiso 1 1 calc R U . . .
H52B H 0.715256 0.138960 0.872909 0.123 Uiso 1 1 calc R U . . .
H52C H 0.707594 0.168757 0.813079 0.123 Uiso 1 1 calc R U . . .
C51 C 0.6170(7) 0.1435(6) 0.8526(10) 0.127(4) Uiso 1 1 d . U . . .
H51A H 0.627025 0.118573 0.825792 0.152 Uiso 1 1 calc R U . . .
C53 C 0.6424(7) 0.2011(6) 0.9197(8) 0.113(4) Uiso 1 1 d . U . . .
H53A H 0.670261 0.223004 0.929167 0.169 Uiso 1 1 calc R U . . .
H53B H 0.612444 0.220921 0.913647 0.169 Uiso 1 1 calc R U . . .
H53C H 0.637021 0.177861 0.952081 0.169 Uiso 1 1 calc R U . . .
C54 C 0.4144(10) 0.7302(9) 0.1607(13) 0.119(6) Uiso 0.65(2) 1 d D U P B 1
H54A H 0.381327 0.715018 0.166369 0.143 Uiso 0.65(2) 1 calc R U P B 1
H54B H 0.420580 0.732944 0.118128 0.143 Uiso 0.65(2) 1 calc R U P B 1
C55 C 0.4154(12) 0.7845(10) 0.1899(13) 0.127(7) Uiso 0.65(2) 1 d D U P B 1
H55A H 0.389917 0.805310 0.171789 0.190 Uiso 0.65(2) 1 calc R U P B 1
H55B H 0.408918 0.781669 0.231928 0.190 Uiso 0.65(2) 1 calc R U P B 1
H55C H 0.448087 0.799557 0.183789 0.190 Uiso 0.65(2) 1 calc R U P B 1
C56 C 0.4364(11) 0.7538(9) 0.5161(15) 0.134(7) Uiso 0.624(16) 1 d D U P C 1
H56A H 0.431371 0.755452 0.473243 0.161 Uiso 0.624(16) 1 calc R U P C 1
H56B H 0.464821 0.775525 0.525696 0.161 Uiso 0.624(16) 1 calc R U P C 1
C57 C 0.3886(10) 0.7756(11) 0.5469(14) 0.133(8) Uiso 0.624(16) 1 d D U P C 1
H57A H 0.383101 0.809657 0.533606 0.200 Uiso 0.624(16) 1 calc R U P C 1
H57B H 0.359777 0.755167 0.536759 0.200 Uiso 0.624(16) 1 calc R U P C 1
H57C H 0.393324 0.775298 0.589364 0.200 Uiso 0.624(16) 1 calc R U P C 1
C54' C 0.432(2) 0.7476(13) 0.196(2) 0.127(7) Uiso 0.35(2) 1 d D U P B 2
H54C H 0.457613 0.768354 0.213792 0.152 Uiso 0.35(2) 1 calc R U P B 2
H54D H 0.403324 0.745611 0.223280 0.152 Uiso 0.35(2) 1 calc R U P B 2
C55' C 0.413(2) 0.773(2) 0.136(2) 0.124(7) Uiso 0.35(2) 1 d D U P B 2
H55D H 0.400464 0.806212 0.143879 0.186 Uiso 0.35(2) 1 calc R U P B 2
H55E H 0.441389 0.775417 0.108555 0.186 Uiso 0.35(2) 1 calc R U P B 2
H55F H 0.387168 0.752703 0.118031 0.186 Uiso 0.35(2) 1 calc R U P B 2
C56' C 0.472(2) 0.7269(14) 0.5788(16) 0.137(9) Uiso 0.376(16) 1 d D U P C 2
H56C H 0.502491 0.709142 0.589323 0.165 Uiso 0.376(16) 1 calc R U P C 2
H56D H 0.449063 0.725876 0.612971 0.165 Uiso 0.376(16) 1 calc R U P C 2
C57' C 0.4844(19) 0.7845(11) 0.562(2) 0.143(8) Uiso 0.376(16) 1 d D U P C 2
H57D H 0.500162 0.800645 0.595946 0.215 Uiso 0.376(16) 1 calc R U P C 2
H57E H 0.507023 0.785311 0.528837 0.215 Uiso 0.376(16) 1 calc R U P C 2
H57F H 0.453718 0.802006 0.552431 0.215 Uiso 0.376(16) 1 calc R U 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
Fe1 O1 2.012(5) . ?
Fe1 O11 2.035(5) . ?
Fe1 O4 2.045(5) . ?
Fe1 O7 2.099(5) . ?
Fe1 S1 2.5663(15) . ?
Fe1 Cl1 2.6246(14) . ?
Fe2 O2 2.026(5) . ?
Fe2 O6 2.059(5) . ?
Fe2 O1 2.060(5) . ?
Fe2 O8 2.075(5) 4_565 ?
Fe2 S2 2.562(2) . ?
Fe2 Cl1 2.657(2) . ?
Fe3 O2 2.029(5) . ?
Fe3 O11 2.048(5) 4_565 ?
Fe3 O3 2.049(5) . ?
Fe3 O7 2.119(5) 4_565 ?
Fe3 S3 2.5581(15) . ?
Fe3 Cl1 2.6202(14) . ?
Fe4 O10 2.010(6) . ?
Fe4 O3 2.048(5) . ?
Fe4 O12 2.054(6) 4_565 ?
Fe4 O4 2.064(5) . ?
Fe4 S4 2.555(2) . ?
Fe5 O5 2.011(4) . ?
Fe5 O8 2.015(5) . ?
Fe5 O5 2.045(5) 4_565 ?
Fe5 O6 2.160(5) 3_655 ?
Fe5 S5 2.566(2) 4_565 ?
Fe5 Cl2 2.6632(17) . ?
V1 O7 1.698(5) . ?
V1 O6 1.701(5) . ?
V1 O8 1.722(5) . ?
V1 O9 1.757(5) . ?
V2 O12 1.622(7) . ?
V2 O10 1.635(6) . ?
V2 O13 1.710(9) . ?
V2 O11 1.714(5) . ?
S1 C24 1.786(8) . ?
S1 C2 1.793(8) . ?
S2 C8 1.776(8) . ?
S2 C6 1.796(8) . ?
S3 C12 1.783(9) . ?
S3 C14 1.786(7) . ?
S4 C20 1.791(8) . ?
S4 C18 1.799(8) . ?
S5 C46 1.792(8) . ?
S5 C42 1.797(8) 3_655 ?
O1 C1 1.329(9) . ?
O2 C7 1.332(8) . ?
O3 C13 1.297(9) . ?
O4 C19 1.321(9) . ?
O5 C41 1.352(8) . ?
O9 C56' 1.39(3) . ?
O9 C56 1.43(2) . ?
O13 C54 1.36(2) . ?
O13 C54' 1.37(3) . ?
C1 C6 1.390(11) . ?
C1 C2 1.422(11) . ?
C2 C3 1.385(11) . ?
C3 C4 1.393(14) . ?
C3 H3A 0.9500 . ?
C4 C5 1.360(14) . ?
C4 C25 1.545(13) . ?
C5 C6 1.397(11) . ?
C5 H5A 0.9500 . ?
C7 C8 1.403(11) . ?
C7 C12 1.405(11) . ?
C8 C9 1.401(11) . ?
C9 C10 1.328(14) . ?
C9 H9A 0.9500 . ?
C10 C11 1.406(15) . ?
C10 C26 1.550(14) . ?
C11 C12 1.389(11) . ?
C11 H11A 0.9500 . ?
C13 C18 1.394(12) . ?
C13 C14 1.424(11) . ?
C14 C15 1.371(11) . ?
C15 C16 1.409(12) . ?
C15 H15A 0.9500 . ?
C16 C17 1.408(12) . ?
C16 C27 1.545(11) . ?
C17 C18 1.386(10) . ?
C17 H17A 0.9500 . ?
C19 C24 1.379(11) . ?
C19 C20 1.420(12) . ?
C20 C21 1.380(11) . ?
C21 C22 1.404(13) . ?
C21 H21A 0.9500 . ?
C22 C23 1.380(13) . ?
C22 C28 1.544(11) . ?
C23 C24 1.398(11) . ?
C23 H23A 0.9500 . ?
C25 C30 1.42(2) . ?
C25 C31 1.464(17) . ?
C25 C29 1.56(2) . ?
C26 C32 1.381(18) . ?
C26 C34 1.470(18) . ?
C26 C33 1.68(2) . ?
C27 C36 1.495(16) . ?
C27 C37 1.512(14) . ?
C27 C35 1.528(15) . ?
C28 C40 1.497(19) . ?
C28 C38 1.518(17) . ?
C28 C39 1.611(19) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 C46 1.378(10) . ?
C41 C42 1.388(10) . ?
C42 C43 1.392(12) . ?
C43 C44 1.367(16) . ?
C43 H43A 0.9500 . ?
C44 C45 1.370(15) . ?
C44 C47 1.498(13) . ?
C44 C47' 1.62(4) . ?
C45 C46 1.390(13) . ?
C45 H45A 0.9500 . ?
C47 C49 1.551(13) . ?
C47 C48 1.566(13) . ?
C47 C50 1.570(13) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C47' C49' 1.529(14) . ?
C47' C50' 1.537(14) . ?
C47' C48' 1.550(14) . ?
C48' H48D 0.9800 . ?
C48' H48E 0.9800 . ?
C48' H48F 0.9800 . ?
C49' H49D 0.9800 . ?
C49' H49E 0.9800 . ?
C49' H49F 0.9800 . ?
C50' H50D 0.9800 . ?
C50' H50E 0.9800 . ?
C50' H50F 0.9800 . ?
O14 C51 1.31(2) . ?
N1 C51 1.318(19) . ?
N1 C52 1.347(14) . ?
N1 C53 1.45(2) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C51 H51A 0.9500 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 C55 1.61(2) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 C57 1.58(2) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C54' C55' 1.61(3) . ?
C54' H54C 0.9900 . ?
C54' H54D 0.9900 . ?
C55' H55D 0.9800 . ?
C55' H55E 0.9800 . ?
C55' H55F 0.9800 . ?
C56' C57' 1.64(3) . ?
C56' H56C 0.9900 . ?
C56' H56D 0.9900 . ?
C57' H57D 0.9800 . ?
C57' H57E 0.9800 . ?
C57' H57F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Fe1 O11 172.6(2) . . ?
O1 Fe1 O4 94.72(16) . . ?
O11 Fe1 O4 92.7(2) . . ?
O1 Fe1 O7 92.0(2) . . ?
O11 Fe1 O7 80.56(16) . . ?
O4 Fe1 O7 173.3(2) . . ?
O1 Fe1 S1 80.56(14) . . ?
O11 Fe1 S1 100.38(16) . . ?
O4 Fe1 S1 80.25(14) . . ?
O7 Fe1 S1 101.00(15) . . ?
O1 Fe1 Cl1 82.50(14) . . ?
O11 Fe1 Cl1 98.54(16) . . ?
O4 Fe1 Cl1 84.97(15) . . ?
O7 Fe1 Cl1 95.82(14) . . ?
S1 Fe1 Cl1 156.44(5) . . ?
O2 Fe2 O6 171.2(2) . . ?
O2 Fe2 O1 94.4(2) . . ?
O6 Fe2 O1 94.2(2) . . ?
O2 Fe2 O8 91.1(2) . 4_565 ?
O6 Fe2 O8 80.27(18) . 4_565 ?
O1 Fe2 O8 174.2(2) . 4_565 ?
O2 Fe2 S2 80.33(14) . . ?
O6 Fe2 S2 103.01(15) . . ?
O1 Fe2 S2 80.01(15) . . ?
O8 Fe2 S2 103.02(15) 4_565 . ?
O2 Fe2 Cl1 82.25(15) . . ?
O6 Fe2 Cl1 97.31(15) . . ?
O1 Fe2 Cl1 80.81(14) . . ?
O8 Fe2 Cl1 97.88(14) 4_565 . ?
S2 Fe2 Cl1 152.91(7) . . ?
O2 Fe3 O11 169.0(2) . 4_565 ?
O2 Fe3 O3 97.91(17) . . ?
O11 Fe3 O3 93.0(2) 4_565 . ?
O2 Fe3 O7 89.3(2) . 4_565 ?
O11 Fe3 O7 79.77(15) 4_565 4_565 ?
O3 Fe3 O7 172.7(2) . 4_565 ?
O2 Fe3 S3 79.96(15) . . ?
O11 Fe3 S3 101.25(16) 4_565 . ?
O3 Fe3 S3 80.30(15) . . ?
O7 Fe3 S3 101.86(15) 4_565 . ?
O2 Fe3 Cl1 83.16(15) . . ?
O11 Fe3 Cl1 98.82(15) 4_565 . ?
O3 Fe3 Cl1 84.00(14) . . ?
O7 Fe3 Cl1 96.14(14) 4_565 . ?
S3 Fe3 Cl1 155.04(5) . . ?
O10 Fe4 O3 172.4(3) . . ?
O10 Fe4 O12 86.5(3) . 4_565 ?
O3 Fe4 O12 89.9(3) . 4_565 ?
O10 Fe4 O4 92.1(2) . . ?
O3 Fe4 O4 90.9(2) . . ?
O12 Fe4 O4 174.9(3) 4_565 . ?
O10 Fe4 S4 106.9(2) . . ?
O3 Fe4 S4 80.53(15) . . ?
O12 Fe4 S4 105.7(2) 4_565 . ?
O4 Fe4 S4 79.40(14) . . ?
O5 Fe5 O8 167.2(2) . . ?
O5 Fe5 O5 96.8(3) . 4_565 ?
O8 Fe5 O5 95.99(19) . 4_565 ?
O5 Fe5 O6 87.99(19) . 3_655 ?
O8 Fe5 O6 79.24(19) . 3_655 ?
O5 Fe5 O6 173.92(19) 4_565 3_655 ?
O5 Fe5 S5 81.16(14) . 4_565 ?
O8 Fe5 S5 101.18(15) . 4_565 ?
O5 Fe5 S5 79.09(13) 4_565 4_565 ?
O6 Fe5 S5 105.43(14) 3_655 4_565 ?
O5 Fe5 Cl2 82.74(14) . . ?
O8 Fe5 Cl2 99.17(15) . . ?
O5 Fe5 Cl2 82.13(13) 4_565 . ?
O6 Fe5 Cl2 94.83(14) 3_655 . ?
S5 Fe5 Cl2 153.53(8) 4_565 . ?
O7 V1 O6 110.5(2) . . ?
O7 V1 O8 109.7(2) . . ?
O6 V1 O8 110.3(2) . . ?
O7 V1 O9 108.2(3) . . ?
O6 V1 O9 107.7(3) . . ?
O8 V1 O9 110.5(3) . . ?
O12 V2 O10 108.6(4) . . ?
O12 V2 O13 111.1(5) . . ?
O10 V2 O13 108.9(5) . . ?
O12 V2 O11 109.6(3) . . ?
O10 V2 O11 109.3(3) . . ?
O13 V2 O11 109.3(4) . . ?
Fe3 Cl1 Fe1 123.59(5) . . ?
Fe3 Cl1 Fe2 78.45(5) . . ?
Fe1 Cl1 Fe2 78.59(5) . . ?
Fe5 Cl2 Fe5 77.71(5) . 4_565 ?
Fe5 Cl2 Fe5 77.71(5) . 3_655 ?
Fe5 Cl2 Fe5 125.04(13) 4_565 3_655 ?
Fe5 Cl2 Fe5 125.04(13) . 2_665 ?
Fe5 Cl2 Fe5 77.71(5) 4_565 2_665 ?
Fe5 Cl2 Fe5 77.71(5) 3_655 2_665 ?
C24 S1 C2 104.2(3) . . ?
C24 S1 Fe1 94.3(3) . . ?
C2 S1 Fe1 94.8(2) . . ?
C8 S2 C6 103.1(4) . . ?
C8 S2 Fe2 94.9(3) . . ?
C6 S2 Fe2 94.9(2) . . ?
C12 S3 C14 100.5(3) . . ?
C12 S3 Fe3 95.5(2) . . ?
C14 S3 Fe3 94.7(2) . . ?
C20 S4 C18 103.8(4) . . ?
C20 S4 Fe4 95.5(3) . . ?
C18 S4 Fe4 94.4(2) . . ?
C46 S5 C42 102.3(4) . 3_655 ?
C46 S5 Fe5 95.9(3) . 3_655 ?
C42 S5 Fe5 94.1(2) 3_655 3_655 ?
C1 O1 Fe1 124.7(5) . . ?
C1 O1 Fe2 123.0(5) . . ?
Fe1 O1 Fe2 110.4(2) . . ?
C7 O2 Fe2 124.3(4) . . ?
C7 O2 Fe3 124.9(4) . . ?
Fe2 O2 Fe3 110.8(2) . . ?
C13 O3 Fe4 123.0(5) . . ?
C13 O3 Fe3 124.7(5) . . ?
Fe4 O3 Fe3 111.4(2) . . ?
C19 O4 Fe1 123.1(5) . . ?
C19 O4 Fe4 125.1(5) . . ?
Fe1 O4 Fe4 110.0(2) . . ?
C41 O5 Fe5 123.5(4) . . ?
C41 O5 Fe5 125.2(4) . 3_655 ?
Fe5 O5 Fe5 110.9(2) . 3_655 ?
V1 O6 Fe2 129.3(3) . . ?
V1 O6 Fe5 132.8(3) . 4_565 ?
Fe2 O6 Fe5 96.99(19) . 4_565 ?
V1 O7 Fe1 131.2(3) . . ?
V1 O7 Fe3 131.6(3) . 3_655 ?
Fe1 O7 Fe3 96.6(2) . 3_655 ?
V1 O8 Fe5 127.6(3) . . ?
V1 O8 Fe2 130.1(3) . 3_655 ?
Fe5 O8 Fe2 101.2(2) . 3_655 ?
C56' O9 V1 136(2) . . ?
C56 O9 V1 132.8(14) . . ?
V2 O10 Fe4 133.3(4) . . ?
V2 O11 Fe1 129.2(3) . . ?
V2 O11 Fe3 129.1(3) . 3_655 ?
Fe1 O11 Fe3 101.0(2) . 3_655 ?
V2 O12 Fe4 135.4(4) . 3_655 ?
C54 O13 V2 145.1(16) . . ?
C54' O13 V2 134(2) . . ?
O1 C1 C6 122.5(7) . . ?
O1 C1 C2 121.5(7) . . ?
C6 C1 C2 116.0(6) . . ?
C3 C2 C1 121.7(8) . . ?
C3 C2 S1 120.3(6) . . ?
C1 C2 S1 117.9(5) . . ?
C2 C3 C4 121.1(8) . . ?
C2 C3 H3A 119.5 . . ?
C4 C3 H3A 119.5 . . ?
C5 C4 C3 117.3(8) . . ?
C5 C4 C25 121.2(9) . . ?
C3 C4 C25 121.3(9) . . ?
C4 C5 C6 123.0(8) . . ?
C4 C5 H5A 118.5 . . ?
C6 C5 H5A 118.5 . . ?
C1 C6 C5 120.9(7) . . ?
C1 C6 S2 118.5(5) . . ?
C5 C6 S2 120.5(6) . . ?
O2 C7 C8 121.4(6) . . ?
O2 C7 C12 121.3(6) . . ?
C8 C7 C12 117.4(6) . . ?
C9 C8 C7 119.0(8) . . ?
C9 C8 S2 121.9(7) . . ?
C7 C8 S2 119.0(5) . . ?
C10 C9 C8 123.9(9) . . ?
C10 C9 H9A 118.0 . . ?
C8 C9 H9A 118.0 . . ?
C9 C10 C11 118.1(8) . . ?
C9 C10 C26 124.0(10) . . ?
C11 C10 C26 117.8(9) . . ?
C12 C11 C10 120.1(8) . . ?
C12 C11 H11A 120.0 . . ?
C10 C11 H11A 120.0 . . ?
C11 C12 C7 121.4(8) . . ?
C11 C12 S3 120.2(6) . . ?
C7 C12 S3 118.4(5) . . ?
O3 C13 C18 123.6(7) . . ?
O3 C13 C14 121.2(7) . . ?
C18 C13 C14 115.3(7) . . ?
C15 C14 C13 123.0(7) . . ?
C15 C14 S3 118.0(6) . . ?
C13 C14 S3 119.0(6) . . ?
C14 C15 C16 120.7(8) . . ?
C14 C15 H15A 119.7 . . ?
C16 C15 H15A 119.7 . . ?
C17 C16 C15 117.3(7) . . ?
C17 C16 C27 124.3(8) . . ?
C15 C16 C27 118.1(8) . . ?
C18 C17 C16 120.9(7) . . ?
C18 C17 H17A 119.5 . . ?
C16 C17 H17A 119.5 . . ?
C17 C18 C13 122.8(7) . . ?
C17 C18 S4 119.2(6) . . ?
C13 C18 S4 118.0(6) . . ?
O4 C19 C24 122.7(7) . . ?
O4 C19 C20 120.0(7) . . ?
C24 C19 C20 117.3(7) . . ?
C21 C20 C19 121.2(8) . . ?
C21 C20 S4 119.9(6) . . ?
C19 C20 S4 118.8(6) . . ?
C20 C21 C22 120.9(8) . . ?
C20 C21 H21A 119.5 . . ?
C22 C21 H21A 119.5 . . ?
C23 C22 C21 117.3(7) . . ?
C23 C22 C28 123.3(9) . . ?
C21 C22 C28 119.4(8) . . ?
C22 C23 C24 122.1(8) . . ?
C22 C23 H23A 119.0 . . ?
C24 C23 H23A 119.0 . . ?
C19 C24 C23 120.9(8) . . ?
C19 C24 S1 119.2(6) . . ?
C23 C24 S1 119.8(7) . . ?
C30 C25 C31 109.2(14) . . ?
C30 C25 C4 109.6(11) . . ?
C31 C25 C4 110.8(9) . . ?
C30 C25 C29 113.1(15) . . ?
C31 C25 C29 104.3(13) . . ?
C4 C25 C29 109.6(11) . . ?
C32 C26 C34 118.8(11) . . ?
C32 C26 C10 115.3(11) . . ?
C34 C26 C10 113.3(10) . . ?
C32 C26 C33 104.2(11) . . ?
C34 C26 C33 96.8(12) . . ?
C10 C26 C33 104.9(11) . . ?
C36 C27 C37 106.5(9) . . ?
C36 C27 C35 110.6(10) . . ?
C37 C27 C35 110.1(9) . . ?
C36 C27 C16 110.4(8) . . ?
C37 C27 C16 110.4(8) . . ?
C35 C27 C16 108.8(8) . . ?
C40 C28 C38 110.4(13) . . ?
C40 C28 C22 112.5(10) . . ?
C38 C28 C22 110.3(9) . . ?
C40 C28 C39 107.2(10) . . ?
C38 C28 C39 110.0(12) . . ?
C22 C28 C39 106.3(10) . . ?
C25 C29 H29A 109.5 . . ?
C25 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C25 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C25 C30 H30A 109.5 . . ?
C25 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C25 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C25 C31 H31A 109.5 . . ?
C25 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C25 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C26 C32 H32A 109.5 . . ?
C26 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C26 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C26 C33 H33A 109.5 . . ?
C26 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C26 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C26 C34 H34A 109.5 . . ?
C26 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C26 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C27 C35 H35A 109.5 . . ?
C27 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C27 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C27 C36 H36A 109.5 . . ?
C27 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C27 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C27 C37 H37A 109.5 . . ?
C27 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C27 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C28 C38 H38A 109.5 . . ?
C28 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C28 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C28 C39 H39A 109.5 . . ?
C28 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C28 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C28 C40 H40A 109.5 . . ?
C28 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C28 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
O5 C41 C46 121.0(6) . . ?
O5 C41 C42 121.8(6) . . ?
C46 C41 C42 117.2(7) . . ?
C41 C42 C43 121.6(8) . . ?
C41 C42 S5 119.2(5) . 4_565 ?
C43 C42 S5 119.0(7) . 4_565 ?
C44 C43 C42 122.0(9) . . ?
C44 C43 H43A 119.0 . . ?
C42 C43 H43A 119.0 . . ?
C43 C44 C45 115.1(10) . . ?
C43 C44 C47 118.2(12) . . ?
C45 C44 C47 123.8(13) . . ?
C43 C44 C47' 118.1(14) . . ?
C45 C44 C47' 124.9(14) . . ?
C44 C45 C46 125.1(9) . . ?
C44 C45 H45A 117.5 . . ?
C46 C45 H45A 117.5 . . ?
C41 C46 C45 119.0(8) . . ?
C41 C46 S5 118.7(6) . . ?
C45 C46 S5 122.4(7) . . ?
C44 C47 C49 110(2) . . ?
C44 C47 C48 117(2) . . ?
C49 C47 C48 107.8(11) . . ?
C44 C47 C50 103.7(19) . . ?
C49 C47 C50 109.1(12) . . ?
C48 C47 C50 108.8(11) . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C47 C49 H49A 109.5 . . ?
C47 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C47 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C47 C50 H50A 109.5 . . ?
C47 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C47 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C49' C47' C50' 113.3(14) . . ?
C49' C47' C48' 112.4(14) . . ?
C50' C47' C48' 111.0(13) . . ?
C49' C47' C44 103(3) . . ?
C50' C47' C44 115(3) . . ?
C48' C47' C44 102(2) . . ?
C47' C48' H48D 109.5 . . ?
C47' C48' H48E 109.5 . . ?
H48D C48' H48E 109.5 . . ?
C47' C48' H48F 109.5 . . ?
H48D C48' H48F 109.5 . . ?
H48E C48' H48F 109.5 . . ?
C47' C49' H49D 109.5 . . ?
C47' C49' H49E 109.5 . . ?
H49D C49' H49E 109.5 . . ?
C47' C49' H49F 109.5 . . ?
H49D C49' H49F 109.5 . . ?
H49E C49' H49F 109.5 . . ?
C47' C50' H50D 109.5 . . ?
C47' C50' H50E 109.5 . . ?
H50D C50' H50E 109.5 . . ?
C47' C50' H50F 109.5 . . ?
H50D C50' H50F 109.5 . . ?
H50E C50' H50F 109.5 . . ?
C51 N1 C52 129.4(14) . . ?
C51 N1 C53 111.5(15) . . ?
C52 N1 C53 114.0(13) . . ?
N1 C52 H52A 109.5 . . ?
N1 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
N1 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
O14 C51 N1 135(2) . . ?
O14 C51 H51A 112.6 . . ?
N1 C51 H51A 112.6 . . ?
N1 C53 H53A 109.5 . . ?
N1 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
N1 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
O13 C54 C55 110(2) . . ?
O13 C54 H54A 109.7 . . ?
C55 C54 H54A 109.7 . . ?
O13 C54 H54B 109.7 . . ?
C55 C54 H54B 109.7 . . ?
H54A C54 H54B 108.2 . . ?
C54 C55 H55A 109.5 . . ?
C54 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C54 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
O9 C56 C57 116(2) . . ?
O9 C56 H56A 108.3 . . ?
C57 C56 H56A 108.3 . . ?
O9 C56 H56B 108.3 . . ?
C57 C56 H56B 108.3 . . ?
H56A C56 H56B 107.4 . . ?
C56 C57 H57A 109.5 . . ?
C56 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C56 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
O13 C54' C55' 111(4) . . ?
O13 C54' H54C 109.5 . . ?
C55' C54' H54C 109.5 . . ?
O13 C54' H54D 109.5 . . ?
C55' C54' H54D 109.5 . . ?
H54C C54' H54D 108.1 . . ?
C54' C55' H55D 109.5 . . ?
C54' C55' H55E 109.5 . . ?
H55D C55' H55E 109.5 . . ?
C54' C55' H55F 109.5 . . ?
H55D C55' H55F 109.5 . . ?
H55E C55' H55F 109.5 . . ?
O9 C56' C57' 110(2) . . ?
O9 C56' H56C 109.7 . . ?
C57' C56' H56C 109.7 . . ?
O9 C56' H56D 109.7 . . ?
C57' C56' H56D 109.7 . . ?
H56C C56' H56D 108.2 . . ?
C56' C57' H57D 109.5 . . ?
C56' C57' H57E 109.5 . . ?
H57D C57' H57E 109.5 . . ?
C56' C57' H57F 109.5 . . ?
H57D C57' H57F 109.5 . . ?
H57E C57' H57F 109.5 . . ?

_refine_diff_density_max         1.063
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.098

# start Validation Reply Form
_vrf_PLAT201_Fe20V8              
;
PROBLEM:  Isotropic non-H Atoms in Main Residue(s) .......9 Report.  
RESPONSE: The disordered t-Bu groups and carbethoxy were refined isotropically.
;
_vrf_PLAT242_Fe20V8              
;
PROBLEM: Low  MainMol Ueq as Compared to Neighbors of    O9 Check. 
RESPONSE:  It is due to disorder.
;
_vrf_FORMU01_Fe20V8              
;
PROBLEM:  Difference between formula and atom_site contents detected.
RESPONSE:  Solvent molecues (8DMF and one CH3CH2OH) determined by SQUEEZE 
and one H atom per cluster to balance the whole charge were included
in the formula directly.
;
_vrf_CELLZ01_Fe20V8              
;
PROBLEM:  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and the formula from the _atom_site* data.
RESPONSE:  Solvent molecues (8DMF and one CH3CH2OH) determined by SQUEEZE 
and one H atom per cluster to balance the whole charge were included
in the formula directly.
;
# end Validation Reply Form




####################################################################### 
# 
# 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_Ni20V8
_database_code_depnum_ccdc_archive 'CCDC 2434505'
loop_
_audit_author_name
_audit_author_address
'Yanfeng Bi'
;Liaoning Petrochemical University
China
;
_audit_update_record             
;
2025-05-08 deposited with the CCDC.	2025-05-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/1
_shelx_SHELXL_version_number     2019/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C216 H260 Cl5 Ni20 O52 S20 V8, 5(C2 H6 O), 12(C3 H7 N O)'
_chemical_formula_sum            'C262 H375 Cl5 N12 Ni20 O69 S20 V8'
_chemical_formula_weight         7196.89

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 '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      tetragonal
_space_group_IT_number           79
_space_group_name_H-M_alt        'I 4'
_space_group_name_Hall           'I 4'

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

_cell_length_a                   26.771(2)
_cell_length_b                   26.771(2)
_cell_length_c                   23.0428(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     16515(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9843
_cell_measurement_theta_min      2.3323
_cell_measurement_theta_max      25.0090

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_F_000             7464
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    1.559
_shelx_estimated_absorpt_T_min   0.777
_shelx_estimated_absorpt_T_max   0.788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6479
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            75315
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.406
_diffrn_reflns_theta_max         25.023
_diffrn_reflns_theta_full        25.023
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.899
_diffrn_reflns_point_group_measured_fraction_full 0.899
_reflns_number_total             13127
_reflns_number_gt                12406
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.754
_reflns_Friedel_fraction_max     0.794
_reflns_Friedel_fraction_full    0.794

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'Bruker Instrument Service vV6.2.3'
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_molecular_graphics    'Diamond 3.2K'
_computing_publication_material  'Adobe Photoshop CS6 and POV-Ray v3.7'
_refine_special_details          
'Refined as a 2-component inversion twin.,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)+(0.0741P)²+34.2669P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.462(15)
_chemical_absolute_configuration unk
_refine_ls_number_reflns         13127
_refine_ls_number_parameters     867
_refine_ls_number_restraints     193
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0380
_refine_ls_wR_factor_ref         0.1075
_refine_ls_wR_factor_gt          0.1049
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.31094(2) 0.48827(2) 0.63438(4) 0.01974(15) Uani 1 1 d . . . . .
Ni2 Ni 0.35559(3) 0.41410(3) 0.53292(4) 0.01775(18) Uani 1 1 d . . . . .
Ni3 Ni 0.40098(2) 0.33865(2) 0.63369(4) 0.02104(16) Uani 1 1 d . . . . .
Ni4 Ni 0.35688(3) 0.41528(3) 0.73899(4) 0.0259(2) Uani 1 1 d . . . . .
Ni5 Ni 0.45359(2) 0.57425(2) 0.43792(3) 0.01668(16) Uani 1 1 d . . . . .
V1 V 0.34889(4) 0.53747(4) 0.50504(4) 0.0161(2) Uani 1 1 d . . . . .
V2 V 0.34945(5) 0.53956(4) 0.76040(5) 0.0278(3) Uani 1 1 d . . . . .
Cl1 Cl 0.39664(5) 0.43905(5) 0.62893(8) 0.0274(3) Uani 1 1 d . . . . .
Cl2 Cl 0.500000 0.500000 0.49289(12) 0.0214(6) Uani 1 4 d S T P . .
S1 S 0.22064(4) 0.50205(5) 0.63571(9) 0.0227(3) Uani 1 1 d . . . . .
S2 S 0.29280(6) 0.37811(6) 0.46669(7) 0.0222(3) Uani 1 1 d . . . . .
S3 S 0.36710(5) 0.25414(4) 0.63382(9) 0.0239(3) Uani 1 1 d . . . . .
S4 S 0.29579(7) 0.37827(6) 0.80365(8) 0.0269(4) Uani 1 1 d . . . . .
S5 S 0.37899(5) 0.42142(5) 0.35451(7) 0.0215(3) Uani 1 1 d . . . . .
O1 O 0.29526(16) 0.44019(16) 0.5730(2) 0.0216(10) Uani 1 1 d . . . . .
O2 O 0.35279(16) 0.34814(16) 0.57019(19) 0.0222(10) Uani 1 1 d . . . . .
O3 O 0.35358(16) 0.34992(16) 0.6984(2) 0.0236(10) Uani 1 1 d . . . . .
O4 O 0.29678(16) 0.44005(16) 0.6973(2) 0.0236(10) Uani 1 1 d . . . . .
O5 O 0.42454(14) 0.51705(13) 0.39547(17) 0.0189(8) Uani 1 1 d . . . . .
O6 O 0.33019(17) 0.54195(15) 0.5751(2) 0.0227(10) Uani 1 1 d . . . . .
O7 O 0.36920(17) 0.47843(15) 0.49003(19) 0.0215(9) Uani 1 1 d . . . . .
O8 O 0.39445(16) 0.58000(16) 0.4909(2) 0.0212(9) Uani 1 1 d . . . . .
O9 O 0.29743(18) 0.5501(2) 0.4598(2) 0.0422(13) Uani 1 1 d D . . . .
O10 O 0.3648(2) 0.4819(2) 0.7767(2) 0.0462(15) Uani 1 1 d . . . . .
O11 O 0.33089(17) 0.54199(16) 0.6894(2) 0.0250(10) Uani 1 1 d . . . . .
O12 O 0.3976(2) 0.5773(2) 0.7723(3) 0.0472(15) Uani 1 1 d . . . . .
O13 O 0.3008(3) 0.5602(4) 0.8049(3) 0.088(3) Uani 1 1 d . U . . .
C1 C 0.2503(2) 0.4375(2) 0.5495(3) 0.0207(13) Uani 1 1 d . . . . .
C2 C 0.2085(2) 0.4634(2) 0.5742(3) 0.0232(14) Uani 1 1 d . . . . .
C3 C 0.1627(3) 0.4612(3) 0.5488(3) 0.0284(15) Uani 1 1 d . . . . .
H3A H 0.135697 0.478511 0.566462 0.034 Uiso 1 1 calc R U . . .
C4 C 0.1536(3) 0.4344(3) 0.4973(3) 0.0313(16) Uani 1 1 d . . . . .
C5 C 0.1944(3) 0.4095(3) 0.4740(3) 0.0282(15) Uani 1 1 d . . . . .
H5A H 0.189772 0.391167 0.439082 0.034 Uiso 1 1 calc R U . . .
C6 C 0.2410(2) 0.4100(2) 0.4986(3) 0.0246(14) Uani 1 1 d . . . . .
C7 C 0.3234(2) 0.3116(2) 0.5496(3) 0.0197(13) Uani 1 1 d . . . . .
C8 C 0.2914(2) 0.3190(2) 0.5038(3) 0.0244(14) Uani 1 1 d . . . . .
C9 C 0.2604(3) 0.2811(3) 0.4847(3) 0.0302(16) Uani 1 1 d . . . . .
H9A H 0.238481 0.287367 0.453185 0.036 Uiso 1 1 calc R U . . .
C10 C 0.2604(3) 0.2342(3) 0.5101(3) 0.0355(18) Uani 1 1 d . . . . .
C11 C 0.2938(3) 0.2263(3) 0.5561(3) 0.0328(17) Uani 1 1 d . . . . .
H11A H 0.295431 0.194411 0.574000 0.039 Uiso 1 1 calc R U . . .
C12 C 0.3243(2) 0.2643(2) 0.5757(3) 0.0234(14) Uani 1 1 d . . . . .
C13 C 0.3269(2) 0.3129(2) 0.7198(3) 0.0239(14) Uani 1 1 d . . . . .
C14 C 0.3276(2) 0.2648(2) 0.6952(3) 0.0223(14) Uani 1 1 d . . . . .
C15 C 0.2981(3) 0.2266(2) 0.7160(3) 0.0259(15) Uani 1 1 d . . . . .
H15A H 0.299911 0.194773 0.697868 0.031 Uiso 1 1 calc R U . . .
C16 C 0.2658(3) 0.2332(3) 0.7624(3) 0.0292(16) Uani 1 1 d . . . . .
C17 C 0.2653(3) 0.2802(3) 0.7888(3) 0.0293(16) Uani 1 1 d . . . . .
H17A H 0.244408 0.285692 0.821524 0.035 Uiso 1 1 calc R U . . .
C18 C 0.2951(2) 0.3194(2) 0.7679(3) 0.0229(14) Uani 1 1 d . . . . .
C19 C 0.2519(2) 0.4382(2) 0.7213(3) 0.0242(14) Uani 1 1 d . . . . .
C20 C 0.2441(3) 0.4107(2) 0.7723(3) 0.0252(15) Uani 1 1 d . . . . .
C21 C 0.1975(3) 0.4084(3) 0.7986(3) 0.0312(16) Uani 1 1 d . . . . .
H21A H 0.193307 0.389501 0.833101 0.037 Uiso 1 1 calc R U . . .
C22 C 0.1563(3) 0.4339(3) 0.7746(3) 0.0329(17) Uani 1 1 d . . . . .
C23 C 0.1633(3) 0.4608(3) 0.7246(3) 0.0306(16) Uani 1 1 d . . . . .
H23A H 0.136081 0.478316 0.707782 0.037 Uiso 1 1 calc R U . . .
C24 C 0.2114(3) 0.4627(2) 0.6976(3) 0.0265(15) Uani 1 1 d . . . . .
C25 C 0.1035(3) 0.4343(3) 0.4657(4) 0.043(2) Uani 1 1 d . . . . .
C26 C 0.2290(4) 0.1903(3) 0.4870(4) 0.056(3) Uani 1 1 d . . . . .
C27 C 0.2352(3) 0.1892(3) 0.7856(4) 0.0366(18) Uani 1 1 d . . . . .
C28 C 0.1050(3) 0.4311(3) 0.8054(4) 0.047(2) Uani 1 1 d . . . . .
C29 C 0.0638(4) 0.4615(7) 0.5002(7) 0.126(6) Uani 1 1 d . U . . .
H29A H 0.073868 0.496368 0.505763 0.189 Uiso 1 1 calc R U . . .
H29B H 0.032041 0.460418 0.478979 0.189 Uiso 1 1 calc R U . . .
H29C H 0.059671 0.445375 0.538033 0.189 Uiso 1 1 calc R U . . .
C30 C 0.1097(5) 0.4574(6) 0.4058(7) 0.118(6) Uani 1 1 d . U . . .
H30A H 0.121060 0.492005 0.409806 0.177 Uiso 1 1 calc R U . . .
H30B H 0.134382 0.438250 0.383664 0.177 Uiso 1 1 calc R U . . .
H30C H 0.077567 0.456774 0.385421 0.177 Uiso 1 1 calc R U . . .
C31 C 0.0862(4) 0.3816(4) 0.4585(6) 0.076(4) Uani 1 1 d . . . . .
H31A H 0.111058 0.362745 0.436329 0.113 Uiso 1 1 calc R U . . .
H31B H 0.081877 0.366258 0.496804 0.113 Uiso 1 1 calc R U . . .
H31C H 0.054247 0.381301 0.437750 0.113 Uiso 1 1 calc R U . . .
C32 C 0.1895(4) 0.2057(4) 0.4462(4) 0.057(2) Uani 1 1 d . . . . .
H32A H 0.166676 0.228910 0.465559 0.085 Uiso 1 1 calc R U . . .
H32B H 0.204732 0.222226 0.412566 0.085 Uiso 1 1 calc R U . . .
H32C H 0.170951 0.176206 0.433164 0.085 Uiso 1 1 calc R U . . .
C33 C 0.2635(5) 0.1546(4) 0.4558(5) 0.074(4) Uani 1 1 d . . . . .
H33A H 0.290083 0.143864 0.482270 0.112 Uiso 1 1 calc R U . . .
H33B H 0.244535 0.125372 0.442755 0.112 Uiso 1 1 calc R U . . .
H33C H 0.278316 0.171392 0.422157 0.112 Uiso 1 1 calc R U . . .
C34 C 0.2052(5) 0.1606(4) 0.5367(5) 0.077(4) Uani 1 1 d . . . . .
H34A H 0.231189 0.150180 0.564110 0.115 Uiso 1 1 calc R U . . .
H34B H 0.180704 0.181574 0.556846 0.115 Uiso 1 1 calc R U . . .
H34C H 0.188442 0.130961 0.521002 0.115 Uiso 1 1 calc R U . . .
C35 C 0.2136(4) 0.1601(3) 0.7352(4) 0.056(2) Uani 1 1 d . . . . .
H35A H 0.240632 0.149453 0.709374 0.083 Uiso 1 1 calc R U . . .
H35B H 0.195927 0.130650 0.749975 0.083 Uiso 1 1 calc R U . . .
H35C H 0.190200 0.181325 0.713741 0.083 Uiso 1 1 calc R U . . .
C36 C 0.2713(3) 0.1538(3) 0.8197(5) 0.053(2) Uani 1 1 d . . . . .
H36A H 0.298050 0.142541 0.793808 0.079 Uiso 1 1 calc R U . . .
H36B H 0.285747 0.171955 0.852555 0.079 Uiso 1 1 calc R U . . .
H36C H 0.252589 0.124863 0.833956 0.079 Uiso 1 1 calc R U . . .
C37 C 0.1943(3) 0.2061(3) 0.8262(4) 0.047(2) Uani 1 1 d . . . . .
H37A H 0.209010 0.224866 0.858478 0.070 Uiso 1 1 calc R U . . .
H37B H 0.170839 0.227545 0.805121 0.070 Uiso 1 1 calc R U . . .
H37C H 0.176566 0.176870 0.841356 0.070 Uiso 1 1 calc R U . . .
C38 C 0.1123(5) 0.4490(6) 0.8676(6) 0.100(4) Uani 1 1 d . U . . .
H38A H 0.138245 0.428881 0.886337 0.150 Uiso 1 1 calc R U . . .
H38B H 0.122359 0.484151 0.867382 0.150 Uiso 1 1 calc R U . . .
H38C H 0.080835 0.445380 0.888990 0.150 Uiso 1 1 calc R U . . .
C39 C 0.0658(4) 0.4601(5) 0.7741(7) 0.098(5) Uani 1 1 d . U . . .
H39A H 0.062466 0.447315 0.734422 0.147 Uiso 1 1 calc R U . . .
H39B H 0.033852 0.456653 0.794426 0.147 Uiso 1 1 calc R U . . .
H39C H 0.075377 0.495424 0.772817 0.147 Uiso 1 1 calc R U . . .
C40 C 0.0892(4) 0.3765(5) 0.8107(7) 0.088(4) Uani 1 1 d . U . . .
H40A H 0.115198 0.357773 0.831351 0.131 Uiso 1 1 calc R U . . .
H40B H 0.057790 0.374414 0.832368 0.131 Uiso 1 1 calc R U . . .
H40C H 0.084605 0.362291 0.771916 0.131 Uiso 1 1 calc R U . . .
C41 C 0.3988(2) 0.5220(2) 0.3475(2) 0.0224(12) Uani 1 1 d . U . . .
C42 C 0.3749(2) 0.4811(2) 0.3207(3) 0.0299(14) Uani 1 1 d . U . . .
C43 C 0.3489(3) 0.4866(3) 0.2694(4) 0.055(2) Uani 1 1 d . U . . .
H43A H 0.334288 0.458007 0.251955 0.066 Uiso 1 1 calc R U . . .
C44 C 0.3435(4) 0.5325(3) 0.2426(5) 0.073(3) Uani 1 1 d . U . . .
C45 C 0.3661(3) 0.5732(3) 0.2689(4) 0.051(2) Uani 1 1 d . U . . .
H45A H 0.363210 0.605183 0.251449 0.061 Uiso 1 1 calc R U . . .
C46 C 0.3928(3) 0.5683(2) 0.3203(3) 0.0334(15) Uani 1 1 d . U . . .
C47 C 0.3110(6) 0.5392(4) 0.1893(5) 0.123(4) Uani 1 1 d D U . . .
C48 C 0.3322(6) 0.5784(5) 0.1483(5) 0.118(5) Uani 1 1 d D U . . .
H48A H 0.340223 0.608719 0.170145 0.177 Uiso 1 1 calc R U . . .
H48B H 0.362521 0.565409 0.129892 0.177 Uiso 1 1 calc R U . . .
H48C H 0.307382 0.586239 0.118324 0.177 Uiso 1 1 calc R U . . .
C49 C 0.2974(7) 0.4912(5) 0.1600(6) 0.150(5) Uani 1 1 d D U . . .
H49A H 0.276443 0.498196 0.126105 0.225 Uiso 1 1 calc R U . . .
H49B H 0.327866 0.473947 0.147563 0.225 Uiso 1 1 calc R U . . .
H49C H 0.278948 0.469877 0.187199 0.225 Uiso 1 1 calc R U . . .
C50 C 0.2593(6) 0.5603(8) 0.2087(8) 0.159(6) Uani 1 1 d D U . . .
H50A H 0.264160 0.592235 0.228694 0.239 Uiso 1 1 calc R U . . .
H50B H 0.238121 0.565331 0.174554 0.239 Uiso 1 1 calc R U . . .
H50C H 0.243215 0.536520 0.235117 0.239 Uiso 1 1 calc R U . . .
N1 N 0.1535(3) 0.3262(3) 0.6240(5) 0.080(2) Uani 1 1 d . U . . .
O14 O 0.0725(3) 0.3579(4) 0.6247(6) 0.122(3) Uani 1 1 d . U . . .
C51 C 0.1167(4) 0.3567(4) 0.6394(7) 0.087(3) Uani 1 1 d . U . . .
H51A H 0.126100 0.381954 0.666317 0.104 Uiso 1 1 calc R U . . .
C52 C 0.2046(4) 0.3281(4) 0.6373(7) 0.090(3) Uani 1 1 d . U . . .
H52A H 0.221632 0.299745 0.619075 0.135 Uiso 1 1 calc R U . . .
H52B H 0.218745 0.359373 0.622676 0.135 Uiso 1 1 calc R U . . .
H52C H 0.208984 0.326395 0.679480 0.135 Uiso 1 1 calc R U . . .
C53 C 0.1427(5) 0.2950(5) 0.5725(6) 0.096(4) Uani 1 1 d . U . . .
H53A H 0.171597 0.273672 0.564130 0.144 Uiso 1 1 calc R U . . .
H53B H 0.113454 0.274056 0.580256 0.144 Uiso 1 1 calc R U . . .
H53C H 0.136006 0.316590 0.539086 0.144 Uiso 1 1 calc R U . . .
N2 N 0.0647(4) 0.5933(5) 0.6994(7) 0.111(3) Uani 1 1 d . U . . .
O15 O 0.0709(3) 0.5238(3) 0.6406(6) 0.110(3) Uani 1 1 d . U . . .
C54 C 0.0465(5) 0.5571(6) 0.6616(7) 0.104(4) Uani 1 1 d . U . . .
H54A H 0.012125 0.558744 0.651622 0.125 Uiso 1 1 calc R U . . .
C55 C 0.0324(6) 0.6336(7) 0.7233(9) 0.132(5) Uani 1 1 d . U . . .
H55A H 0.052239 0.655115 0.748841 0.198 Uiso 1 1 calc R U . . .
H55B H 0.018714 0.653489 0.691371 0.198 Uiso 1 1 calc R U . . .
H55C H 0.004980 0.618624 0.745481 0.198 Uiso 1 1 calc R U . . .
C56 C 0.1171(5) 0.5954(6) 0.7186(8) 0.113(4) Uani 1 1 d . U . . .
H56A H 0.121665 0.623772 0.744909 0.170 Uiso 1 1 calc R U . . .
H56B H 0.125641 0.564358 0.738817 0.170 Uiso 1 1 calc R U . . .
H56C H 0.138929 0.599427 0.684734 0.170 Uiso 1 1 calc R U . . .
N3 N 0.0811(4) 0.6427(6) 0.5622(6) 0.126(4) Uani 1 1 d . U . . .
O16 O 0.1175(2) 0.6932(3) 0.6311(5) 0.088(2) Uani 1 1 d . U . . .
C57 C 0.0830(6) 0.6794(7) 0.6006(8) 0.121(4) Uani 1 1 d . U . . .
H57A H 0.052874 0.697728 0.605140 0.145 Uiso 1 1 calc R U . . .
C58 C 0.1254(6) 0.6084(8) 0.5576(9) 0.144(5) Uani 1 1 d . U . . .
H58A H 0.119026 0.583118 0.527666 0.217 Uiso 1 1 calc R U . . .
H58B H 0.155129 0.627754 0.547025 0.217 Uiso 1 1 calc R U . . .
H58C H 0.131024 0.591824 0.594947 0.217 Uiso 1 1 calc R U . . .
C59 C 0.0360(7) 0.6263(9) 0.5365(9) 0.154(6) Uani 1 1 d . U . . .
H59A H 0.043162 0.598892 0.509445 0.231 Uiso 1 1 calc R U . . .
H59B H 0.013184 0.614468 0.566741 0.231 Uiso 1 1 calc R U . . .
H59C H 0.020521 0.653984 0.515331 0.231 Uiso 1 1 calc R U . . .
C60 C 0.2497(6) 0.5563(7) 0.8038(9) 0.155(9) Uani 1 1 d D . . . .
H60A H 0.239848 0.524225 0.821779 0.185 Uiso 1 1 calc R U . . .
H60B H 0.238382 0.555780 0.762884 0.185 Uiso 1 1 calc R U . . .
C61 C 0.2237(6) 0.5981(6) 0.8349(8) 0.132(6) Uani 1 1 d D . . . .
H61A H 0.187478 0.593208 0.832547 0.199 Uiso 1 1 calc R U . . .
H61B H 0.234049 0.598418 0.875665 0.199 Uiso 1 1 calc R U . . .
H61C H 0.232581 0.629999 0.816722 0.199 Uiso 1 1 calc R U . . .
C62 C 0.2485(5) 0.5629(8) 0.4690(9) 0.087(5) Uiso 0.602(16) 1 d D U P A 1
H62A H 0.246199 0.594735 0.490759 0.104 Uiso 0.602(16) 1 calc R U P A 1
H62B H 0.230974 0.536557 0.491200 0.104 Uiso 0.602(16) 1 calc R U P A 1
C63 C 0.2253(11) 0.5686(13) 0.4071(11) 0.134(7) Uiso 0.602(16) 1 d D U P A 1
H63A H 0.190033 0.577900 0.410568 0.202 Uiso 0.602(16) 1 calc R U P A 1
H63B H 0.243275 0.594724 0.385768 0.202 Uiso 0.602(16) 1 calc R U P A 1
H63C H 0.228142 0.536895 0.386206 0.202 Uiso 0.602(16) 1 calc R U P A 1
C62' C 0.2805(10) 0.5870(11) 0.4266(14) 0.108(7) Uiso 0.398(16) 1 d D U P A 2
H62C H 0.286560 0.577843 0.385576 0.130 Uiso 0.398(16) 1 calc R U P A 2
H62D H 0.300573 0.617152 0.434940 0.130 Uiso 0.398(16) 1 calc R U P A 2
C63' C 0.2255(9) 0.6007(12) 0.4329(16) 0.084(7) Uiso 0.398(16) 1 d D U P A 2
H63D H 0.217469 0.628176 0.406442 0.125 Uiso 0.398(16) 1 calc R U P A 2
H63E H 0.204794 0.571614 0.423420 0.125 Uiso 0.398(16) 1 calc R U P A 2
H63F H 0.218860 0.611070 0.472969 0.125 Uiso 0.398(16) 1 calc R U P A 2
O17 O 0.500000 0.500000 0.7060(8) 0.101(5) Uiso 1 4 d DS U P . .
H17B H 0.517964 0.513688 0.680735 0.152 Uiso 0.25 1 calc R U P . .
C64 C 0.504(3) 0.5263(11) 0.7567(8) 0.075(8) Uiso 0.25 1 d D U P . .
H64A H 0.479786 0.552598 0.756092 0.089 Uiso 0.25 1 d R U P . .
H64B H 0.536342 0.541979 0.756092 0.089 Uiso 0.25 1 d R U P . .
C65 C 0.500000 0.500000 0.8130(10) 0.087(6) Uiso 1 4 d DS U P . .
H65A H 0.476481 0.517473 0.838450 0.131 Uiso 0.25 1 d R U P . .
H65B H 0.487640 0.466199 0.805185 0.131 Uiso 0.25 1 d R U P . .
H65C H 0.532723 0.498026 0.831878 0.131 Uiso 0.25 1 d R U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 1.959(4) . ?
Ni1 O4 1.978(4) . ?
Ni1 O11 1.990(5) . ?
Ni1 O6 2.049(4) . ?
Ni1 S1 2.4456(14) . ?
Ni1 Cl1 2.6487(15) . ?
Ni2 O2 1.965(4) . ?
Ni2 O1 1.987(4) . ?
Ni2 O7 2.019(4) . ?
Ni2 O8 2.046(4) 3_655 ?
Ni2 S2 2.4666(18) . ?
Ni2 Cl1 2.5588(19) . ?
Ni3 O2 1.967(4) . ?
Ni3 O3 1.981(4) . ?
Ni3 O11 2.005(5) 3_655 ?
Ni3 O6 2.052(4) 3_655 ?
Ni3 S3 2.4375(14) . ?
Ni3 Cl1 2.6925(15) . ?
Ni4 O12 1.980(5) 3_655 ?
Ni4 O3 1.986(5) . ?
Ni4 O4 1.987(5) . ?
Ni4 O10 1.995(5) . ?
Ni4 S4 2.424(2) . ?
Ni5 O5 1.961(4) 4_565 ?
Ni5 O5 1.977(4) . ?
Ni5 O8 2.006(4) . ?
Ni5 O7 2.044(4) 4_565 ?
Ni5 S5 2.4500(16) 4_565 ?
Ni5 Cl2 2.6645(15) . ?
V1 O6 1.694(5) . ?
V1 O8 1.700(4) . ?
V1 O7 1.707(4) . ?
V1 O9 1.761(5) . ?
V2 O10 1.642(6) . ?
V2 O12 1.660(6) . ?
V2 O11 1.712(5) . ?
V2 O13 1.747(7) . ?
S1 C2 1.785(7) . ?
S1 C24 1.790(7) . ?
S2 C6 1.787(7) . ?
S2 C8 1.799(7) . ?
S3 C12 1.784(7) . ?
S3 C14 1.789(6) . ?
S4 C18 1.779(7) . ?
S4 C20 1.786(7) . ?
S5 C42 1.781(6) . ?
S5 C46 1.790(7) 3_655 ?
O1 C1 1.321(8) . ?
O2 C7 1.342(8) . ?
O3 C13 1.316(8) . ?
O4 C19 1.324(8) . ?
O5 C41 1.310(7) . ?
O9 C62' 1.328(13) . ?
O9 C62 1.371(12) . ?
O13 C60 1.373(17) . ?
C1 C6 1.407(10) . ?
C1 C2 1.435(9) . ?
C2 C3 1.360(10) . ?
C3 C4 1.407(11) . ?
C4 C5 1.387(10) . ?
C4 C25 1.527(10) . ?
C5 C6 1.370(10) . ?
C7 C8 1.376(10) . ?
C7 C12 1.401(9) . ?
C8 C9 1.382(10) . ?
C9 C10 1.383(10) . ?
C10 C11 1.402(11) . ?
C10 C26 1.541(10) . ?
C11 C12 1.380(10) . ?
C13 C14 1.408(10) . ?
C13 C18 1.408(10) . ?
C14 C15 1.378(9) . ?
C15 C16 1.387(10) . ?
C16 C17 1.397(10) . ?
C16 C27 1.530(9) . ?
C17 C18 1.404(10) . ?
C19 C24 1.380(10) . ?
C19 C20 1.404(10) . ?
C20 C21 1.388(10) . ?
C21 C22 1.409(11) . ?
C22 C23 1.373(11) . ?
C22 C28 1.547(10) . ?
C23 C24 1.430(10) . ?
C25 C31 1.494(14) . ?
C25 C29 1.515(15) . ?
C25 C30 1.521(15) . ?
C26 C32 1.473(14) . ?
C26 C33 1.512(15) . ?
C26 C34 1.534(13) . ?
C27 C37 1.510(12) . ?
C27 C35 1.512(13) . ?
C27 C36 1.564(12) . ?
C28 C39 1.491(15) . ?
C28 C38 1.523(16) . ?
C28 C40 1.525(15) . ?
C41 C46 1.397(9) . ?
C41 C42 1.410(9) . ?
C42 C43 1.380(10) . ?
C43 C44 1.383(11) . ?
C44 C45 1.385(12) . ?
C44 C47 1.516(13) . ?
C45 C46 1.389(10) . ?
C47 C49 1.498(11) . ?
C47 C48 1.522(11) . ?
C47 C50 1.559(12) . ?
N1 C51 1.329(13) . ?
N1 C52 1.401(14) . ?
N1 C53 1.479(15) . ?
O14 C51 1.232(15) . ?
N2 C54 1.391(19) . ?
N2 C56 1.471(19) . ?
N2 C55 1.487(19) . ?
O15 C54 1.207(16) . ?
N3 C57 1.322(19) . ?
N3 C59 1.42(2) . ?
N3 C58 1.51(2) . ?
O16 C57 1.219(17) . ?
C60 C61 1.500(12) . ?
C62 C63 1.562(13) . ?
C62' C63' 1.524(13) . ?
O17 C64 1.367(13) 4_565 ?
O17 C64 1.367(13) 3_655 ?
O17 C64 1.367(13) 2_665 ?
O17 C64 1.367(13) . ?
C64 C64 1.01(4) 4_565 ?
C64 C64 1.01(4) 3_655 ?
C64 C64 1.42(5) 2_665 ?
C64 C65 1.479(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
O1 Ni1 O4 93.44(15) . . ?
O1 Ni1 O11 173.06(19) . . ?
O4 Ni1 O11 93.2(2) . . ?
O1 Ni1 O6 91.89(18) . . ?
O4 Ni1 O6 174.16(19) . . ?
O11 Ni1 O6 81.38(14) . . ?
O1 Ni1 S1 84.05(13) . . ?
O4 Ni1 S1 84.26(13) . . ?
O11 Ni1 S1 98.53(14) . . ?
O6 Ni1 S1 98.69(13) . . ?
O1 Ni1 Cl1 79.89(13) . . ?
O4 Ni1 Cl1 82.88(13) . . ?
O11 Ni1 Cl1 99.04(14) . . ?
O6 Ni1 Cl1 95.71(13) . . ?
S1 Ni1 Cl1 158.73(5) . . ?
O2 Ni2 O1 94.70(19) . . ?
O2 Ni2 O7 170.92(18) . . ?
O1 Ni2 O7 94.25(18) . . ?
O2 Ni2 O8 90.44(18) . 3_655 ?
O1 Ni2 O8 174.31(18) . 3_655 ?
O7 Ni2 O8 80.55(17) . 3_655 ?
O2 Ni2 S2 83.88(13) . . ?
O1 Ni2 S2 82.56(14) . . ?
O7 Ni2 S2 98.81(14) . . ?
O8 Ni2 S2 100.45(14) 3_655 . ?
O2 Ni2 Cl1 82.71(13) . . ?
O1 Ni2 Cl1 81.72(14) . . ?
O7 Ni2 Cl1 97.08(13) . . ?
O8 Ni2 Cl1 96.55(13) 3_655 . ?
S2 Ni2 Cl1 158.37(6) . . ?
O2 Ni3 O3 96.89(15) . . ?
O2 Ni3 O11 171.38(19) . 3_655 ?
O3 Ni3 O11 91.26(19) . 3_655 ?
O2 Ni3 O6 90.75(18) . 3_655 ?
O3 Ni3 O6 171.60(19) . 3_655 ?
O11 Ni3 O6 80.95(14) 3_655 3_655 ?
O2 Ni3 S3 82.93(13) . . ?
O3 Ni3 S3 84.38(13) . . ?
O11 Ni3 S3 100.74(14) 3_655 . ?
O6 Ni3 S3 100.10(13) 3_655 . ?
O2 Ni3 Cl1 79.19(13) . . ?
O3 Ni3 Cl1 81.43(13) . . ?
O11 Ni3 Cl1 99.34(14) 3_655 . ?
O6 Ni3 Cl1 96.64(13) 3_655 . ?
S3 Ni3 Cl1 155.58(5) . . ?
O12 Ni4 O3 90.6(2) 3_655 . ?
O12 Ni4 O4 171.0(2) 3_655 . ?
O3 Ni4 O4 91.7(2) . . ?
O12 Ni4 O10 87.1(3) 3_655 . ?
O3 Ni4 O10 175.8(2) . . ?
O4 Ni4 O10 89.9(2) . . ?
O12 Ni4 S4 105.3(2) 3_655 . ?
O3 Ni4 S4 84.23(13) . . ?
O4 Ni4 S4 83.53(13) . . ?
O10 Ni4 S4 99.76(19) . . ?
O5 Ni5 O5 96.1(2) 4_565 . ?
O5 Ni5 O8 170.61(18) 4_565 . ?
O5 Ni5 O8 92.88(17) . . ?
O5 Ni5 O7 89.94(17) 4_565 4_565 ?
O5 Ni5 O7 173.13(18) . 4_565 ?
O8 Ni5 O7 80.92(18) . 4_565 ?
O5 Ni5 S5 84.53(12) 4_565 4_565 ?
O5 Ni5 S5 82.49(11) . 4_565 ?
O8 Ni5 S5 99.28(14) . 4_565 ?
O7 Ni5 S5 101.35(13) 4_565 4_565 ?
O5 Ni5 Cl2 81.10(12) 4_565 . ?
O5 Ni5 Cl2 80.83(11) . . ?
O8 Ni5 Cl2 97.80(14) . . ?
O7 Ni5 Cl2 96.99(13) 4_565 . ?
S5 Ni5 Cl2 156.63(7) 4_565 . ?
O6 V1 O8 110.3(2) . . ?
O6 V1 O7 110.7(2) . . ?
O8 V1 O7 110.7(2) . . ?
O6 V1 O9 108.6(2) . . ?
O8 V1 O9 108.6(3) . . ?
O7 V1 O9 107.9(2) . . ?
O10 V2 O12 109.9(3) . . ?
O10 V2 O11 109.1(2) . . ?
O12 V2 O11 111.1(3) . . ?
O10 V2 O13 110.5(4) . . ?
O12 V2 O13 106.8(4) . . ?
O11 V2 O13 109.4(3) . . ?
Ni2 Cl1 Ni1 78.40(5) . . ?
Ni2 Cl1 Ni3 78.07(5) . . ?
Ni1 Cl1 Ni3 122.14(5) . . ?
Ni5 Cl2 Ni5 76.94(5) . 3_655 ?
Ni5 Cl2 Ni5 76.94(5) . 4_565 ?
Ni5 Cl2 Ni5 123.24(11) 3_655 4_565 ?
Ni5 Cl2 Ni5 123.24(11) . 2_665 ?
Ni5 Cl2 Ni5 76.94(5) 3_655 2_665 ?
Ni5 Cl2 Ni5 76.94(5) 4_565 2_665 ?
C2 S1 C24 105.4(2) . . ?
C2 S1 Ni1 94.8(2) . . ?
C24 S1 Ni1 93.3(2) . . ?
C6 S2 C8 102.0(3) . . ?
C6 S2 Ni2 95.0(2) . . ?
C8 S2 Ni2 93.7(2) . . ?
C12 S3 C14 101.0(2) . . ?
C12 S3 Ni3 95.5(2) . . ?
C14 S3 Ni3 94.2(2) . . ?
C18 S4 C20 103.6(3) . . ?
C18 S4 Ni4 94.9(2) . . ?
C20 S4 Ni4 94.4(2) . . ?
C42 S5 C46 103.9(3) . 3_655 ?
C42 S5 Ni5 93.4(2) . 3_655 ?
C46 S5 Ni5 95.3(2) 3_655 3_655 ?
C1 O1 Ni1 121.8(4) . . ?
C1 O1 Ni2 122.1(4) . . ?
Ni1 O1 Ni2 113.1(2) . . ?
C7 O2 Ni2 121.6(4) . . ?
C7 O2 Ni3 123.5(4) . . ?
Ni2 O2 Ni3 114.6(2) . . ?
C13 O3 Ni3 121.0(4) . . ?
C13 O3 Ni4 120.7(4) . . ?
Ni3 O3 Ni4 117.4(2) . . ?
C19 O4 Ni1 120.3(4) . . ?
C19 O4 Ni4 121.4(4) . . ?
Ni1 O4 Ni4 114.6(2) . . ?
C41 O5 Ni5 121.2(3) . 3_655 ?
C41 O5 Ni5 123.1(3) . . ?
Ni5 O5 Ni5 114.71(19) 3_655 . ?
V1 O6 Ni1 131.3(2) . . ?
V1 O6 Ni3 130.3(2) . 4_565 ?
Ni1 O6 Ni3 96.38(19) . 4_565 ?
V1 O7 Ni2 129.3(2) . . ?
V1 O7 Ni5 131.0(2) . 3_655 ?
Ni2 O7 Ni5 98.26(18) . 3_655 ?
V1 O8 Ni5 129.2(2) . . ?
V1 O8 Ni2 131.2(2) . 4_565 ?
Ni5 O8 Ni2 98.60(18) . 4_565 ?
C62' O9 V1 138.6(15) . . ?
C62 O9 V1 134.7(10) . . ?
V2 O10 Ni4 135.6(3) . . ?
V2 O11 Ni1 131.2(3) . . ?
V2 O11 Ni3 127.7(3) . 4_565 ?
Ni1 O11 Ni3 99.8(2) . 4_565 ?
V2 O12 Ni4 131.6(3) . 4_565 ?
C60 O13 V2 135.1(9) . . ?
O1 C1 C6 122.1(6) . . ?
O1 C1 C2 121.5(6) . . ?
C6 C1 C2 116.4(6) . . ?
C3 C2 C1 120.8(6) . . ?
C3 C2 S1 122.1(5) . . ?
C1 C2 S1 116.9(5) . . ?
C2 C3 C4 122.7(7) . . ?
C5 C4 C3 115.9(6) . . ?
C5 C4 C25 120.3(7) . . ?
C3 C4 C25 123.7(7) . . ?
C6 C5 C4 123.4(7) . . ?
C5 C6 C1 120.8(6) . . ?
C5 C6 S2 122.1(5) . . ?
C1 C6 S2 117.1(5) . . ?
O2 C7 C8 122.1(6) . . ?
O2 C7 C12 119.9(6) . . ?
C8 C7 C12 118.1(6) . . ?
C7 C8 C9 120.7(6) . . ?
C7 C8 S2 118.6(5) . . ?
C9 C8 S2 120.6(5) . . ?
C8 C9 C10 122.2(7) . . ?
C9 C10 C11 117.1(7) . . ?
C9 C10 C26 123.1(7) . . ?
C11 C10 C26 119.6(7) . . ?
C12 C11 C10 120.9(7) . . ?
C11 C12 C7 121.0(7) . . ?
C11 C12 S3 120.9(6) . . ?
C7 C12 S3 118.1(5) . . ?
O3 C13 C14 122.0(6) . . ?
O3 C13 C18 122.1(6) . . ?
C14 C13 C18 115.9(6) . . ?
C15 C14 C13 122.2(6) . . ?
C15 C14 S3 119.7(5) . . ?
C13 C14 S3 118.2(5) . . ?
C14 C15 C16 122.1(6) . . ?
C15 C16 C17 117.1(6) . . ?
C15 C16 C27 120.3(6) . . ?
C17 C16 C27 122.4(6) . . ?
C16 C17 C18 121.2(6) . . ?
C17 C18 C13 121.5(6) . . ?
C17 C18 S4 120.6(5) . . ?
C13 C18 S4 117.8(5) . . ?
O4 C19 C24 122.1(6) . . ?
O4 C19 C20 120.3(6) . . ?
C24 C19 C20 117.6(6) . . ?
C21 C20 C19 121.4(7) . . ?
C21 C20 S4 120.0(5) . . ?
C19 C20 S4 118.6(5) . . ?
C20 C21 C22 120.8(7) . . ?
C23 C22 C21 118.3(7) . . ?
C23 C22 C28 122.2(7) . . ?
C21 C22 C28 119.5(7) . . ?
C22 C23 C24 120.6(7) . . ?
C19 C24 C23 121.2(6) . . ?
C19 C24 S1 119.0(5) . . ?
C23 C24 S1 119.5(5) . . ?
C31 C25 C29 107.1(10) . . ?
C31 C25 C30 108.5(10) . . ?
C29 C25 C30 110.9(11) . . ?
C31 C25 C4 109.2(7) . . ?
C29 C25 C4 111.5(8) . . ?
C30 C25 C4 109.7(8) . . ?
C32 C26 C33 108.2(8) . . ?
C32 C26 C34 109.0(9) . . ?
C33 C26 C34 106.3(9) . . ?
C32 C26 C10 113.5(8) . . ?
C33 C26 C10 108.2(9) . . ?
C34 C26 C10 111.4(7) . . ?
C37 C27 C35 110.6(7) . . ?
C37 C27 C16 111.9(7) . . ?
C35 C27 C16 109.5(7) . . ?
C37 C27 C36 108.5(7) . . ?
C35 C27 C36 108.0(8) . . ?
C16 C27 C36 108.1(6) . . ?
C39 C28 C38 112.4(10) . . ?
C39 C28 C40 110.1(10) . . ?
C38 C28 C40 105.1(10) . . ?
C39 C28 C22 112.2(8) . . ?
C38 C28 C22 107.6(8) . . ?
C40 C28 C22 109.2(7) . . ?
O5 C41 C46 121.9(5) . . ?
O5 C41 C42 121.9(5) . . ?
C46 C41 C42 116.1(5) . . ?
C43 C42 C41 121.3(6) . . ?
C43 C42 S5 120.1(5) . . ?
C41 C42 S5 118.5(5) . . ?
C42 C43 C44 122.1(7) . . ?
C43 C44 C45 117.2(7) . . ?
C43 C44 C47 121.8(8) . . ?
C45 C44 C47 120.8(8) . . ?
C44 C45 C46 121.6(7) . . ?
C45 C46 C41 121.7(6) . . ?
C45 C46 S5 121.4(5) . 4_565 ?
C41 C46 S5 116.9(5) . 4_565 ?
C49 C47 C44 113.8(10) . . ?
C49 C47 C48 113.7(12) . . ?
C44 C47 C48 111.8(10) . . ?
C49 C47 C50 103.0(14) . . ?
C44 C47 C50 108.7(12) . . ?
C48 C47 C50 105.0(12) . . ?
C51 N1 C52 130.0(11) . . ?
C51 N1 C53 114.7(11) . . ?
C52 N1 C53 112.7(10) . . ?
O14 C51 N1 130.8(13) . . ?
C54 N2 C56 123.2(12) . . ?
C54 N2 C55 122.2(13) . . ?
C56 N2 C55 114.6(14) . . ?
O15 C54 N2 125.3(14) . . ?
C57 N3 C59 123.1(16) . . ?
C57 N3 C58 118.1(15) . . ?
C59 N3 C58 116.8(17) . . ?
O16 C57 N3 129.9(16) . . ?
O13 C60 C61 113.4(14) . . ?
O9 C62 C63 105.2(16) . . ?
O9 C62' C63' 117(2) . . ?
C64 O17 C64 63(3) 4_565 3_655 ?
C64 O17 C64 43.2(16) 4_565 2_665 ?
C64 O17 C64 43.2(16) 3_655 2_665 ?
C64 O17 C64 43.2(16) 4_565 . ?
C64 O17 C64 43.2(16) 3_655 . ?
C64 O17 C64 63(3) 2_665 . ?
C64 C64 C64 90.00(3) 4_565 3_655 ?
C64 C64 O17 68.4(8) 4_565 . ?
C64 C64 O17 68.4(8) 3_655 . ?
C64 C64 C64 45.00(4) 4_565 2_665 ?
C64 C64 C64 45.001(14) 3_655 2_665 ?
O17 C64 C64 58.6(13) . 2_665 ?
C64 C64 C65 70.1(8) 4_565 . ?
C64 C64 C65 70.1(8) 3_655 . ?
O17 C64 C65 120(2) . . ?
C64 C64 C65 61.2(11) 2_665 . ?
C64 C65 C64 58(2) . 2_665 ?
C64 C65 C64 39.8(15) . 3_655 ?
C64 C65 C64 39.8(15) 2_665 3_655 ?
C64 C65 C64 39.8(15) . 4_565 ?
C64 C65 C64 39.8(15) 2_665 4_565 ?
C64 C65 C64 58(2) 3_655 4_565 ?

_refine_diff_density_max         1.121
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.090

# start Validation Reply Form
_vrf_PLAT201_Ni20V8              
;
PROBLEM:  Isotropic non-H Atoms in Main Residue(s) .......2 Report.  
RESPONSE: The disordered carbethoxy were refined isotropically.
;
_vrf_PLAT220_Ni20V8              
;
PROBLEM:  NonSolvent   Resd 1  C   Ueq(max)/Ueq(min) Range       7.9 Ratio
RESPONSE:  It is due to disorder.
;
_vrf_FORMU01_Ni20V8              
;
PROBLEM:  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and the formula from the _atom_site* data.
RESPONSE:  Solvent molecues (four CH3CH2OH) determined by SQUEEZE 
and one H atom per cluster to balance the whole charge were included
in the formula directly.
;
_vrf_CELLZ01_Ni20V8              
;
PROBLEM:  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and the formula from the _atom_site* data.
RESPONSE:  Solvent molecues (four CH3CH2OH) determined by SQUEEZE 
and one H atom per cluster to balance the whole charge were included
in the formula directly.
;
# end Validation Reply Form





####################################################################### 
# 
# 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_Co20V8
_database_code_depnum_ccdc_archive 'CCDC 2434504'
loop_
_audit_author_name
_audit_author_address
'Yanfeng Bi'
;Liaoning Petrochemical University
China
;
_audit_update_record             
;
2025-05-08 deposited with the CCDC.	2025-05-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/1
_shelx_SHELXL_version_number     2019/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C216 H260 Cl5 Co20 O52 S20V8, 12(C3 H7 N O), 4(C2 H6 O)'
_chemical_formula_sum            'C260 H369 Cl5 Co20 N12 O68 S20 V8'
_chemical_formula_weight         7155.22

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'
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'
V V 0.3005 0.5294 '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      tetragonal
_space_group_IT_number           79
_space_group_name_H-M_alt        'I 4'
_space_group_name_Hall           'I 4'

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

_cell_length_a                   26.857(3)
_cell_length_b                   26.857(3)
_cell_length_c                   23.006(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     16594(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9862
_cell_measurement_theta_min      2.3981
_cell_measurement_theta_max      24.9059

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_F_000             7372
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    1.416
_shelx_estimated_absorpt_T_min   0.816
_shelx_estimated_absorpt_T_max   0.826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6612
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            77285
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.331
_diffrn_reflns_theta_max         25.029
_diffrn_reflns_theta_full        25.029
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_point_group_measured_fraction_full 0.950
_reflns_number_total             13959
_reflns_number_gt                11947
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.856
_reflns_Friedel_fraction_max     0.901
_reflns_Friedel_fraction_full    0.901

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'Bruker Instrument Service vV6.2.3'
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_molecular_graphics    'Diamond 3.2K'
_computing_publication_material  'Adobe Photoshop CS6 and POV-Ray v3.7'
_refine_special_details          
'Refined as a 2-component inversion twin.,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)+(0.0728P)²+25.1469P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.44(2)
_chemical_absolute_configuration unk
_refine_ls_number_reflns         13959
_refine_ls_number_parameters     879
_refine_ls_number_restraints     151
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0450
_refine_ls_wR_factor_ref         0.1205
_refine_ls_wR_factor_gt          0.1132
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.64568(4) 0.41478(4) 0.52320(5) 0.0170(3) Uani 1 1 d . . . . .
Co2 Co 0.68848(3) 0.48842(3) 0.62679(6) 0.0186(2) Uani 1 1 d . . . . .
Co3 Co 0.64346(4) 0.41579(4) 0.73259(5) 0.0233(3) Uani 1 1 d . . . . .
Co4 Co 0.60130(3) 0.34103(3) 0.62577(6) 0.0189(2) Uani 1 1 d . . . . .
Co01 Co 0.54618(3) 0.57372(3) 0.42552(5) 0.0167(2) Uani 1 1 d . . . . .
V1 V 0.65042(5) 0.53826(5) 0.49567(6) 0.0163(3) Uani 1 1 d . . . . .
V2 V 0.65033(6) 0.53938(5) 0.75318(6) 0.0262(4) Uani 1 1 d . . . . .
S1 S 0.71089(8) 0.37778(8) 0.45753(9) 0.0215(5) Uani 1 1 d . . . . .
S2 S 0.78074(6) 0.50293(6) 0.62803(11) 0.0225(3) Uani 1 1 d . . . . .
S3 S 0.70743(9) 0.37808(8) 0.79722(10) 0.0260(5) Uani 1 1 d . . . . .
S4 S 0.63563(6) 0.25458(5) 0.62595(11) 0.0228(3) Uani 1 1 d . . . . .
S5 S 0.57861(7) 0.62083(7) 0.33921(9) 0.0231(4) Uani 1 1 d . . . . .
Cl1 Cl 0.60370(5) 0.43899(5) 0.62163(10) 0.0204(3) Uani 1 1 d . . . . .
Cl2 Cl 0.500000 0.500000 0.48107(15) 0.0192(7) Uani 1 4 d S T P . .
O1 O 0.70607(19) 0.4426(2) 0.5626(2) 0.0197(13) Uani 1 1 d . . . . .
O2 O 0.7043(2) 0.4414(2) 0.6914(3) 0.0233(13) Uani 1 1 d . . . . .
O3 O 0.6495(2) 0.3500(2) 0.6912(2) 0.0227(13) Uani 1 1 d . . . . .
O4 O 0.6478(2) 0.34775(19) 0.5590(2) 0.0204(13) Uani 1 1 d . . . . .
O5 O 0.48280(16) 0.57689(18) 0.3824(2) 0.0201(11) Uani 1 1 d . . . . .
O6 O 0.6309(2) 0.47933(19) 0.4794(2) 0.0195(12) Uani 1 1 d . . . . .
O7 O 0.6676(2) 0.5426(2) 0.5661(3) 0.0226(13) Uani 1 1 d . . . . .
O8 O 0.60482(19) 0.58049(19) 0.4804(2) 0.0192(12) Uani 1 1 d . . . . .
O9 O 0.7027(2) 0.5518(2) 0.4524(3) 0.0331(15) Uani 1 1 d D U . . .
O10 O 0.6675(2) 0.5432(2) 0.6815(2) 0.0231(13) Uani 1 1 d . . . . .
O11 O 0.6316(3) 0.4831(3) 0.7677(3) 0.0468(19) Uani 1 1 d . . . . .
O12 O 0.6055(3) 0.5784(3) 0.7666(3) 0.050(2) Uani 1 1 d . . . . .
O13 O 0.7050(6) 0.5392(7) 0.7972(7) 0.048(4) Uani 0.55(2) 1 d . U P A 1
C54 C 0.7316(14) 0.5839(14) 0.8133(17) 0.114(9) Uiso 0.55(2) 1 d . U P A 1
H54A H 0.719721 0.607791 0.783638 0.137 Uiso 0.55(2) 1 calc R U P A 1
H54B H 0.714042 0.593700 0.849407 0.137 Uiso 0.55(2) 1 calc R U P A 1
C55 C 0.7774(14) 0.6006(16) 0.8236(18) 0.123(9) Uiso 0.55(2) 1 d . U P A 1
H55A H 0.775965 0.635977 0.833762 0.185 Uiso 0.55(2) 1 calc R U P A 1
H55B H 0.792053 0.581817 0.855865 0.185 Uiso 0.55(2) 1 calc R U P A 1
H55C H 0.797853 0.596207 0.788702 0.185 Uiso 0.55(2) 1 calc R U P A 1
O13' O 0.6965(7) 0.5672(8) 0.7954(8) 0.038(4) Uani 0.45(2) 1 d . U P A 2
C54' C 0.7510(11) 0.5619(12) 0.7913(13) 0.061(8) Uiso 0.45(2) 1 d . . P A 2
H54C H 0.755981 0.527332 0.777340 0.074 Uiso 0.45(2) 1 calc R U P A 2
H54D H 0.760469 0.583535 0.758256 0.074 Uiso 0.45(2) 1 calc R U P A 2
C55' C 0.7861(18) 0.568(2) 0.829(2) 0.128(10) Uiso 0.45(2) 1 d . U P A 2
H55D H 0.818338 0.561299 0.810603 0.192 Uiso 0.45(2) 1 calc R U P A 2
H55E H 0.785598 0.602961 0.842425 0.192 Uiso 0.45(2) 1 calc R U P A 2
H55F H 0.781043 0.545912 0.861796 0.192 Uiso 0.45(2) 1 calc R U P A 2
C1 C 0.7521(3) 0.4386(3) 0.5406(4) 0.0208(18) Uani 1 1 d . . . . .
C2 C 0.7616(3) 0.4097(3) 0.4906(4) 0.0239(19) Uani 1 1 d . . . . .
C3 C 0.8087(4) 0.4088(3) 0.4667(4) 0.031(2) Uani 1 1 d . . . . .
H3 H 0.814183 0.389408 0.432745 0.037 Uiso 1 1 calc R U . . .
C4 C 0.8486(3) 0.4353(4) 0.4903(5) 0.036(2) Uani 1 1 d . . . . .
C5 C 0.8394(3) 0.4614(3) 0.5422(4) 0.026(2) Uani 1 1 d . . . . .
H5 H 0.866294 0.477969 0.560752 0.031 Uiso 1 1 calc R U . . .
C6 C 0.7927(3) 0.4639(3) 0.5671(4) 0.0222(19) Uani 1 1 d . . . . .
C7 C 0.7499(3) 0.4392(3) 0.7140(4) 0.0231(19) Uani 1 1 d . . . . .
C8 C 0.7902(3) 0.4637(3) 0.6905(4) 0.025(2) Uani 1 1 d . . . . .
C9 C 0.8379(3) 0.4608(3) 0.7159(4) 0.030(2) Uani 1 1 d . . . . .
H9 H 0.864733 0.478622 0.698850 0.037 Uiso 1 1 calc R U . . .
C10 C 0.8464(4) 0.4330(3) 0.7645(4) 0.032(2) Uani 1 1 d . . . . .
C11 C 0.8060(3) 0.4088(3) 0.7892(4) 0.033(2) Uani 1 1 d . . . . .
H11 H 0.810678 0.390418 0.824016 0.039 Uiso 1 1 calc R U . . .
C12 C 0.7585(3) 0.4109(3) 0.7641(4) 0.027(2) Uani 1 1 d . . . . .
C13 C 0.6755(3) 0.3131(3) 0.7123(4) 0.0222(19) Uani 1 1 d . . . . .
C14 C 0.7073(3) 0.3194(3) 0.7603(4) 0.0217(19) Uani 1 1 d . . . . .
C15 C 0.7369(3) 0.2805(3) 0.7811(4) 0.026(2) Uani 1 1 d . . . . .
H15 H 0.757533 0.285927 0.814009 0.032 Uiso 1 1 calc R U . . .
C16 C 0.7366(3) 0.2339(3) 0.7547(4) 0.027(2) Uani 1 1 d . . . . .
C17 C 0.7043(3) 0.2265(3) 0.7080(4) 0.028(2) Uani 1 1 d . . . . .
H17 H 0.702060 0.194451 0.690582 0.034 Uiso 1 1 calc R U . . .
C18 C 0.6751(3) 0.2654(3) 0.6865(4) 0.0225(19) Uani 1 1 d . . . . .
C19 C 0.6787(3) 0.3119(3) 0.5408(4) 0.0167(17) Uani 1 1 d . . . . .
C20 C 0.6784(3) 0.2647(3) 0.5667(4) 0.0223(19) Uani 1 1 d . . . . .
C21 C 0.7097(3) 0.2275(3) 0.5488(4) 0.031(2) Uani 1 1 d . . . . .
H21 H 0.708795 0.196206 0.567986 0.037 Uiso 1 1 calc R U . . .
C22 C 0.7432(4) 0.2346(4) 0.5026(4) 0.036(2) Uani 1 1 d . . . . .
C23 C 0.7430(3) 0.2806(3) 0.4772(4) 0.028(2) Uani 1 1 d . . . . .
H23 H 0.765396 0.286682 0.446095 0.033 Uiso 1 1 calc R U . . .
C24 C 0.7116(3) 0.3190(3) 0.4947(4) 0.0226(19) Uani 1 1 d . . . . .
C25 C 0.8993(4) 0.4342(4) 0.4612(5) 0.045(3) Uani 1 1 d . . . . .
C26 C 0.8967(4) 0.4302(4) 0.7965(5) 0.046(3) Uani 1 1 d . . . . .
C27 C 0.7661(4) 0.1887(4) 0.7768(5) 0.041(3) Uani 1 1 d . . . . .
C28 C 0.7734(5) 0.1902(4) 0.4793(5) 0.052(3) Uani 1 1 d . . . . .
C29 C 0.8932(6) 0.4596(7) 0.4007(8) 0.107(6) Uani 1 1 d . U . . .
H29A H 0.924821 0.457883 0.379529 0.161 Uiso 1 1 calc R U . . .
H29B H 0.883733 0.494537 0.406120 0.161 Uiso 1 1 calc R U . . .
H29C H 0.867293 0.442379 0.378497 0.161 Uiso 1 1 calc R U . . .
C30 C 0.9390(5) 0.4602(7) 0.4993(8) 0.110(6) Uani 1 1 d . U . . .
H30A H 0.971453 0.458548 0.479811 0.165 Uiso 1 1 calc R U . . .
H30B H 0.941130 0.443385 0.537016 0.165 Uiso 1 1 calc R U . . .
H30C H 0.929725 0.495119 0.505171 0.165 Uiso 1 1 calc R U . . .
C31 C 0.9163(5) 0.3798(5) 0.4539(7) 0.078(4) Uani 1 1 d . U . . .
H31A H 0.889472 0.360326 0.435976 0.117 Uiso 1 1 calc R U . . .
H31B H 0.924343 0.365708 0.492031 0.117 Uiso 1 1 calc R U . . .
H31C H 0.945854 0.378639 0.428941 0.117 Uiso 1 1 calc R U . . .
C32 C 0.9366(5) 0.4574(7) 0.7622(8) 0.102(6) Uani 1 1 d . U . . .
H32A H 0.935622 0.446551 0.721583 0.152 Uiso 1 1 calc R U . . .
H32B H 0.969376 0.449873 0.778777 0.152 Uiso 1 1 calc R U . . .
H32C H 0.930605 0.493368 0.764214 0.152 Uiso 1 1 calc R U . . .
C33 C 0.8915(6) 0.4513(8) 0.8557(8) 0.114(6) Uani 1 1 d . U . . .
H33A H 0.922737 0.446751 0.877103 0.171 Uiso 1 1 calc R U . . .
H33B H 0.864499 0.434164 0.876283 0.171 Uiso 1 1 calc R U . . .
H33C H 0.883828 0.486891 0.853025 0.171 Uiso 1 1 calc R U . . .
C35 C 0.8070(4) 0.2054(4) 0.8213(5) 0.049(3) Uani 1 1 d . . . . .
H35A H 0.826790 0.176482 0.833084 0.074 Uiso 1 1 calc R U . . .
H35B H 0.791052 0.220114 0.855529 0.074 Uiso 1 1 calc R U . . .
H35C H 0.828817 0.230178 0.803020 0.074 Uiso 1 1 calc R U . . .
C34 C 0.9137(5) 0.3784(5) 0.8035(7) 0.083(5) Uani 1 1 d . . . . .
H34A H 0.911658 0.361130 0.766072 0.125 Uiso 1 1 calc R U . . .
H34B H 0.892537 0.361371 0.831954 0.125 Uiso 1 1 calc R U . . .
H34C H 0.948269 0.378244 0.817190 0.125 Uiso 1 1 calc R U . . .
C36 C 0.7292(4) 0.1538(4) 0.8107(5) 0.054(3) Uani 1 1 d . . . . .
H36A H 0.703139 0.142075 0.784197 0.081 Uiso 1 1 calc R U . . .
H36B H 0.714031 0.172273 0.842800 0.081 Uiso 1 1 calc R U . . .
H36C H 0.747532 0.125103 0.826155 0.081 Uiso 1 1 calc R U . . .
C37 C 0.7897(4) 0.1612(4) 0.7263(5) 0.059(3) Uani 1 1 d . . . . .
H37A H 0.763770 0.143933 0.704109 0.088 Uiso 1 1 calc R U . . .
H37B H 0.813651 0.136776 0.741232 0.088 Uiso 1 1 calc R U . . .
H37C H 0.806905 0.184960 0.701073 0.088 Uiso 1 1 calc R U . . .
C38 C 0.7980(5) 0.1624(5) 0.5297(5) 0.065(4) Uani 1 1 d . . . . .
H38A H 0.812676 0.131350 0.515318 0.098 Uiso 1 1 calc R U . . .
H38B H 0.772914 0.154754 0.559337 0.098 Uiso 1 1 calc R U . . .
H38C H 0.824113 0.183266 0.546743 0.098 Uiso 1 1 calc R U . . .
C39 C 0.7389(5) 0.1537(4) 0.4501(6) 0.069(4) Uani 1 1 d . . . . .
H39A H 0.719149 0.171086 0.420598 0.103 Uiso 1 1 calc R U . . .
H39B H 0.716621 0.139064 0.479187 0.103 Uiso 1 1 calc R U . . .
H39C H 0.758502 0.127352 0.431632 0.103 Uiso 1 1 calc R U . . .
C40 C 0.8116(4) 0.2051(4) 0.4377(5) 0.049(3) Uani 1 1 d . . . . .
H40A H 0.795737 0.220445 0.403747 0.074 Uiso 1 1 calc R U . . .
H40B H 0.830466 0.175693 0.425329 0.074 Uiso 1 1 calc R U . . .
H40C H 0.834167 0.229070 0.455946 0.074 Uiso 1 1 calc R U . . .
C41 C 0.4781(3) 0.6023(3) 0.3325(3) 0.0201(16) Uani 1 1 d . . . . .
C42 C 0.5192(3) 0.6249(3) 0.3056(3) 0.0272(18) Uani 1 1 d . . . . .
C43 C 0.5137(4) 0.6495(5) 0.2541(5) 0.066(4) Uani 1 1 d . . . . .
H43 H 0.542248 0.664452 0.237128 0.079 Uiso 1 1 calc R U . . .
C44 C 0.4693(4) 0.6537(6) 0.2255(6) 0.088(5) Uani 1 1 d . . . . .
C45 C 0.4286(4) 0.6321(5) 0.2536(5) 0.065(3) Uani 1 1 d . . . . .
H45 H 0.396647 0.635259 0.236250 0.078 Uiso 1 1 calc R U . . .
C46 C 0.4322(3) 0.6065(3) 0.3051(3) 0.0293(18) Uani 1 1 d . . . . .
C47 C 0.4613(6) 0.6901(8) 0.1736(8) 0.142(5) Uani 1 1 d D U . . .
C48 C 0.5100(7) 0.6913(8) 0.1397(8) 0.159(6) Uani 1 1 d D U . . .
H48A H 0.536271 0.705576 0.164061 0.238 Uiso 1 1 calc R U . . .
H48B H 0.519177 0.657385 0.128346 0.238 Uiso 1 1 calc R U . . .
H48C H 0.505743 0.711811 0.104768 0.238 Uiso 1 1 calc R U . . .
C49 C 0.4234(6) 0.6672(6) 0.1311(8) 0.120(5) Uani 1 1 d D U . . .
H49A H 0.427220 0.682659 0.092774 0.180 Uiso 1 1 calc R U . . .
H49B H 0.389565 0.673191 0.145541 0.180 Uiso 1 1 calc R U . . .
H49C H 0.429213 0.631320 0.128009 0.180 Uiso 1 1 calc R U . . .
C50 C 0.4430(9) 0.7409(8) 0.1971(9) 0.171(7) Uani 1 1 d D U . . .
H50A H 0.470073 0.765320 0.194663 0.256 Uiso 1 1 calc R U . . .
H50B H 0.432630 0.737228 0.237706 0.256 Uiso 1 1 calc R U . . .
H50C H 0.414715 0.752433 0.173782 0.256 Uiso 1 1 calc R U . . .
N1 N 0.8481(3) 0.3272(3) 0.6157(5) 0.076(3) Uani 1 1 d . U . . .
O14 O 0.9270(4) 0.3588(4) 0.6179(7) 0.123(4) Uani 1 1 d . U . . .
C51 C 0.7976(4) 0.3287(4) 0.6280(8) 0.083(3) Uani 1 1 d . U . . .
H51A H 0.792728 0.333871 0.669765 0.125 Uiso 1 1 calc R U . . .
H51B H 0.782145 0.297124 0.616417 0.125 Uiso 1 1 calc R U . . .
H51C H 0.782086 0.356093 0.606429 0.125 Uiso 1 1 calc R U . . .
C52 C 0.8587(6) 0.2948(5) 0.5636(6) 0.090(4) Uani 1 1 d . U . . .
H52A H 0.893908 0.297760 0.553033 0.134 Uiso 1 1 calc R U . . .
H52B H 0.837970 0.305622 0.530890 0.134 Uiso 1 1 calc R U . . .
H52C H 0.851052 0.260088 0.573080 0.134 Uiso 1 1 calc R U . . .
C53 C 0.8833(5) 0.3568(4) 0.6312(9) 0.088(3) Uani 1 1 d . U . . .
H53 H 0.873300 0.381788 0.658035 0.106 Uiso 1 1 calc R U . . .
C56 C 0.7517(6) 0.5610(11) 0.4625(14) 0.124(8) Uiso 0.68(2) 1 d D U P B 1
H56A H 0.770610 0.529437 0.461399 0.149 Uiso 0.68(2) 1 calc R U P B 1
H56B H 0.755750 0.575880 0.501634 0.149 Uiso 0.68(2) 1 calc R U P B 1
C57 C 0.7718(13) 0.5966(13) 0.4167(15) 0.142(9) Uiso 0.68(2) 1 d . U P B 1
H57A H 0.807146 0.603138 0.424236 0.213 Uiso 0.68(2) 1 calc R U P B 1
H57B H 0.768072 0.581666 0.378087 0.213 Uiso 0.68(2) 1 calc R U P B 1
H57C H 0.753243 0.628012 0.418236 0.213 Uiso 0.68(2) 1 calc R U P B 1
C56' C 0.7239(18) 0.555(3) 0.3973(12) 0.144(10) Uiso 0.32(2) 1 d D U P B 2
H56C H 0.712218 0.586177 0.378533 0.173 Uiso 0.32(2) 1 calc R U P B 2
H56D H 0.711936 0.526840 0.373511 0.173 Uiso 0.32(2) 1 calc R U P B 2
C57' C 0.7798(18) 0.555(3) 0.397(3) 0.138(10) Uiso 0.32(2) 1 d D U P B 2
H57D H 0.791823 0.557312 0.356959 0.206 Uiso 0.32(2) 1 calc R U P B 2
H57E H 0.792117 0.583296 0.419558 0.206 Uiso 0.32(2) 1 calc R U P B 2
H57F H 0.791835 0.523866 0.414529 0.206 Uiso 0.32(2) 1 calc R U P B 2
N2 N 0.6478(5) 0.0824(5) 0.5533(6) 0.0957(19) Uiso 1 1 d D U . . .
O15 O 0.6957(3) 0.1176(3) 0.6253(6) 0.0915(18) Uiso 1 1 d . U . . .
C58 C 0.6849(10) 0.0854(11) 0.5939(12) 0.0942(19) Uiso 0.585(11) 1 d . U P C 1
H58A H 0.705124 0.056454 0.597045 0.113 Uiso 0.585(11) 1 calc R U P C 1
C59 C 0.6337(11) 0.0372(11) 0.5254(12) 0.096(2) Uiso 0.585(11) 1 d . U P C 1
H59A H 0.606468 0.043798 0.498124 0.144 Uiso 0.585(11) 1 calc R U P C 1
H59B H 0.662251 0.023524 0.504277 0.144 Uiso 0.585(11) 1 calc R U P C 1
H59C H 0.622562 0.013118 0.554719 0.144 Uiso 0.585(11) 1 calc R U P C 1
C60 C 0.6121(10) 0.1250(10) 0.5501(13) 0.096(2) Uiso 0.585(11) 1 d . U P C 1
H60A H 0.587463 0.118519 0.519640 0.143 Uiso 0.585(11) 1 calc R U P C 1
H60B H 0.595127 0.128677 0.587597 0.143 Uiso 0.585(11) 1 calc R U P C 1
H60C H 0.630306 0.155630 0.541098 0.143 Uiso 0.585(11) 1 calc R U P C 1
C58' C 0.6529(15) 0.1155(14) 0.5991(16) 0.0946(19) Uiso 0.415(11) 1 d . U P C 2
H58B H 0.625910 0.136037 0.611027 0.114 Uiso 0.415(11) 1 calc R U P C 2
C59' C 0.6875(11) 0.0485(12) 0.5357(16) 0.096(2) Uiso 0.415(11) 1 d D U P C 2
H59D H 0.676168 0.028479 0.502599 0.143 Uiso 0.415(11) 1 calc R U P C 2
H59E H 0.716869 0.067822 0.524318 0.143 Uiso 0.415(11) 1 calc R U P C 2
H59F H 0.695979 0.026548 0.568164 0.143 Uiso 0.415(11) 1 calc R U P C 2
C60' C 0.6019(10) 0.0681(14) 0.5825(16) 0.096(2) Uiso 0.415(11) 1 d D U P C 2
H60D H 0.585286 0.041850 0.560178 0.144 Uiso 0.415(11) 1 calc R U P C 2
H60E H 0.609523 0.055867 0.621582 0.144 Uiso 0.415(11) 1 calc R U P C 2
H60F H 0.579869 0.097155 0.585287 0.144 Uiso 0.415(11) 1 calc R U P C 2
N3 N 0.9361(5) 0.5965(6) 0.6961(8) 0.120(4) Uani 1 1 d . U . . .
O16 O 0.9284(4) 0.5266(4) 0.6316(8) 0.124(3) Uani 1 1 d . U . . .
C61 C 0.9524(7) 0.5599(7) 0.6520(9) 0.119(4) Uani 1 1 d . U . . .
H61A H 0.985666 0.563147 0.638349 0.143 Uiso 1 1 calc R U . . .
C62 C 0.8842(6) 0.5945(6) 0.7137(9) 0.117(5) Uani 1 1 d . U . . .
H62A H 0.868948 0.564025 0.698499 0.176 Uiso 1 1 calc R U . . .
H62B H 0.882120 0.594575 0.756209 0.176 Uiso 1 1 calc R U . . .
H62C H 0.866610 0.623565 0.698195 0.176 Uiso 1 1 calc R U . . .
C63 C 0.9673(6) 0.6387(8) 0.7135(10) 0.129(5) Uani 1 1 d . U . . .
H63A H 1.001010 0.634079 0.698091 0.193 Uiso 1 1 calc R U . . .
H63B H 0.953128 0.669546 0.697987 0.193 Uiso 1 1 calc R U . . .
H63C H 0.968638 0.640556 0.756000 0.193 Uiso 1 1 calc R U . . .
O17 O 0.500000 0.500000 0.7014(9) 0.091(5) Uiso 1 4 d DS U P . .
H17A H 0.508754 0.520206 0.675432 0.136 Uiso 0.25 1 calc R U P . .
C64 C 0.5252(14) 0.511(3) 0.7510(9) 0.067(9) Uiso 0.25 1 d D U P . .
H64A H 0.533153 0.545393 0.750311 0.080 Uiso 0.25 1 d R U P . .
H64B H 0.556132 0.492554 0.750311 0.080 Uiso 0.25 1 d R U P . .
C65 C 0.500000 0.500000 0.8075(10) 0.071(6) Uiso 1 4 d DS U P . .
H65A H 0.520590 0.508800 0.839989 0.106 Uiso 0.25 1 d R U P . .
H65B H 0.469590 0.518740 0.808939 0.106 Uiso 0.25 1 d R U P . .
H65C H 0.492530 0.465070 0.808939 0.106 Uiso 0.25 1 d R U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O4 1.981(5) . ?
Co1 O1 2.003(5) . ?
Co1 O6 2.044(5) . ?
Co1 O8 2.077(5) 4_565 ?
Co1 S1 2.517(2) . ?
Co1 Cl1 2.612(2) . ?
Co2 O1 1.978(5) . ?
Co2 O2 1.997(6) . ?
Co2 O10 2.015(5) . ?
Co2 O7 2.092(6) . ?
Co2 S2 2.5083(17) . ?
Co2 Cl1 2.6385(17) . ?
Co3 O12 2.000(7) 4_565 ?
Co3 O11 2.005(7) . ?
Co3 O2 2.011(6) . ?
Co3 O3 2.013(6) . ?
Co3 S3 2.488(3) . ?
Co4 O4 1.987(5) . ?
Co4 O3 2.000(5) . ?
Co4 O10 2.033(6) 4_565 ?
Co4 O7 2.103(6) 4_565 ?
Co4 S4 2.4983(17) . ?
Co4 Cl1 2.6334(17) . ?
Co01 O5 1.972(5) . ?
Co01 O5 1.992(5) 4_565 ?
Co01 O8 2.026(5) . ?
Co01 O6 2.090(5) 3_655 ?
Co01 S5 2.510(2) . ?
Co01 Cl2 2.6630(19) . ?
V1 O7 1.689(6) . ?
V1 O8 1.706(5) . ?
V1 O6 1.708(5) . ?
V1 O9 1.759(6) . ?
V2 O12 1.625(7) . ?
V2 O11 1.627(7) . ?
V2 O10 1.716(6) . ?
V2 O13' 1.744(16) . ?
V2 O13 1.784(16) . ?
S1 C2 1.779(9) . ?
S1 C24 1.795(9) . ?
S2 C6 1.780(9) . ?
S2 C8 1.799(9) . ?
S3 C14 1.790(8) . ?
S3 C12 1.798(9) . ?
S4 C18 1.775(8) . ?
S4 C20 1.803(9) . ?
S5 C42 1.776(8) . ?
S5 C46 1.790(8) 4_565 ?
O1 C1 1.339(10) . ?
O2 C7 1.331(10) . ?
O3 C13 1.308(10) . ?
O4 C19 1.339(9) . ?
O5 C41 1.342(9) . ?
O9 C56 1.359(13) . ?
O9 C56' 1.394(14) . ?
O13 C54 1.44(4) . ?
C54 C55 1.33(5) . ?
O13' C54' 1.48(4) . ?
C54' C55' 1.29(5) . ?
C1 C2 1.412(12) . ?
C1 C6 1.423(12) . ?
C2 C3 1.380(13) . ?
C3 C4 1.399(13) . ?
C4 C5 1.405(14) . ?
C4 C25 1.517(13) . ?
C5 C6 1.381(12) . ?
C7 C8 1.376(12) . ?
C7 C12 1.401(12) . ?
C8 C9 1.411(12) . ?
C9 C10 1.364(13) . ?
C10 C11 1.383(14) . ?
C10 C26 1.540(13) . ?
C11 C12 1.403(12) . ?
C13 C14 1.406(11) . ?
C13 C18 1.412(12) . ?
C14 C15 1.397(12) . ?
C15 C16 1.392(13) . ?
C16 C17 1.396(12) . ?
C16 C27 1.535(13) . ?
C17 C18 1.397(12) . ?
C19 C24 1.392(12) . ?
C19 C20 1.401(12) . ?
C20 C21 1.370(12) . ?
C21 C22 1.405(13) . ?
C22 C23 1.366(13) . ?
C22 C28 1.540(13) . ?
C23 C24 1.392(12) . ?
C25 C31 1.541(17) . ?
C25 C30 1.549(18) . ?
C25 C29 1.557(19) . ?
C26 C34 1.474(17) . ?
C26 C33 1.48(2) . ?
C26 C32 1.519(18) . ?
C27 C37 1.515(15) . ?
C27 C35 1.568(14) . ?
C27 C36 1.571(16) . ?
C28 C40 1.459(15) . ?
C28 C39 1.506(17) . ?
C28 C38 1.529(15) . ?
C41 C46 1.388(10) . ?
C41 C42 1.403(10) . ?
C42 C43 1.366(12) . ?
C43 C44 1.367(14) . ?
C44 C45 1.397(15) . ?
C44 C47 1.56(2) . ?
C45 C46 1.372(12) . ?
C47 C48 1.522(13) . ?
C47 C49 1.540(13) . ?
C47 C50 1.548(13) . ?
N1 C53 1.287(15) . ?
N1 C51 1.387(14) . ?
N1 C52 1.507(16) . ?
O14 C53 1.214(16) . ?
C56 C57 1.52(4) . ?
C56' C57' 1.499(14) . ?
N2 C58 1.37(3) . ?
N2 C58' 1.39(4) . ?
N2 C59 1.42(3) . ?
N2 C60' 1.456(14) . ?
N2 C59' 1.457(14) . ?
N2 C60 1.50(3) . ?
O15 C58 1.16(3) . ?
O15 C58' 1.30(4) . ?
C58' C60' 1.91(5) . ?
C60' C61 2.03(3) 4_565 ?
N3 C62 1.45(2) . ?
N3 C63 1.46(2) . ?
N3 C61 1.48(2) . ?
O16 C61 1.200(19) . ?
O17 C64 1.359(14) 3_655 ?
O17 C64 1.359(14) 4_565 ?
O17 C64 1.359(14) 2_665 ?
O17 C64 1.359(14) . ?
C64 C64 1.04(4) 4_565 ?
C64 C64 1.04(4) 3_655 ?
C64 C64 1.47(6) 2_665 ?
C64 C65 1.491(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
O4 Co1 O1 97.3(2) . . ?
O4 Co1 O6 169.0(2) . . ?
O1 Co1 O6 93.6(2) . . ?
O4 Co1 O8 89.5(2) . 4_565 ?
O1 Co1 O8 172.8(2) . 4_565 ?
O6 Co1 O8 79.5(2) . 4_565 ?
O4 Co1 S1 82.61(17) . . ?
O1 Co1 S1 81.72(16) . . ?
O6 Co1 S1 100.00(17) . . ?
O8 Co1 S1 101.64(17) 4_565 . ?
O4 Co1 Cl1 82.97(17) . . ?
O1 Co1 Cl1 82.17(16) . . ?
O6 Co1 Cl1 97.62(16) . . ?
O8 Co1 Cl1 96.34(16) 4_565 . ?
S1 Co1 Cl1 156.77(8) . . ?
O1 Co2 O2 96.37(17) . . ?
O1 Co2 O10 170.4(2) . . ?
O2 Co2 O10 93.3(2) . . ?
O1 Co2 O7 89.9(2) . . ?
O2 Co2 O7 173.5(2) . . ?
O10 Co2 O7 80.45(17) . . ?
O1 Co2 S2 82.49(16) . . ?
O2 Co2 S2 83.07(17) . . ?
O10 Co2 S2 98.98(18) . . ?
O7 Co2 S2 99.46(16) . . ?
O1 Co2 Cl1 81.94(16) . . ?
O2 Co2 Cl1 84.21(16) . . ?
O10 Co2 Cl1 98.82(18) . . ?
O7 Co2 Cl1 95.07(16) . . ?
S2 Co2 Cl1 158.63(6) . . ?
O12 Co3 O11 87.8(3) 4_565 . ?
O12 Co3 O2 173.4(3) 4_565 . ?
O11 Co3 O2 90.6(3) . . ?
O12 Co3 O3 90.2(3) 4_565 . ?
O11 Co3 O3 173.8(3) . . ?
O2 Co3 O3 90.7(2) . . ?
O12 Co3 S3 104.7(2) 4_565 . ?
O11 Co3 S3 103.6(2) . . ?
O2 Co3 S3 81.91(17) . . ?
O3 Co3 S3 82.52(16) . . ?
O4 Co4 O3 99.48(18) . . ?
O4 Co4 O10 168.5(2) . 4_565 ?
O3 Co4 O10 92.0(2) . 4_565 ?
O4 Co4 O7 88.7(2) . 4_565 ?
O3 Co4 O7 171.7(2) . 4_565 ?
O10 Co4 O7 79.79(17) 4_565 4_565 ?
O4 Co4 S4 81.60(16) . . ?
O3 Co4 S4 82.65(17) . . ?
O10 Co4 S4 100.26(18) 4_565 . ?
O7 Co4 S4 100.11(16) 4_565 . ?
O4 Co4 Cl1 82.30(16) . . ?
O3 Co4 Cl1 83.74(16) . . ?
O10 Co4 Cl1 98.85(17) 4_565 . ?
O7 Co4 Cl1 96.02(16) 4_565 . ?
S4 Co4 Cl1 156.86(6) . . ?
O5 Co01 O5 98.0(3) . 4_565 ?
O5 Co01 O8 168.6(2) . . ?
O5 Co01 O8 93.2(2) 4_565 . ?
O5 Co01 O6 89.1(2) . 3_655 ?
O5 Co01 O6 172.5(2) 4_565 3_655 ?
O8 Co01 O6 79.6(2) . 3_655 ?
O5 Co01 S5 83.10(15) . . ?
O5 Co01 S5 81.18(14) 4_565 . ?
O8 Co01 S5 100.23(16) . . ?
O6 Co01 S5 102.26(16) 3_655 . ?
O5 Co01 Cl2 82.62(15) . . ?
O5 Co01 Cl2 82.25(14) 4_565 . ?
O8 Co01 Cl2 97.46(16) . . ?
O6 Co01 Cl2 96.28(16) 3_655 . ?
S5 Co01 Cl2 156.33(9) . . ?
O7 V1 O8 110.4(3) . . ?
O7 V1 O6 110.9(3) . . ?
O8 V1 O6 110.5(3) . . ?
O7 V1 O9 108.1(3) . . ?
O8 V1 O9 108.6(3) . . ?
O6 V1 O9 108.2(3) . . ?
O12 V2 O11 109.3(4) . . ?
O12 V2 O10 110.1(3) . . ?
O11 V2 O10 109.6(3) . . ?
O12 V2 O13' 98.3(8) . . ?
O11 V2 O13' 120.2(7) . . ?
O10 V2 O13' 108.6(6) . . ?
O12 V2 O13 120.2(7) . . ?
O11 V2 O13 97.8(7) . . ?
O10 V2 O13 108.9(6) . . ?
C2 S1 C24 102.3(4) . . ?
C2 S1 Co1 94.9(3) . . ?
C24 S1 Co1 93.9(3) . . ?
C6 S2 C8 105.0(3) . . ?
C6 S2 Co2 94.5(3) . . ?
C8 S2 Co2 93.3(3) . . ?
C14 S3 C12 103.3(4) . . ?
C14 S3 Co3 94.2(3) . . ?
C12 S3 Co3 94.2(3) . . ?
C18 S4 C20 100.9(3) . . ?
C18 S4 Co4 94.0(3) . . ?
C20 S4 Co4 95.4(3) . . ?
C42 S5 C46 103.5(4) . 4_565 ?
C42 S5 Co01 93.6(3) . . ?
C46 S5 Co01 95.2(3) 4_565 . ?
Co1 Cl1 Co4 78.06(6) . . ?
Co1 Cl1 Co2 77.97(6) . . ?
Co4 Cl1 Co2 121.48(6) . . ?
Co01 Cl2 Co01 76.68(6) 2_665 3_655 ?
Co01 Cl2 Co01 76.68(6) 2_665 4_565 ?
Co01 Cl2 Co01 122.64(14) 3_655 4_565 ?
Co01 Cl2 Co01 122.64(14) 2_665 . ?
Co01 Cl2 Co01 76.69(6) 3_655 . ?
Co01 Cl2 Co01 76.68(6) 4_565 . ?
C1 O1 Co2 123.5(5) . . ?
C1 O1 Co1 123.0(5) . . ?
Co2 O1 Co1 112.1(2) . . ?
C7 O2 Co2 120.9(5) . . ?
C7 O2 Co3 123.3(5) . . ?
Co2 O2 Co3 113.2(3) . . ?
C13 O3 Co4 122.3(5) . . ?
C13 O3 Co3 122.3(5) . . ?
Co4 O3 Co3 114.2(3) . . ?
C19 O4 Co1 122.7(5) . . ?
C19 O4 Co4 124.5(5) . . ?
Co1 O4 Co4 112.7(3) . . ?
C41 O5 Co01 122.3(4) . . ?
C41 O5 Co01 124.4(4) . 3_655 ?
Co01 O5 Co01 112.9(2) . 3_655 ?
V1 O6 Co1 128.2(3) . . ?
V1 O6 Co01 131.2(3) . 4_565 ?
Co1 O6 Co01 99.0(2) . 4_565 ?
V1 O7 Co2 131.7(3) . . ?
V1 O7 Co4 130.3(3) . 3_655 ?
Co2 O7 Co4 96.6(2) . 3_655 ?
V1 O8 Co01 128.8(3) . . ?
V1 O8 Co1 130.1(3) . 3_655 ?
Co01 O8 Co1 100.0(2) . 3_655 ?
C56 O9 V1 135.5(14) . . ?
C56' O9 V1 149(2) . . ?
V2 O10 Co2 129.2(3) . . ?
V2 O10 Co4 128.4(3) . 3_655 ?
Co2 O10 Co4 101.4(2) . 3_655 ?
V2 O11 Co3 134.9(4) . . ?
V2 O12 Co3 134.5(4) . 3_655 ?
C54 O13 V2 123(2) . . ?
C55 C54 O13 141(4) . . ?
C54' O13' V2 128.9(18) . . ?
C55' C54' O13' 132(3) . . ?
O1 C1 C2 121.3(7) . . ?
O1 C1 C6 120.5(8) . . ?
C2 C1 C6 118.2(7) . . ?
C3 C2 C1 120.0(8) . . ?
C3 C2 S1 121.5(7) . . ?
C1 C2 S1 118.4(6) . . ?
C2 C3 C4 122.7(9) . . ?
C3 C4 C5 116.7(8) . . ?
C3 C4 C25 120.4(9) . . ?
C5 C4 C25 123.0(9) . . ?
C6 C5 C4 122.5(8) . . ?
C5 C6 C1 119.7(8) . . ?
C5 C6 S2 121.3(6) . . ?
C1 C6 S2 118.7(6) . . ?
O2 C7 C8 123.3(8) . . ?
O2 C7 C12 119.7(8) . . ?
C8 C7 C12 117.0(8) . . ?
C7 C8 C9 121.6(8) . . ?
C7 C8 S2 118.8(6) . . ?
C9 C8 S2 119.4(7) . . ?
C10 C9 C8 121.4(9) . . ?
C9 C10 C11 117.5(8) . . ?
C9 C10 C26 124.3(9) . . ?
C11 C10 C26 117.9(9) . . ?
C10 C11 C12 121.7(9) . . ?
C7 C12 C11 120.6(8) . . ?
C7 C12 S3 119.3(6) . . ?
C11 C12 S3 120.0(7) . . ?
O3 C13 C14 121.6(7) . . ?
O3 C13 C18 121.9(7) . . ?
C14 C13 C18 116.5(7) . . ?
C15 C14 C13 121.5(8) . . ?
C15 C14 S3 119.7(6) . . ?
C13 C14 S3 118.7(6) . . ?
C16 C15 C14 121.4(8) . . ?
C15 C16 C17 117.9(8) . . ?
C15 C16 C27 124.3(8) . . ?
C17 C16 C27 117.6(8) . . ?
C16 C17 C18 121.0(8) . . ?
C17 C18 C13 121.7(8) . . ?
C17 C18 S4 119.4(6) . . ?
C13 C18 S4 118.9(6) . . ?
O4 C19 C24 122.2(7) . . ?
O4 C19 C20 120.9(7) . . ?
C24 C19 C20 116.9(7) . . ?
C21 C20 C19 121.9(8) . . ?
C21 C20 S4 120.6(7) . . ?
C19 C20 S4 117.5(6) . . ?
C20 C21 C22 121.4(8) . . ?
C23 C22 C21 116.3(8) . . ?
C23 C22 C28 123.7(9) . . ?
C21 C22 C28 119.7(9) . . ?
C22 C23 C24 123.3(9) . . ?
C23 C24 C19 120.1(8) . . ?
C23 C24 S1 121.4(7) . . ?
C19 C24 S1 118.5(6) . . ?
C4 C25 C31 109.5(9) . . ?
C4 C25 C30 111.0(10) . . ?
C31 C25 C30 106.5(12) . . ?
C4 C25 C29 107.0(10) . . ?
C31 C25 C29 110.4(11) . . ?
C30 C25 C29 112.4(13) . . ?
C34 C26 C33 106.8(12) . . ?
C34 C26 C32 106.9(12) . . ?
C33 C26 C32 111.1(13) . . ?
C34 C26 C10 111.7(9) . . ?
C33 C26 C10 109.8(10) . . ?
C32 C26 C10 110.4(9) . . ?
C37 C27 C16 110.3(9) . . ?
C37 C27 C35 110.3(9) . . ?
C16 C27 C35 110.6(8) . . ?
C37 C27 C36 110.6(10) . . ?
C16 C27 C36 108.2(8) . . ?
C35 C27 C36 106.8(9) . . ?
C40 C28 C39 108.5(10) . . ?
C40 C28 C38 109.2(10) . . ?
C39 C28 C38 106.6(10) . . ?
C40 C28 C22 112.7(9) . . ?
C39 C28 C22 109.5(10) . . ?
C38 C28 C22 110.0(9) . . ?
O5 C41 C46 120.9(6) . . ?
O5 C41 C42 121.5(6) . . ?
C46 C41 C42 117.6(7) . . ?
C43 C42 C41 120.4(7) . . ?
C43 C42 S5 120.3(7) . . ?
C41 C42 S5 119.3(6) . . ?
C42 C43 C44 123.5(9) . . ?
C43 C44 C45 115.2(10) . . ?
C43 C44 C47 122.6(10) . . ?
C45 C44 C47 120.6(10) . . ?
C46 C45 C44 123.5(9) . . ?
C45 C46 C41 119.7(8) . . ?
C45 C46 S5 122.1(7) . 3_655 ?
C41 C46 S5 118.2(6) . 3_655 ?
C48 C47 C49 104.5(15) . . ?
C48 C47 C50 115.7(18) . . ?
C49 C47 C50 111.3(16) . . ?
C48 C47 C44 106.8(14) . . ?
C49 C47 C44 109.0(14) . . ?
C50 C47 C44 109.3(15) . . ?
C53 N1 C51 130.2(12) . . ?
C53 N1 C52 116.0(13) . . ?
C51 N1 C52 111.3(11) . . ?
O14 C53 N1 131.9(17) . . ?
O9 C56 C57 110(2) . . ?
O9 C56' C57' 114(4) . . ?
C58 N2 C59 124(2) . . ?
C58' N2 C60' 84(2) . . ?
C58' N2 C59' 123(3) . . ?
C60' N2 C59' 126(2) . . ?
C58 N2 C60 117.1(19) . . ?
C59 N2 C60 117.3(19) . . ?
O15 C58 N2 130(3) . . ?
O15 C58' N2 118(3) . . ?
O15 C58' C60' 139(3) . . ?
N2 C58' C60' 49.4(14) . . ?
N2 C60' C58' 46.3(15) . . ?
N2 C60' C61 155(3) . 4_565 ?
C62 N3 C63 120.1(17) . . ?
C62 N3 C61 116.9(15) . . ?
C63 N3 C61 122.0(16) . . ?
O16 C61 N3 127.1(18) . . ?
O16 C61 C60' 87.6(17) . 3_655 ?
N3 C61 C60' 95.2(15) . 3_655 ?
C64 O17 C64 65(3) 3_655 4_565 ?
C64 O17 C64 45.0(17) 3_655 2_665 ?
C64 O17 C64 45.0(17) 4_565 2_665 ?
C64 O17 C64 45.0(17) 3_655 . ?
C64 O17 C64 45.0(17) 4_565 . ?
C64 O17 C64 65(3) 2_665 . ?
C64 C64 C64 90.00(3) 4_565 3_655 ?
C64 C64 O17 67.5(8) 4_565 . ?
C64 C64 O17 67.5(8) 3_655 . ?
C64 C64 C64 44.999(11) 4_565 2_665 ?
C64 C64 C64 45.00(2) 3_655 2_665 ?
O17 C64 C64 57.3(13) . 2_665 ?
C64 C64 C65 69.6(8) 4_565 . ?
C64 C64 C65 69.6(8) 3_655 . ?
O17 C64 C65 118(2) . . ?
C64 C64 C65 60.5(12) 2_665 . ?
C64 C65 C64 59(2) . 2_665 ?
C64 C65 C64 40.8(15) . 4_565 ?
C64 C65 C64 40.8(15) 2_665 4_565 ?
C64 C65 C64 40.8(15) . 3_655 ?
C64 C65 C64 40.8(15) 2_665 3_655 ?
C64 C65 C64 59(2) 4_565 3_655 ?

_refine_diff_density_max         0.844
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.097


# start Validation Reply Form
_vrf_PLAT201_Co20V8              
;
PROBLEM:  Isotropic non-H Atoms in Main Residue(s) .......4 Report.  
RESPONSE: The disordered carbethoxy were refined isotropically.
;
_vrf_PLAT220_Co20V8              
;
PROBLEM:  NonSolvent   Resd 1  C   Ueq(max)/Ueq(min) Range        10.0 Ratio
RESPONSE:  It is due to disorder.
;
_vrf_PLAT242_Co20V8              
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of         O9 Check. 
RESPONSE:   It is due to disorder.
;
_vrf_PLAT341_Co20V8              
;
PROBLEM:  Low Bond Precision on  C-C Bonds ...............  0.01504 Ang. 
RESPONSE:   It is due to the weak high-angle diffraction of the crystal and 
disorder of the t-Bu groups.
;
_vrf_FORMU01_Co20V8              
;
PROBLEM:  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and the formula from the _atom_site* data.
RESPONSE:  Solvent molecues (three CH3CH2OH) determined by SQUEEZE 
and one H atom per cluster to balance the whole charge were included
in the formula directly.
;
_vrf_CELLZ01_Co20V8              
;
PROBLEM:  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and the formula from the _atom_site* data.
RESPONSE:  Solvent molecues (three CH3CH2OH) determined by SQUEEZE 
and one H atom per cluster to balance the whole charge were included
in the formula directly.
;
# end Validation Reply Form





