# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_160602shiga_0m_a_4
_database_code_depnum_ccdc_archive 'CCDC 2036134'
loop_
_audit_author_name
_audit_author_address
'Hajime Kamebuchi'
;Nihon University
Japan
;
_audit_update_record             
;
2021-03-16 deposited with the CCDC.	2021-03-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H70 Cu4 N24 O4 S3, 8(C2 H6 O S), 4(Cl O4)'
_chemical_formula_sum            'C62 H118 Cl4 Cu4 N24 O28 S11'
_chemical_formula_weight         2396.42

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   17.5963(8)
_cell_length_b                   17.8058(8)
_cell_length_c                   18.9440(8)
_cell_angle_alpha                77.9020(10)
_cell_angle_beta                 67.6080(10)
_cell_angle_gamma                67.1220(10)
_cell_volume                     5043.0(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    8929
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      27.70

_exptl_crystal_description       plate
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_F_000             2484
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    1.247
_shelx_estimated_absorpt_T_min   0.789
_shelx_estimated_absorpt_T_max   0.940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6478
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   
'SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction. Reference: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23993
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_av_R_equivalents  0.0184
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.332
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_full        25.027
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 0.982
_reflns_number_total             17484
_reflns_number_gt                13956
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0974P)²+28.7001P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         17484
_refine_ls_number_parameters     1330
_refine_ls_number_restraints     143
_refine_ls_R_factor_all          0.0883
_refine_ls_R_factor_gt           0.0729
_refine_ls_wR_factor_ref         0.2023
_refine_ls_wR_factor_gt          0.1888
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.129
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

# start Validation Reply Form
_vrf_PLAT220_160602shiga_0m_a_4  
;
PROBLEM: NonSolvent   Resd 1  C   Ueq(max)/Ueq(min) Range        8.5 Ratio 
RESPONSE: This alert is generated because there are many disordered DMSO 
molecules in the structure.
;
_vrf_PLAT241_160602shiga_0m_a_4  
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of        C40 Check 
RESPONSE: This alert is generated because there are many disordered DMSO 
molecules in the structure.
;
_vrf_PLAT971_160602shiga_0m_a_4  
;
PROBLEM: Check Calcd Resid. Dens.  0.37A   From S23A            2.62 eA-3  
RESPONSE: This alert is due to the disordering of the 
S(23A) DMSO molecule.
;
_vrf_PLAT972_160602shiga_0m_a_4  
;
PROBLEM: Check Calcd Resid. Dens.  0.46A   From S23A           -2.52 eA-3  
RESPONSE: This alert is due to the disordering of the 
S(23A) DMSO molecule.
;
# end Validation Reply Form

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.54859(4) 0.55981(4) 0.67603(3) 0.01959(16) Uani 1 1 d . . . . .
Cu2 Cu 0.43854(4) 0.74451(4) 0.39353(3) 0.01858(16) Uani 1 1 d . . . . .
Cu3 Cu 0.69503(4) 0.44423(4) 0.20347(3) 0.01874(16) Uani 1 1 d . . . . .
Cu4 Cu 0.79268(4) 0.25574(4) 0.49093(3) 0.01853(16) Uani 1 1 d . . . . .
N1 N 0.4619(3) 0.6571(3) 0.7317(3) 0.0253(10) Uani 1 1 d . . . . .
N2 N 0.3642(3) 0.7793(3) 0.7310(2) 0.0315(12) Uani 1 1 d . . . . .
H2 H 0.329182 0.822200 0.712349 0.038 Uiso 1 1 calc DR U . . .
N3 N 0.4969(3) 0.6216(3) 0.5940(2) 0.0201(9) Uani 1 1 d . . . . .
N4 N 0.4612(3) 0.6890(3) 0.4910(2) 0.0189(9) Uani 1 1 d . . . . .
N5 N 0.3524(3) 0.8320(3) 0.4644(3) 0.0241(10) Uani 1 1 d . . . . .
N6 N 0.3254(3) 0.8877(3) 0.5686(2) 0.0314(11) Uani 1 1 d . . . . .
H6 H 0.326237 0.888956 0.614439 0.038 Uiso 1 1 calc DR U . . .
N7 N 0.4042(3) 0.7934(3) 0.3004(3) 0.0213(9) Uani 1 1 d . . . . .
N8 N 0.4320(4) 0.7884(2) 0.1785(3) 0.0385(13) Uani 1 1 d . . . . .
H8 H 0.458728 0.767176 0.133710 0.046 Uiso 1 1 calc DR U . . .
N9 N 0.5166(3) 0.6520(3) 0.3256(2) 0.0196(9) Uani 1 1 d . . . . .
N10 N 0.6040(3) 0.5429(3) 0.2592(2) 0.0200(9) Uani 1 1 d . . . . .
N11 N 0.6454(3) 0.5054(3) 0.1198(2) 0.0231(10) Uani 1 1 d . . . . .
N12 N 0.5548(3) 0.6146(2) 0.0802(3) 0.0339(12) Uani 1 1 d . . . . .
H12 H 0.512586 0.662460 0.084064 0.041 Uiso 1 1 calc DR U . . .
N13 N 0.7724(3) 0.3413(3) 0.1520(3) 0.0244(10) Uani 1 1 d . . . . .
N14 N 0.8772(3) 0.2213(3) 0.1551(3) 0.0302(11) Uani 1 1 d . . . . .
H14A H 0.913881 0.180949 0.174400 0.036 Uiso 1 1 calc R U . . .
N15 N 0.7271(3) 0.3732(3) 0.2930(2) 0.0194(9) Uani 1 1 d . . . . .
N16 N 0.7576(3) 0.3044(3) 0.3977(2) 0.0197(9) Uani 1 1 d . . . . .
N17 N 0.8675(3) 0.1617(3) 0.4248(3) 0.0239(10) Uani 1 1 d . . . . .
N18 N 0.9006(3) 0.1101(3) 0.3144(3) 0.0257(10) Uani 1 1 d . . . . .
H18 H 0.900500 0.110056 0.268020 0.031 Uiso 1 1 calc R U . . .
N19 N 0.8199(3) 0.2033(3) 0.5855(2) 0.0217(10) Uani 1 1 d . . . . .
N20 N 0.8073(3) 0.2207(3) 0.7039(3) 0.0343(12) Uani 1 1 d . . . . .
H20 H 0.783810 0.243801 0.747536 0.041 Uiso 1 1 calc R U . . .
N21 N 0.7070(3) 0.3439(3) 0.5617(2) 0.0198(9) Uani 1 1 d . . . . .
N22 N 0.6199(3) 0.4532(3) 0.6286(2) 0.0202(9) Uani 1 1 d . . . . .
N23 N 0.5889(3) 0.4956(3) 0.7627(2) 0.0223(10) Uani 1 1 d . . . . .
N24 N 0.6618(4) 0.3753(3) 0.8093(3) 0.0386(14) Uani 1 1 d . . . . .
H24 H 0.685600 0.321666 0.813019 0.046 Uiso 1 1 calc R U . . .
C1 C 0.4339(4) 0.6849(3) 0.8082(3) 0.0301(13) Uani 1 1 d . . . . .
H1A H 0.484318 0.685393 0.819370 0.036 Uiso 1 1 calc R U . . .
H1B H 0.405935 0.648966 0.848051 0.036 Uiso 1 1 calc R U . . .
C2 C 0.3677(4) 0.7722(4) 0.8051(3) 0.0318(14) Uani 1 1 d . . . . .
H2A H 0.309945 0.777467 0.844673 0.038 Uiso 1 1 calc R U . . .
H2B H 0.389179 0.813514 0.811200 0.038 Uiso 1 1 calc R U . . .
C3 C 0.4194(3) 0.7141(3) 0.6921(3) 0.0190(11) Uani 1 1 d . . . . .
C4 C 0.4394(3) 0.6982(3) 0.6133(3) 0.0178(10) Uani 1 1 d . . . . .
C5 C 0.5073(4) 0.6193(3) 0.5202(3) 0.0225(11) Uani 1 1 d . . . . .
H5 H 0.543844 0.572674 0.491777 0.027 Uiso 1 1 calc R U . . .
C6 C 0.4178(3) 0.7402(3) 0.5500(3) 0.0182(10) Uani 1 1 d . . . . .
C7 C 0.3638(3) 0.8209(3) 0.5296(3) 0.0191(11) Uani 1 1 d . . . . .
C8 C 0.2830(4) 0.9565(4) 0.5268(4) 0.0362(15) Uani 1 1 d . . . . .
H8A H 0.307953 1.000436 0.516185 0.043 Uiso 1 1 calc R U . . .
H8B H 0.219280 0.978432 0.554258 0.043 Uiso 1 1 calc R U . . .
C9 C 0.3027(4) 0.9192(3) 0.4527(4) 0.0328(14) Uani 1 1 d . . . . .
H9A H 0.247902 0.925958 0.444769 0.039 Uiso 1 1 calc R U . . .
H9B H 0.337860 0.945344 0.407756 0.039 Uiso 1 1 calc R U . . .
C10 C 0.3525(4) 0.8748(3) 0.2742(3) 0.0266(12) Uani 1 1 d . . . . .
H10A H 0.372779 0.917764 0.278612 0.032 Uiso 1 1 calc R U . . .
H10B H 0.289577 0.888426 0.304593 0.032 Uiso 1 1 calc R U . . .
C11 C 0.3689(5) 0.8665(4) 0.1897(4) 0.0429(17) Uani 1 1 d . . . . .
H11A H 0.315110 0.869739 0.181995 0.051 Uiso 1 1 calc R U . . .
H11B H 0.391535 0.908787 0.155353 0.051 Uiso 1 1 calc R U . . .
C12 C 0.4475(3) 0.7493(3) 0.2423(3) 0.0184(10) Uani 1 1 d . . . . .
C13 C 0.5076(3) 0.6681(3) 0.2545(3) 0.0181(10) Uani 1 1 d . . . . .
C14 C 0.5753(3) 0.5767(3) 0.3250(3) 0.0226(11) Uani 1 1 d . . . . .
H14 H 0.594637 0.549999 0.367164 0.027 Uiso 1 1 calc R U . . .
C15 C 0.5614(3) 0.6004(3) 0.2137(3) 0.0183(10) Uani 1 1 d . . . . .
C16 C 0.5851(3) 0.5759(3) 0.1372(3) 0.0205(11) Uani 1 1 d . . . . .
C17 C 0.5961(4) 0.5724(4) 0.0136(3) 0.0351(14) Uani 1 1 d . . . . .
H17A H 0.624873 0.604448 -0.030392 0.042 Uiso 1 1 calc R U . . .
H17B H 0.554532 0.557718 0.000444 0.042 Uiso 1 1 calc R U . . .
C18 C 0.6636(4) 0.4960(3) 0.0386(3) 0.0274(12) Uani 1 1 d . . . . .
H18A H 0.656074 0.445441 0.033227 0.033 Uiso 1 1 calc R U . . .
H18B H 0.724017 0.493929 0.007372 0.033 Uiso 1 1 calc R U . . .
C19 C 0.8179(4) 0.3208(4) 0.0714(3) 0.0319(14) Uani 1 1 d . . . . .
H19A H 0.852157 0.356808 0.042235 0.038 Uiso 1 1 calc R U . . .
H19B H 0.775636 0.325881 0.046511 0.038 Uiso 1 1 calc R U . . .
C20 C 0.8785(4) 0.2312(4) 0.0767(3) 0.0323(14) Uani 1 1 d . . . . .
H20A H 0.855041 0.193026 0.067759 0.039 Uiso 1 1 calc R U . . .
H20B H 0.938266 0.222986 0.039818 0.039 Uiso 1 1 calc R U . . .
C21 C 0.8117(3) 0.2828(3) 0.1931(3) 0.0187(10) Uani 1 1 d . . . . .
C22 C 0.7835(3) 0.2956(3) 0.2743(3) 0.0192(11) Uani 1 1 d . . . . .
C23 C 0.7143(3) 0.3757(3) 0.3668(3) 0.0199(11) Uani 1 1 d . . . . .
H23 H 0.678346 0.422946 0.394591 0.024 Uiso 1 1 calc R U . . .
C24 C 0.8009(3) 0.2531(3) 0.3389(3) 0.0169(10) Uani 1 1 d . . . . .
C25 C 0.8561(3) 0.1728(3) 0.3594(3) 0.0186(10) Uani 1 1 d . . . . .
C26 C 0.9499(4) 0.0412(3) 0.3561(3) 0.0297(13) Uani 1 1 d . . . . .
H26A H 1.013347 0.023285 0.327078 0.036 Uiso 1 1 calc R U . . .
H26B H 0.929300 -0.005716 0.366723 0.036 Uiso 1 1 calc R U . . .
C27 C 0.9296(4) 0.0779(3) 0.4306(3) 0.0318(14) Uani 1 1 d . . . . .
H27A H 0.902791 0.045786 0.475853 0.038 Uiso 1 1 calc R U . . .
H27B H 0.983459 0.079167 0.434811 0.038 Uiso 1 1 calc R U . . .
C28 C 0.8881(4) 0.1297(3) 0.6058(3) 0.0261(12) Uani 1 1 d . . . . .
H28A H 0.946814 0.124839 0.568084 0.031 Uiso 1 1 calc R U . . .
H28B H 0.875828 0.079403 0.607834 0.031 Uiso 1 1 calc R U . . .
C29 C 0.8823(4) 0.1442(4) 0.6853(4) 0.0345(15) Uani 1 1 d . . . . .
H29A H 0.871429 0.098665 0.723180 0.041 Uiso 1 1 calc R U . . .
H29B H 0.936520 0.150444 0.683397 0.041 Uiso 1 1 calc R U . . .
C30 C 0.7813(3) 0.2489(3) 0.6427(3) 0.0183(10) Uani 1 1 d . . . . .
C31 C 0.7158(3) 0.3276(3) 0.6332(3) 0.0180(10) Uani 1 1 d . . . . .
C32 C 0.6495(3) 0.4198(3) 0.5622(3) 0.0218(11) Uani 1 1 d . . . . .
H32 H 0.631521 0.447265 0.519541 0.026 Uiso 1 1 calc R U . . .
C33 C 0.6615(3) 0.3946(3) 0.6747(3) 0.0182(10) Uani 1 1 d . . . . .
C34 C 0.6390(3) 0.4205(3) 0.7503(3) 0.0196(11) Uani 1 1 d . . . . .
C35 C 0.6404(4) 0.4306(4) 0.8671(3) 0.0339(14) Uani 1 1 d . . . . .
H35A H 0.693030 0.439507 0.865837 0.041 Uiso 1 1 calc R U . . .
H35B H 0.611849 0.409706 0.919216 0.041 Uiso 1 1 calc R U . . .
C36 C 0.5767(4) 0.5093(3) 0.8409(3) 0.0246(12) Uani 1 1 d . . . . .
H36A H 0.515559 0.517457 0.874690 0.030 Uiso 1 1 calc R U . . .
H36B H 0.591243 0.557681 0.840914 0.030 Uiso 1 1 calc R U . . .
S1 S 0.70677(12) 0.60485(11) 0.68503(10) 0.0417(4) Uani 1 1 d . . . . .
O1 O 0.6620(3) 0.6122(3) 0.6296(3) 0.0456(12) Uani 1 1 d . . . . .
C37 C 0.7461(8) 0.6874(6) 0.6591(7) 0.082(3) Uani 1 1 d . . . . .
H37A H 0.781938 0.686697 0.604845 0.124 Uiso 1 1 calc R U . . .
H37B H 0.781577 0.682463 0.690189 0.124 Uiso 1 1 calc R U . . .
H37C H 0.696544 0.738905 0.667910 0.124 Uiso 1 1 calc R U . . .
C38 C 0.8082(6) 0.5270(6) 0.6569(6) 0.071(3) Uani 1 1 d . . . . .
H38A H 0.799538 0.474062 0.667229 0.107 Uiso 1 1 calc R U . . .
H38B H 0.843974 0.527441 0.685642 0.107 Uiso 1 1 calc R U . . .
H38C H 0.837985 0.535698 0.601998 0.107 Uiso 1 1 calc R U . . .
O2 O 0.5366(4) 0.8086(3) 0.3658(3) 0.0601(15) Uani 1 1 d D . . . .
C39 C 0.5947(7) 0.8678(7) 0.2166(3) 0.090(4) Uani 1 1 d D . . . .
H39A H 0.554867 0.854597 0.200480 0.136 Uiso 1 1 calc R U . A 1
H39B H 0.650375 0.860416 0.174490 0.136 Uiso 1 1 calc R U . A 1
H39C H 0.568571 0.924652 0.230151 0.136 Uiso 1 1 calc R U . A 1
C40 C 0.6684(5) 0.8560(8) 0.3165(8) 0.111(4) Uani 1 1 d D U . . .
H40A H 0.629611 0.912437 0.326430 0.167 Uiso 1 1 calc R U . B 1
H40B H 0.720948 0.855885 0.272568 0.167 Uiso 1 1 calc R U . B 1
H40C H 0.685147 0.828977 0.361669 0.167 Uiso 1 1 calc R U . B 1
S2A S 0.61328(16) 0.80282(16) 0.29617(15) 0.0414(8) Uani 0.676(6) 1 d . . P C 1
S2B S 0.5587(4) 0.8795(3) 0.3172(3) 0.062(2) Uani 0.324(6) 1 d D U P C 2
O3 O 0.8065(2) 0.4965(3) 0.1637(3) 0.0506(13) Uani 1 1 d D . . . .
C41 C 0.9756(6) 0.3764(5) 0.1321(7) 0.100(4) Uani 1 1 d D U . . .
H41A H 0.958690 0.329596 0.161116 0.151 Uiso 1 1 calc R U . D 1
H41B H 1.032151 0.371099 0.134465 0.151 Uiso 1 1 calc R U . D 1
H41C H 0.980404 0.377708 0.078611 0.151 Uiso 1 1 calc R U . D 1
C42 C 0.9453(5) 0.5416(4) 0.1142(6) 0.077(3) Uani 1 1 d D . . . .
H42A H 0.921598 0.565725 0.072223 0.115 Uiso 1 1 calc R U . E 1
H42B H 1.008596 0.513711 0.093035 0.115 Uiso 1 1 calc R U . E 1
H42C H 0.933563 0.584818 0.145466 0.115 Uiso 1 1 calc R U . E 1
S3A S 0.8943(3) 0.4692(3) 0.1725(3) 0.0449(19) Uani 0.350(7) 1 d D U P F 1
S3B S 0.89726(17) 0.47263(17) 0.11118(18) 0.0441(11) Uani 0.650(7) 1 d . . P F
2
O4 O 0.8994(4) 0.3181(3) 0.4539(3) 0.0545(14) Uani 1 1 d . . . . .
C43 C 0.9216(9) 0.3606(9) 0.3866(7) 0.106(4) Uani 1 1 d . U . . .
H43A H 0.870726 0.408903 0.381722 0.127 Uiso 1 1 calc R U . . .
H43B H 0.942299 0.326139 0.343747 0.127 Uiso 1 1 calc R U . . .
C44 C 0.9933(10) 0.3869(12) 0.3857(8) 0.143(7) Uani 1 1 d . . . . .
H44A H 1.050792 0.342700 0.370164 0.171 Uiso 1 1 calc R U . . .
H44B H 0.996145 0.436236 0.350636 0.171 Uiso 1 1 calc R U . . .
C45 C 0.9678(7) 0.4039(8) 0.4637(7) 0.091(3) Uani 1 1 d . . . . .
H45A H 0.933676 0.462581 0.470820 0.109 Uiso 1 1 calc R U . . .
H45B H 1.019786 0.388982 0.479396 0.109 Uiso 1 1 calc R U . . .
C46 C 0.9143(9) 0.3535(9) 0.5078(7) 0.106(4) Uani 1 1 d . U . . .
H46A H 0.944909 0.309731 0.539416 0.127 Uiso 1 1 calc R U . . .
H46B H 0.857887 0.387338 0.542186 0.127 Uiso 1 1 calc R U . . .
O21 O 0.5583(5) 0.9608(5) 0.8057(4) 0.105(3) Uani 1 1 d D . . . .
C47 C 0.4474(8) 0.9548(8) 0.9516(5) 0.103(4) Uani 1 1 d D . . . .
H47A H 0.442710 1.003800 0.971065 0.155 Uiso 1 1 calc R U . G 1
H47B H 0.440449 0.912727 0.993794 0.155 Uiso 1 1 calc R U . G 1
H47C H 0.401514 0.968445 0.929020 0.155 Uiso 1 1 calc R U . G 1
C48 C 0.5510(7) 0.8157(5) 0.8754(6) 0.085(3) Uani 1 1 d D . . . .
H48A H 0.508868 0.821641 0.850784 0.128 Uiso 1 1 calc R U . H 1
H48B H 0.533469 0.790484 0.927485 0.128 Uiso 1 1 calc R U . H 1
H48C H 0.609245 0.780967 0.845858 0.128 Uiso 1 1 calc R U . H 1
S22 S 0.81473(13) 0.90247(12) 0.76017(13) 0.0540(5) Uani 1 1 d . . . . .
O22 O 0.8329(4) 0.9742(3) 0.7129(4) 0.078(2) Uani 1 1 d . . . . .
C49 C 0.7755(8) 0.8602(7) 0.7119(7) 0.088(3) Uani 1 1 d . . . . .
H49A H 0.718294 0.898114 0.709922 0.133 Uiso 1 1 calc R U . . .
H49B H 0.769569 0.808379 0.739084 0.133 Uiso 1 1 calc R U . . .
H49C H 0.816560 0.850252 0.659753 0.133 Uiso 1 1 calc R U . . .
C50 C 0.9178(7) 0.8247(6) 0.7509(8) 0.100(4) Uani 1 1 d . . . . .
H50A H 0.948580 0.812753 0.696999 0.149 Uiso 1 1 calc R U . . .
H50B H 0.909132 0.775221 0.781598 0.149 Uiso 1 1 calc R U . . .
H50C H 0.952506 0.843197 0.768845 0.149 Uiso 1 1 calc R U . . .
S21A S 0.5538(2) 0.9166(2) 0.87923(19) 0.0705(12) Uani 0.759(8) 1 d . . P I 1
S21B S 0.4926(5) 0.9216(5) 0.8562(5) 0.081(4) Uani 0.241(8) 1 d D . P I 2
O23 O 0.9938(2) -0.0490(3) 0.8426(2) 0.0681(17) Uani 1 1 d D . . . .
C51 C 0.9190(4) 0.0737(3) 0.9357(4) 0.148(6) Uani 1 1 d D U . . .
H51A H 0.914033 0.039956 0.984124 0.222 Uiso 1 1 calc R U . J 1
H51B H 0.870947 0.126264 0.943880 0.222 Uiso 1 1 calc R U . J 1
H51C H 0.974989 0.083088 0.916559 0.222 Uiso 1 1 calc R U . J 1
C52 C 0.8245(2) -0.0100(4) 0.9267(4) 0.067(2) Uani 1 1 d D . . . .
H52A H 0.782351 0.003863 0.899971 0.101 Uiso 1 1 calc R U . K 1
H52B H 0.796000 0.017359 0.974616 0.101 Uiso 1 1 calc R U . K 1
H52C H 0.846078 -0.069266 0.938065 0.101 Uiso 1 1 calc R U . K 1
S23A S 0.9136(2) 0.0229(2) 0.8678(2) 0.0503(15) Uani 0.456(6) 1 d D . P L 1
S23B S 0.93380(18) -0.02624(19) 0.91955(17) 0.0444(12) Uani 0.544(6) 1 d D . P
L 2
O24 O 0.42039(19) 0.2075(3) 0.9479(3) 0.086(2) Uani 1 1 d D . . . .
C53 C 0.2691(5) 0.3146(5) 0.9262(5) 0.061(2) Uani 1 1 d . . . . .
H53A H 0.292875 0.357158 0.895901 0.092 Uiso 1 1 calc R U . M 1
H53B H 0.207361 0.339871 0.955887 0.092 Uiso 1 1 calc R U . M 1
H53C H 0.274451 0.277194 0.891896 0.092 Uiso 1 1 calc R U . M 1
C54 C 0.2612(6) 0.2013(5) 1.0420(4) 0.057(2) Uani 1 1 d . . . . .
H54A H 0.254030 0.173739 1.006521 0.085 Uiso 1 1 calc R U . N 1
H54B H 0.203945 0.237666 1.071328 0.085 Uiso 1 1 calc R U . N 1
H54C H 0.287666 0.160376 1.077211 0.085 Uiso 1 1 calc R U . N 1
S24A S 0.32915(18) 0.25855(19) 0.99029(17) 0.0373(10) Uani 0.554(6) 1 d D . P O
1
S24B S 0.3339(3) 0.2120(3) 0.9482(3) 0.0477(14) Uani 0.446(6) 1 d D . P O 2
S25 S 0.07271(12) 0.71098(11) 0.21681(12) 0.0472(4) Uani 1 1 d . . . . .
O25 O 0.1460(3) 0.6699(3) 0.2503(3) 0.0488(12) Uani 1 1 d . . . . .
C55 C 0.1101(5) 0.6663(6) 0.1299(5) 0.059(2) Uani 1 1 d . . . . .
H55A H 0.155702 0.686329 0.092218 0.088 Uiso 1 1 calc R U . . .
H55B H 0.061244 0.680899 0.110779 0.088 Uiso 1 1 calc R U . . .
H55C H 0.134116 0.606719 0.138178 0.088 Uiso 1 1 calc R U . . .
C56 C -0.0073(6) 0.6644(7) 0.2697(6) 0.078(3) Uani 1 1 d . . . . .
H56A H 0.020087 0.604897 0.268861 0.116 Uiso 1 1 calc R U . . .
H56B H -0.053537 0.683140 0.246713 0.116 Uiso 1 1 calc R U . . .
H56C H -0.032702 0.679595 0.322777 0.116 Uiso 1 1 calc R U . . .
S26A S 0.8331(2) 0.02123(16) 0.18959(19) 0.0278(11) Uani 0.535(8) 1 d D . P P 1
C57A C 0.7414(4) 0.0109(6) 0.1764(6) 0.040(3) Uani 0.535(8) 1 d D U P P 1
H57A H 0.721299 0.054510 0.139618 0.060 Uiso 0.535(8) 1 calc R U P P 1
H57B H 0.693795 0.014949 0.225477 0.060 Uiso 0.535(8) 1 calc R U P P 1
H57C H 0.759427 -0.042328 0.156826 0.060 Uiso 0.535(8) 1 calc R U P P 1
C58A C 0.8618(8) -0.0761(2) 0.2428(5) 0.072(6) Uani 0.535(8) 1 d D U P P 1
H58A H 0.869817 -0.119476 0.213392 0.108 Uiso 0.535(8) 1 calc R U P P 1
H58B H 0.814854 -0.075599 0.291894 0.108 Uiso 0.535(8) 1 calc R U P P 1
H58C H 0.916246 -0.086204 0.251875 0.108 Uiso 0.535(8) 1 calc R U P P 1
S26B S 0.7891(3) 0.0083(2) 0.2287(3) 0.0409(14) Uani 0.465(8) 1 d D . P P 2
C57B C 0.8341(11) 0.0072(6) 0.1260(3) 0.096(8) Uiso 0.465(8) 1 d D . P P 2
H57D H 0.789279 0.043215 0.103627 0.143 Uiso 0.465(8) 1 calc R U P P 2
H57E H 0.853325 -0.048673 0.111470 0.143 Uiso 0.465(8) 1 calc R U P P 2
H57F H 0.884103 0.026274 0.107006 0.143 Uiso 0.465(8) 1 calc R U P P 2
C58B C 0.8802(7) -0.0747(3) 0.2470(8) 0.035(4) Uiso 0.465(8) 1 d D . P P 2
H58D H 0.888989 -0.123576 0.224716 0.052 Uiso 0.465(8) 1 calc R U P P 2
H58E H 0.868031 -0.085881 0.302413 0.052 Uiso 0.465(8) 1 calc R U P P 2
H58F H 0.933021 -0.059765 0.223979 0.052 Uiso 0.465(8) 1 calc R U P P 2
O26 O 0.7939(3) 0.0847(2) 0.2471(3) 0.0677(17) Uani 1 1 d D U . . .
C59 C 0.4219(4) 0.1539(5) 0.4688(4) 0.158(8) Uani 1 1 d D . . . .
H59A H 0.458143 0.188293 0.455068 0.237 Uiso 1 1 calc R U . Q 1
H59B H 0.403882 0.140629 0.524287 0.237 Uiso 1 1 calc R U . Q 1
H59C H 0.369879 0.183371 0.453572 0.237 Uiso 1 1 calc R U . Q 1
C60 C 0.4168(4) 0.0771(6) 0.3640(5) 0.175(9) Uani 1 1 d D . . . .
H60A H 0.414950 0.127985 0.331397 0.263 Uiso 1 1 calc R U . R 1
H60B H 0.357365 0.080713 0.397619 0.263 Uiso 1 1 calc R U . R 1
H60C H 0.441380 0.031186 0.331790 0.263 Uiso 1 1 calc R U . R 1
S27A S 0.4834(3) 0.0616(3) 0.4206(3) 0.077(2) Uani 0.468(8) 1 d D . P S 1
S27B S 0.4820(2) 0.1287(3) 0.3717(3) 0.083(2) Uani 0.532(8) 1 d D . P S 2
O27 O 0.5697(2) 0.0674(4) 0.3690(3) 0.086(2) Uani 1 1 d D . . . .
S28A S 0.2355(4) 0.4158(3) 0.6004(6) 0.144(3) Uani 0.676(10) 1 d D U P T 1
C61A C 0.2418(17) 0.3676(15) 0.6926(8) 0.176(11) Uani 0.676(10) 1 d D U P T 1
H61A H 0.297752 0.322628 0.685777 0.264 Uiso 0.676(10) 1 calc R U P T 1
H61B H 0.193682 0.346094 0.718511 0.264 Uiso 0.676(10) 1 calc R U P T 1
H61C H 0.237373 0.407730 0.723576 0.264 Uiso 0.676(10) 1 calc R U P T 1
C62A C 0.3020(11) 0.3246(7) 0.5501(9) 0.122(9) Uani 0.676(10) 1 d D . P T 1
H62A H 0.315637 0.338606 0.494875 0.183 Uiso 0.676(10) 1 calc R U P T 1
H62B H 0.270094 0.286058 0.565876 0.183 Uiso 0.676(10) 1 calc R U P T 1
H62C H 0.356413 0.299420 0.562159 0.183 Uiso 0.676(10) 1 calc R U P T 1
S28B S 0.2806(5) 0.3834(3) 0.6075(4) 0.060(3) Uani 0.324(10) 1 d D U P T 2
C61B C 0.1977(12) 0.3967(10) 0.7007(5) 0.064(3) Uani 0.324(10) 1 d D U P T 2
H61D H 0.141459 0.404161 0.696430 0.096 Uiso 0.324(10) 1 calc R U P T 2
H61E H 0.192975 0.444983 0.721511 0.096 Uiso 0.324(10) 1 calc R U P T 2
H61F H 0.213734 0.348283 0.735012 0.096 Uiso 0.324(10) 1 calc R U P T 2
C62B C 0.2123(12) 0.3782(9) 0.5594(9) 0.056(4) Uani 0.324(10) 1 d D U P T 2
H62D H 0.239287 0.387074 0.504015 0.084 Uiso 0.324(10) 1 calc R U P T 2
H62E H 0.154635 0.420455 0.576729 0.084 Uiso 0.324(10) 1 calc R U P T 2
H62F H 0.205963 0.324250 0.571243 0.084 Uiso 0.324(10) 1 calc R U P T 2
O28 O 0.2953(3) 0.4635(2) 0.5806(3) 0.0441(11) Uani 1 1 d D . . . .
Cl1 Cl 0.15506(14) 0.18348(11) 0.53947(11) 0.0563(5) Uani 1 1 d . . . . .
O5 O 0.0934(5) 0.1489(6) 0.5795(6) 0.130(4) Uani 1 1 d . . . . .
O6 O 0.2210(5) 0.1536(5) 0.5763(5) 0.101(3) Uani 1 1 d . . . . .
O7 O 0.2046(7) 0.1578(6) 0.4667(4) 0.132(4) Uani 1 1 d . . . . .
O8 O 0.1218(6) 0.2689(5) 0.5353(6) 0.129(4) Uani 1 1 d . . . . .
Cl2 Cl 0.17442(12) 0.40817(11) 0.15801(10) 0.0447(4) Uani 1 1 d . . . . .
O9 O 0.0981(5) 0.4602(5) 0.2099(4) 0.102(3) Uani 1 1 d . . . . .
O10 O 0.2459(5) 0.4253(7) 0.1553(4) 0.129(4) Uani 1 1 d . . . . .
O11 O 0.1796(9) 0.3296(5) 0.1840(5) 0.141(4) Uani 1 1 d . . . . .
O12 O 0.1668(4) 0.4247(4) 0.0838(3) 0.0716(18) Uani 1 1 d . . . . .
Cl3 Cl 0.32764(10) 0.77062(9) 0.02143(8) 0.0314(3) Uani 1 1 d . . . . .
O13 O 0.2668(4) 0.7810(4) 0.0964(4) 0.094(3) Uani 1 1 d . . . . .
O14 O 0.3249(8) 0.7083(5) -0.0106(5) 0.130(4) Uani 1 1 d . . . . .
O15 O 0.3101(4) 0.8436(3) -0.0272(3) 0.0544(14) Uani 1 1 d . . . . .
O16 O 0.4099(4) 0.7477(5) 0.0275(4) 0.102(3) Uani 1 1 d . . . . .
Cl4 Cl 0.87928(10) 0.79386(10) 0.09076(9) 0.0365(3) Uani 1 1 d . . . . .
O17 O 0.8016(4) 0.8547(4) 0.0832(4) 0.0727(18) Uani 1 1 d . . . . .
O18 O 0.9382(4) 0.8312(4) 0.0893(4) 0.0681(17) Uani 1 1 d . . . . .
O19 O 0.8569(5) 0.7483(5) 0.1609(4) 0.094(2) Uani 1 1 d . . . . .
O20 O 0.9191(4) 0.7413(4) 0.0303(4) 0.0741(19) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1 1.981(4) . ?
Cu1 N23 1.994(4) . ?
Cu1 N22 1.998(4) . ?
Cu1 N3 2.010(4) . ?
Cu1 O1 2.322(5) . ?
Cu2 N7 1.999(4) . ?
Cu2 N5 2.004(4) . ?
Cu2 N4 2.009(4) . ?
Cu2 N9 2.009(4) . ?
Cu2 O2 2.268(4) . ?
Cu3 N13 1.990(4) . ?
Cu3 N11 2.012(4) . ?
Cu3 N10 2.017(4) . ?
Cu3 N15 2.017(4) . ?
Cu3 O3 2.299(4) . ?
Cu4 N19 1.979(4) . ?
Cu4 N17 2.003(4) . ?
Cu4 N16 2.005(4) . ?
Cu4 N21 2.010(4) . ?
Cu4 O4 2.353(5) . ?
N1 C3 1.291(7) . ?
N1 C1 1.470(7) . ?
N2 C3 1.330(7) . ?
N2 C2 1.406(7) . ?
N2 H2 0.8800 . ?
N3 C5 1.345(7) . ?
N3 C4 1.368(6) . ?
N4 C5 1.332(7) . ?
N4 C6 1.377(6) . ?
N5 C7 1.288(7) . ?
N5 C9 1.473(7) . ?
N6 C7 1.333(7) . ?
N6 C8 1.421(7) . ?
N6 H6 0.8800 . ?
N7 C12 1.290(7) . ?
N7 C10 1.481(6) . ?
N8 C12 1.332(7) . ?
N8 C11 1.399(7) . ?
N8 H8 0.8800 . ?
N9 C14 1.337(7) . ?
N9 C13 1.374(6) . ?
N10 C14 1.330(7) . ?
N10 C15 1.371(6) . ?
N11 C16 1.297(7) . ?
N11 C18 1.480(7) . ?
N12 C16 1.328(7) . ?
N12 C17 1.400(7) . ?
N12 H12 0.8800 . ?
N13 C21 1.296(7) . ?
N13 C19 1.477(7) . ?
N14 C21 1.329(7) . ?
N14 C20 1.451(7) . ?
N14 H14A 0.8800 . ?
N15 C23 1.337(7) . ?
N15 C22 1.375(6) . ?
N16 C23 1.346(6) . ?
N16 C24 1.377(6) . ?
N17 C25 1.293(7) . ?
N17 C27 1.479(7) . ?
N18 C25 1.340(7) . ?
N18 C26 1.472(7) . ?
N18 H18 0.8800 . ?
N19 C30 1.294(7) . ?
N19 C28 1.491(6) . ?
N20 C30 1.335(7) . ?
N20 C29 1.473(7) . ?
N20 H20 0.8800 . ?
N21 C32 1.336(7) . ?
N21 C31 1.380(6) . ?
N22 C32 1.333(7) . ?
N22 C33 1.379(6) . ?
N23 C34 1.296(7) . ?
N23 C36 1.472(6) . ?
N24 C34 1.331(7) . ?
N24 C35 1.470(8) . ?
N24 H24 0.8800 . ?
C1 C2 1.544(8) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.461(7) . ?
C4 C6 1.375(7) . ?
C5 H5 0.9500 . ?
C6 C7 1.451(7) . ?
C8 C9 1.540(9) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.543(8) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.456(7) . ?
C13 C15 1.376(7) . ?
C14 H14 0.9500 . ?
C15 C16 1.459(7) . ?
C17 C18 1.546(8) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.544(8) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.463(7) . ?
C22 C24 1.370(7) . ?
C23 H23 0.9500 . ?
C24 C25 1.454(7) . ?
C26 C27 1.539(8) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.539(8) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.457(7) . ?
C31 C33 1.374(7) . ?
C32 H32 0.9500 . ?
C33 C34 1.456(7) . ?
C35 C36 1.541(8) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
S1 O1 1.495(5) . ?
S1 C38 1.748(9) . ?
S1 C37 1.763(8) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
O2 S2A 1.470(6) . ?
O2 S2B 1.489(2) . ?
C39 S2A 1.752(9) . ?
C39 S2B 1.796(2) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 S2A 1.771(11) . ?
C40 S2B 1.804(2) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
O3 S3B 1.470(5) . ?
O3 S3A 1.492(2) . ?
C41 S3A 1.795(2) . ?
C41 S3B 1.814(9) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 S3B 1.761(8) . ?
C42 S3A 1.800(2) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
O4 C43 1.340(13) . ?
O4 C46 1.454(12) . ?
C43 C44 1.500(16) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 C45 1.433(16) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 C46 1.461(14) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
O21 S21A 1.439(8) . ?
O21 S21B 1.498(2) . ?
C47 S21B 1.798(2) . ?
C47 S21A 1.815(11) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 S21B 1.799(2) . ?
C48 S21A 1.834(10) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
S22 O22 1.469(6) . ?
S22 C49 1.747(9) . ?
S22 C50 1.772(10) . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
O23 S23B 1.4647(19) . ?
O23 S23A 1.4818(19) . ?
C51 S23A 1.768(2) . ?
C51 S23B 1.771(2) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 S23A 1.775(2) . ?
C52 S23B 1.784(2) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
O24 S24B 1.490(2) . ?
O24 S24A 1.496(2) . ?
C53 S24B 1.798(9) . ?
C53 S24A 1.798(8) . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 S24A 1.751(8) . ?
C54 S24B 1.774(9) . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
S25 O25 1.514(5) . ?
S25 C55 1.760(8) . ?
S25 C56 1.777(10) . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
S26A O26 1.5095(19) . ?
S26A C58A 1.803(2) . ?
S26A C57A 1.803(2) . ?
C57A H57A 0.9800 . ?
C57A H57B 0.9800 . ?
C57A H57C 0.9800 . ?
C58A H58A 0.9800 . ?
C58A H58B 0.9800 . ?
C58A H58C 0.9800 . ?
S26B O26 1.5122(19) . ?
S26B C58B 1.799(2) . ?
S26B C57B 1.801(2) . ?
C57B H57D 0.9800 . ?
C57B H57E 0.9800 . ?
C57B H57F 0.9800 . ?
C58B H58D 0.9800 . ?
C58B H58E 0.9800 . ?
C58B H58F 0.9800 . ?
C59 S27B 1.789(2) . ?
C59 S27A 1.790(2) . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 S27A 1.784(2) . ?
C60 S27B 1.785(2) . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
S27A O27 1.491(2) . ?
S27B O27 1.493(2) . ?
S28A O28 1.493(2) . ?
S28A C62A 1.799(2) . ?
S28A C61A 1.800(2) . ?
C61A H61A 0.9800 . ?
C61A H61B 0.9800 . ?
C61A H61C 0.9800 . ?
C62A H62A 0.9800 . ?
C62A H62B 0.9800 . ?
C62A H62C 0.9800 . ?
S28B O28 1.498(2) . ?
S28B C62B 1.799(2) . ?
S28B C61B 1.801(2) . ?
C61B H61D 0.9800 . ?
C61B H61E 0.9800 . ?
C61B H61F 0.9800 . ?
C62B H62D 0.9800 . ?
C62B H62E 0.9800 . ?
C62B H62F 0.9800 . ?
Cl1 O5 1.352(7) . ?
Cl1 O7 1.381(8) . ?
Cl1 O8 1.399(8) . ?
Cl1 O6 1.450(8) . ?
Cl2 O11 1.361(8) . ?
Cl2 O10 1.385(7) . ?
Cl2 O12 1.422(6) . ?
Cl2 O9 1.427(7) . ?
Cl3 O16 1.387(6) . ?
Cl3 O14 1.396(6) . ?
Cl3 O13 1.412(6) . ?
Cl3 O15 1.427(5) . ?
Cl4 O19 1.406(6) . ?
Cl4 O17 1.412(6) . ?
Cl4 O20 1.416(6) . ?
Cl4 O18 1.423(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 N23 97.32(18) . . ?
N1 Cu1 N22 170.1(2) . . ?
N23 Cu1 N22 81.22(17) . . ?
N1 Cu1 N3 81.20(17) . . ?
N23 Cu1 N3 174.19(19) . . ?
N22 Cu1 N3 99.26(17) . . ?
N1 Cu1 O1 94.6(2) . . ?
N23 Cu1 O1 92.29(18) . . ?
N22 Cu1 O1 95.24(19) . . ?
N3 Cu1 O1 93.43(17) . . ?
N7 Cu2 N5 98.58(18) . . ?
N7 Cu2 N4 172.73(18) . . ?
N5 Cu2 N4 81.10(17) . . ?
N7 Cu2 N9 81.35(17) . . ?
N5 Cu2 N9 174.87(19) . . ?
N4 Cu2 N9 98.31(17) . . ?
N7 Cu2 O2 94.59(18) . . ?
N5 Cu2 O2 87.9(2) . . ?
N4 Cu2 O2 92.66(18) . . ?
N9 Cu2 O2 97.2(2) . . ?
N13 Cu3 N11 97.95(18) . . ?
N13 Cu3 N10 172.66(19) . . ?
N11 Cu3 N10 80.97(17) . . ?
N13 Cu3 N15 80.83(17) . . ?
N11 Cu3 N15 169.13(18) . . ?
N10 Cu3 N15 98.85(17) . . ?
N13 Cu3 O3 92.82(19) . . ?
N11 Cu3 O3 95.02(18) . . ?
N10 Cu3 O3 94.51(18) . . ?
N15 Cu3 O3 95.83(17) . . ?
N19 Cu4 N17 98.06(18) . . ?
N19 Cu4 N16 175.27(18) . . ?
N17 Cu4 N16 81.48(17) . . ?
N19 Cu4 N21 81.34(17) . . ?
N17 Cu4 N21 173.35(19) . . ?
N16 Cu4 N21 98.56(17) . . ?
N19 Cu4 O4 91.98(19) . . ?
N17 Cu4 O4 95.5(2) . . ?
N16 Cu4 O4 92.74(18) . . ?
N21 Cu4 O4 91.1(2) . . ?
C3 N1 C1 108.3(4) . . ?
C3 N1 Cu1 115.3(4) . . ?
C1 N1 Cu1 136.3(4) . . ?
C3 N2 C2 112.7(4) . . ?
C3 N2 H2 123.6 . . ?
C2 N2 H2 123.6 . . ?
C5 N3 C4 105.1(4) . . ?
C5 N3 Cu1 141.6(4) . . ?
C4 N3 Cu1 112.4(3) . . ?
C5 N4 C6 105.0(4) . . ?
C5 N4 Cu2 142.6(4) . . ?
C6 N4 Cu2 112.3(3) . . ?
C7 N5 C9 107.9(4) . . ?
C7 N5 Cu2 113.3(3) . . ?
C9 N5 Cu2 133.9(4) . . ?
C7 N6 C8 111.5(4) . . ?
C7 N6 H6 124.2 . . ?
C8 N6 H6 124.2 . . ?
C12 N7 C10 108.1(4) . . ?
C12 N7 Cu2 114.5(3) . . ?
C10 N7 Cu2 136.2(4) . . ?
C12 N8 C11 113.1(5) . . ?
C12 N8 H8 123.4 . . ?
C11 N8 H8 123.4 . . ?
C14 N9 C13 105.3(4) . . ?
C14 N9 Cu2 142.2(4) . . ?
C13 N9 Cu2 112.5(3) . . ?
C14 N10 C15 105.5(4) . . ?
C14 N10 Cu3 141.2(4) . . ?
C15 N10 Cu3 112.9(3) . . ?
C16 N11 C18 107.7(4) . . ?
C16 N11 Cu3 114.6(3) . . ?
C18 N11 Cu3 137.4(4) . . ?
C16 N12 C17 113.8(4) . . ?
C16 N12 H12 123.1 . . ?
C17 N12 H12 123.1 . . ?
C21 N13 C19 107.3(4) . . ?
C21 N13 Cu3 115.5(3) . . ?
C19 N13 Cu3 134.4(4) . . ?
C21 N14 C20 109.0(4) . . ?
C21 N14 H14A 125.5 . . ?
C20 N14 H14A 125.5 . . ?
C23 N15 C22 105.4(4) . . ?
C23 N15 Cu3 141.5(4) . . ?
C22 N15 Cu3 113.1(3) . . ?
C23 N16 C24 104.7(4) . . ?
C23 N16 Cu4 141.7(4) . . ?
C24 N16 Cu4 112.7(3) . . ?
C25 N17 C27 107.7(4) . . ?
C25 N17 Cu4 113.9(3) . . ?
C27 N17 Cu4 138.2(4) . . ?
C25 N18 C26 108.1(4) . . ?
C25 N18 H18 125.9 . . ?
C26 N18 H18 125.9 . . ?
C30 N19 C28 107.3(4) . . ?
C30 N19 Cu4 115.1(3) . . ?
C28 N19 Cu4 136.2(4) . . ?
C30 N20 C29 108.0(4) . . ?
C30 N20 H20 126.0 . . ?
C29 N20 H20 126.0 . . ?
C32 N21 C31 105.1(4) . . ?
C32 N21 Cu4 141.8(4) . . ?
C31 N21 Cu4 112.4(3) . . ?
C32 N22 C33 105.5(4) . . ?
C32 N22 Cu1 141.0(4) . . ?
C33 N22 Cu1 113.1(3) . . ?
C34 N23 C36 107.6(4) . . ?
C34 N23 Cu1 115.0(3) . . ?
C36 N23 Cu1 137.3(3) . . ?
C34 N24 C35 107.9(5) . . ?
C34 N24 H24 126.0 . . ?
C35 N24 H24 126.0 . . ?
N1 C1 C2 104.5(4) . . ?
N1 C1 H1A 110.9 . . ?
C2 C1 H1A 110.9 . . ?
N1 C1 H1B 110.9 . . ?
C2 C1 H1B 110.9 . . ?
H1A C1 H1B 108.9 . . ?
N2 C2 C1 101.2(4) . . ?
N2 C2 H2A 111.5 . . ?
C1 C2 H2A 111.5 . . ?
N2 C2 H2B 111.5 . . ?
C1 C2 H2B 111.5 . . ?
H2A C2 H2B 109.3 . . ?
N1 C3 N2 113.1(5) . . ?
N1 C3 C4 116.5(4) . . ?
N2 C3 C4 130.4(5) . . ?
N3 C4 C6 108.3(4) . . ?
N3 C4 C3 114.1(4) . . ?
C6 C4 C3 137.6(5) . . ?
N4 C5 N3 113.3(4) . . ?
N4 C5 H5 123.4 . . ?
N3 C5 H5 123.4 . . ?
C4 C6 N4 108.3(4) . . ?
C4 C6 C7 137.8(5) . . ?
N4 C6 C7 113.9(4) . . ?
N5 C7 N6 114.1(4) . . ?
N5 C7 C6 117.2(5) . . ?
N6 C7 C6 128.6(5) . . ?
N6 C8 C9 101.6(4) . . ?
N6 C8 H8A 111.4 . . ?
C9 C8 H8A 111.4 . . ?
N6 C8 H8B 111.4 . . ?
C9 C8 H8B 111.4 . . ?
H8A C8 H8B 109.3 . . ?
N5 C9 C8 104.7(5) . . ?
N5 C9 H9A 110.8 . . ?
C8 C9 H9A 110.8 . . ?
N5 C9 H9B 110.8 . . ?
C8 C9 H9B 110.8 . . ?
H9A C9 H9B 108.9 . . ?
N7 C10 C11 104.2(4) . . ?
N7 C10 H10A 110.9 . . ?
C11 C10 H10A 110.9 . . ?
N7 C10 H10B 110.9 . . ?
C11 C10 H10B 110.9 . . ?
H10A C10 H10B 108.9 . . ?
N8 C11 C10 101.3(5) . . ?
N8 C11 H11A 111.5 . . ?
C10 C11 H11A 111.5 . . ?
N8 C11 H11B 111.5 . . ?
C10 C11 H11B 111.5 . . ?
H11A C11 H11B 109.3 . . ?
N7 C12 N8 112.9(4) . . ?
N7 C12 C13 117.0(5) . . ?
N8 C12 C13 130.0(5) . . ?
N9 C13 C15 107.9(4) . . ?
N9 C13 C12 114.2(4) . . ?
C15 C13 C12 137.8(5) . . ?
N10 C14 N9 113.2(5) . . ?
N10 C14 H14 123.4 . . ?
N9 C14 H14 123.4 . . ?
N10 C15 C13 108.1(4) . . ?
N10 C15 C16 114.4(4) . . ?
C13 C15 C16 137.4(5) . . ?
N11 C16 N12 112.8(5) . . ?
N11 C16 C15 116.9(5) . . ?
N12 C16 C15 130.3(5) . . ?
N12 C17 C18 100.7(4) . . ?
N12 C17 H17A 111.6 . . ?
C18 C17 H17A 111.6 . . ?
N12 C17 H17B 111.6 . . ?
C18 C17 H17B 111.6 . . ?
H17A C17 H17B 109.4 . . ?
N11 C18 C17 104.8(4) . . ?
N11 C18 H18A 110.8 . . ?
C17 C18 H18A 110.8 . . ?
N11 C18 H18B 110.8 . . ?
C17 C18 H18B 110.8 . . ?
H18A C18 H18B 108.9 . . ?
N13 C19 C20 103.9(4) . . ?
N13 C19 H19A 111.0 . . ?
C20 C19 H19A 111.0 . . ?
N13 C19 H19B 111.0 . . ?
C20 C19 H19B 111.0 . . ?
H19A C19 H19B 109.0 . . ?
N14 C20 C19 101.6(4) . . ?
N14 C20 H20A 111.5 . . ?
C19 C20 H20A 111.5 . . ?
N14 C20 H20B 111.5 . . ?
C19 C20 H20B 111.5 . . ?
H20A C20 H20B 109.3 . . ?
N13 C21 N14 115.7(5) . . ?
N13 C21 C22 116.3(4) . . ?
N14 C21 C22 127.8(5) . . ?
C24 C22 N15 108.1(4) . . ?
C24 C22 C21 138.1(5) . . ?
N15 C22 C21 113.7(4) . . ?
N15 C23 N16 113.0(4) . . ?
N15 C23 H23 123.5 . . ?
N16 C23 H23 123.5 . . ?
C22 C24 N16 108.7(4) . . ?
C22 C24 C25 137.4(5) . . ?
N16 C24 C25 113.7(4) . . ?
N17 C25 N18 116.6(5) . . ?
N17 C25 C24 117.6(4) . . ?
N18 C25 C24 125.7(5) . . ?
N18 C26 C27 102.7(4) . . ?
N18 C26 H26A 111.2 . . ?
C27 C26 H26A 111.2 . . ?
N18 C26 H26B 111.2 . . ?
C27 C26 H26B 111.2 . . ?
H26A C26 H26B 109.1 . . ?
N17 C27 C26 104.7(4) . . ?
N17 C27 H27A 110.8 . . ?
C26 C27 H27A 110.8 . . ?
N17 C27 H27B 110.8 . . ?
C26 C27 H27B 110.8 . . ?
H27A C27 H27B 108.9 . . ?
N19 C28 C29 104.4(4) . . ?
N19 C28 H28A 110.9 . . ?
C29 C28 H28A 110.9 . . ?
N19 C28 H28B 110.9 . . ?
C29 C28 H28B 110.9 . . ?
H28A C28 H28B 108.9 . . ?
N20 C29 C28 102.9(4) . . ?
N20 C29 H29A 111.2 . . ?
C28 C29 H29A 111.2 . . ?
N20 C29 H29B 111.2 . . ?
C28 C29 H29B 111.2 . . ?
H29A C29 H29B 109.1 . . ?
N19 C30 N20 117.1(5) . . ?
N19 C30 C31 116.8(5) . . ?
N20 C30 C31 126.1(5) . . ?
C33 C31 N21 108.3(4) . . ?
C33 C31 C30 137.8(5) . . ?
N21 C31 C30 113.8(4) . . ?
N22 C32 N21 113.3(5) . . ?
N22 C32 H32 123.3 . . ?
N21 C32 H32 123.3 . . ?
C31 C33 N22 107.8(4) . . ?
C31 C33 C34 138.3(5) . . ?
N22 C33 C34 113.9(4) . . ?
N23 C34 N24 115.8(5) . . ?
N23 C34 C33 116.6(5) . . ?
N24 C34 C33 127.6(5) . . ?
N24 C35 C36 101.4(4) . . ?
N24 C35 H35A 111.5 . . ?
C36 C35 H35A 111.5 . . ?
N24 C35 H35B 111.5 . . ?
C36 C35 H35B 111.5 . . ?
H35A C35 H35B 109.3 . . ?
N23 C36 C35 104.2(4) . . ?
N23 C36 H36A 110.9 . . ?
C35 C36 H36A 110.9 . . ?
N23 C36 H36B 110.9 . . ?
C35 C36 H36B 110.9 . . ?
H36A C36 H36B 108.9 . . ?
O1 S1 C38 107.3(4) . . ?
O1 S1 C37 105.8(4) . . ?
C38 S1 C37 97.3(5) . . ?
S1 O1 Cu1 115.1(3) . . ?
S1 C37 H37A 109.5 . . ?
S1 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
S1 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
S1 C38 H38A 109.5 . . ?
S1 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
S1 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
S2A O2 Cu2 126.7(3) . . ?
S2B O2 Cu2 139.7(4) . . ?
S2A C39 H39A 109.5 . . ?
S2A C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
S2A C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
S2A C40 H40A 109.5 . . ?
S2A C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
S2A C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
O2 S2A C39 116.5(4) . . ?
O2 S2A C40 103.4(5) . . ?
C39 S2A C40 95.5(6) . . ?
O2 S2B C39 113.0(5) . . ?
O2 S2B C40 101.1(5) . . ?
C39 S2B C40 92.8(6) . . ?
S3B O3 Cu3 135.5(3) . . ?
S3A O3 Cu3 135.1(3) . . ?
S3A C41 H41A 109.5 . . ?
S3A C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
S3A C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
S3A C42 H42A 109.5 . . ?
S3A C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
S3A C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O3 S3A C41 118.7(5) . . ?
O3 S3A C42 106.1(4) . . ?
C41 S3A C42 99.8(5) . . ?
O3 S3B C42 109.1(4) . . ?
O3 S3B C41 118.8(4) . . ?
C42 S3B C41 100.5(5) . . ?
C43 O4 C46 105.7(8) . . ?
C43 O4 Cu4 124.1(6) . . ?
C46 O4 Cu4 122.8(6) . . ?
O4 C43 C44 106.5(11) . . ?
O4 C43 H43A 110.4 . . ?
C44 C43 H43A 110.4 . . ?
O4 C43 H43B 110.4 . . ?
C44 C43 H43B 110.4 . . ?
H43A C43 H43B 108.6 . . ?
C45 C44 C43 102.7(10) . . ?
C45 C44 H44A 111.2 . . ?
C43 C44 H44A 111.2 . . ?
C45 C44 H44B 111.2 . . ?
C43 C44 H44B 111.2 . . ?
H44A C44 H44B 109.1 . . ?
C44 C45 C46 104.7(9) . . ?
C44 C45 H45A 110.8 . . ?
C46 C45 H45A 110.8 . . ?
C44 C45 H45B 110.8 . . ?
C46 C45 H45B 110.8 . . ?
H45A C45 H45B 108.9 . . ?
O4 C46 C45 107.8(10) . . ?
O4 C46 H46A 110.2 . . ?
C45 C46 H46A 110.2 . . ?
O4 C46 H46B 110.2 . . ?
C45 C46 H46B 110.2 . . ?
H46A C46 H46B 108.5 . . ?
S21A C47 H47A 109.5 . . ?
S21A C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
S21A C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
S21A C48 H48A 109.5 . . ?
S21A C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
S21A C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
O22 S22 C49 107.7(5) . . ?
O22 S22 C50 106.3(4) . . ?
C49 S22 C50 99.3(6) . . ?
S22 C49 H49A 109.5 . . ?
S22 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
S22 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
S22 C50 H50A 109.5 . . ?
S22 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
S22 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
O21 S21A C47 112.8(6) . . ?
O21 S21A C48 108.8(5) . . ?
C47 S21A C48 97.5(5) . . ?
O21 S21B C47 110.8(7) . . ?
O21 S21B C48 107.9(6) . . ?
C47 S21B C48 99.4(7) . . ?
S23A C51 H51A 109.5 . . ?
S23A C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
S23A C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
S23A C52 H52A 109.5 . . ?
S23A C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
S23A C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
O23 S23A C51 111.28(18) . . ?
O23 S23A C52 109.83(17) . . ?
C51 S23A C52 98.97(14) . . ?
O23 S23B C51 112.00(18) . . ?
O23 S23B C52 110.19(17) . . ?
C51 S23B C52 98.55(14) . . ?
S24A C53 H53A 109.5 . . ?
S24A C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
S24A C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
S24A C54 H54A 109.5 . . ?
S24A C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
S24A C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
O24 S24A C54 113.5(4) . . ?
O24 S24A C53 111.6(4) . . ?
C54 S24A C53 96.7(4) . . ?
O24 S24B C54 112.5(4) . . ?
O24 S24B C53 111.9(4) . . ?
C54 S24B C53 95.9(5) . . ?
O25 S25 C55 105.3(3) . . ?
O25 S25 C56 105.1(4) . . ?
C55 S25 C56 98.1(5) . . ?
S25 C55 H55A 109.5 . . ?
S25 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
S25 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
S25 C56 H56A 109.5 . . ?
S25 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
S25 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
O26 S26A C58A 105.69(17) . . ?
O26 S26A C57A 105.61(17) . . ?
C58A S26A C57A 95.52(14) . . ?
S26A C57A H57A 109.5 . . ?
S26A C57A H57B 109.5 . . ?
H57A C57A H57B 109.5 . . ?
S26A C57A H57C 109.5 . . ?
H57A C57A H57C 109.5 . . ?
H57B C57A H57C 109.5 . . ?
S26A C58A H58A 109.5 . . ?
S26A C58A H58B 109.5 . . ?
H58A C58A H58B 109.5 . . ?
S26A C58A H58C 109.5 . . ?
H58A C58A H58C 109.5 . . ?
H58B C58A H58C 109.5 . . ?
O26 S26B C58B 105.84(17) . . ?
O26 S26B C57B 105.66(18) . . ?
C58B S26B C57B 95.78(14) . . ?
S26B C57B H57D 109.5 . . ?
S26B C57B H57E 109.5 . . ?
H57D C57B H57E 109.5 . . ?
S26B C57B H57F 109.5 . . ?
H57D C57B H57F 109.5 . . ?
H57E C57B H57F 109.5 . . ?
S26B C58B H58D 109.5 . . ?
S26B C58B H58E 109.5 . . ?
H58D C58B H58E 109.5 . . ?
S26B C58B H58F 109.5 . . ?
H58D C58B H58F 109.5 . . ?
H58E C58B H58F 109.5 . . ?
S27A C59 H59A 109.5 . . ?
S27A C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
S27A C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
S27A C60 H60A 109.5 . . ?
S27A C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
S27A C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
O27 S27A C60 108.68(18) . . ?
O27 S27A C59 108.00(18) . . ?
C60 S27A C59 97.28(14) . . ?
O27 S27B C60 108.51(18) . . ?
O27 S27B C59 107.90(18) . . ?
C60 S27B C59 97.25(14) . . ?
O28 S28A C62A 104.2(7) . . ?
O28 S28A C61A 101.2(10) . . ?
C62A S28A C61A 95.0(11) . . ?
S28A C61A H61A 109.5 . . ?
S28A C61A H61B 109.5 . . ?
H61A C61A H61B 109.5 . . ?
S28A C61A H61C 109.5 . . ?
H61A C61A H61C 109.5 . . ?
H61B C61A H61C 109.5 . . ?
S28A C62A H62A 109.5 . . ?
S28A C62A H62B 109.5 . . ?
H62A C62A H62B 109.5 . . ?
S28A C62A H62C 109.5 . . ?
H62A C62A H62C 109.5 . . ?
H62B C62A H62C 109.5 . . ?
O28 S28B C62B 106.65(18) . . ?
O28 S28B C61B 106.50(18) . . ?
C62B S28B C61B 95.69(14) . . ?
S28B C61B H61D 109.5 . . ?
S28B C61B H61E 109.5 . . ?
H61D C61B H61E 109.5 . . ?
S28B C61B H61F 109.5 . . ?
H61D C61B H61F 109.5 . . ?
H61E C61B H61F 109.5 . . ?
S28B C62B H62D 109.5 . . ?
S28B C62B H62E 109.5 . . ?
H62D C62B H62E 109.5 . . ?
S28B C62B H62F 109.5 . . ?
H62D C62B H62F 109.5 . . ?
H62E C62B H62F 109.5 . . ?
O5 Cl1 O7 115.4(7) . . ?
O5 Cl1 O8 113.3(6) . . ?
O7 Cl1 O8 109.0(6) . . ?
O5 Cl1 O6 107.3(5) . . ?
O7 Cl1 O6 101.1(6) . . ?
O8 Cl1 O6 110.0(6) . . ?
O11 Cl2 O10 112.7(7) . . ?
O11 Cl2 O12 110.1(5) . . ?
O10 Cl2 O12 109.1(4) . . ?
O11 Cl2 O9 107.4(6) . . ?
O10 Cl2 O9 108.1(6) . . ?
O12 Cl2 O9 109.4(5) . . ?
O16 Cl3 O14 108.5(6) . . ?
O16 Cl3 O13 106.9(5) . . ?
O14 Cl3 O13 110.5(6) . . ?
O16 Cl3 O15 111.2(4) . . ?
O14 Cl3 O15 108.2(4) . . ?
O13 Cl3 O15 111.5(3) . . ?
O19 Cl4 O17 107.9(5) . . ?
O19 Cl4 O20 109.2(5) . . ?
O17 Cl4 O20 110.1(4) . . ?
O19 Cl4 O18 110.4(5) . . ?
O17 Cl4 O18 109.7(4) . . ?
O20 Cl4 O18 109.5(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N2 H2 O26 0.88 2.12 2.842(6) 138.6 2_666 yes
N6 H6 O27 0.88 2.39 2.942(7) 121.2 2_666 yes
N8 H8 O24 0.88 2.25 2.797(7) 120.0 2_666 yes
N8 H8 O16 0.88 2.60 3.285(10) 135.6 . yes
N12 H12 O16 0.88 2.32 3.059(8) 141.8 . yes
N14 H14A N18 0.88 2.65 3.317(7) 133.1 . yes
N14 H14A O23 0.88 2.28 3.027(6) 142.3 2_756 yes
N18 H18 N14 0.88 2.63 3.317(7) 135.5 . yes
N18 H18 O23 0.88 2.33 3.010(5) 133.7 2_756 yes
N18 H18 O26 0.88 2.28 2.844(6) 122.1 . yes
N20 H20 N24 0.88 2.60 3.323(7) 139.6 . yes
N20 H20 O25 0.88 2.33 2.780(7) 111.7 2_666 yes
N24 H24 N20 0.88 2.70 3.323(7) 128.9 . yes
N24 H24 O13 0.88 2.36 3.070(8) 137.6 2_666 yes
C5 H5 O28 0.95 2.51 3.168(7) 126.4 2_666 yes
C10 H10B O22 0.99 2.62 3.283(8) 124.8 2_676 yes
C14 H14 O28 0.95 2.41 3.193(7) 140.1 2_666 yes
C17 H17A O10 0.99 2.56 3.351(10) 137.1 2_665 yes
C19 H19B O14 0.99 2.43 3.372(11) 159.6 2_665 yes
C20 H20B O18 0.99 2.64 3.532(8) 150.8 2_765 yes
C20 H20B O20 0.99 2.61 3.532(9) 154.9 2_765 yes
C23 H23 O28 0.95 2.41 3.148(6) 134.1 2_666 yes
C26 H26A O22 0.99 2.53 3.452(9) 154.5 2_766 yes
C28 H28B O22 0.99 2.54 3.310(8) 134.9 1_545 yes
C29 H29A O22 0.99 2.62 3.349(9) 130.7 1_545 yes
C29 H29A S23A^a 0.99 3.02 3.784(7) 135.2 . yes
C32 H32 O28 0.95 2.50 3.129(7) 123.8 2_666 yes
C35 H35B O14 0.99 2.60 3.340(9) 131.3 2_666 yes
C38 H38B O9 0.98 2.63 3.584(13) 165.6 2_666 yes
C39 H39B^a O17 0.98 2.54 3.503(11) 168.2 . yes
C39 H39C^a O21 0.98 2.58 3.268(14) 127.6 2_676 yes
C40 H40C^a O6 0.98 2.50 3.247(12) 133.3 2_666 yes
C42 H42B^a O12 0.98 2.57 3.513(11) 161.3 1_655 yes
C43 H43A S28A^a 0.99 2.96 3.858(16) 151.0 2_666 yes
C44 H44B O9 0.99 2.64 3.401(15) 133.5 1_655 yes
C45 H45B O8 0.99 2.54 3.366(16) 141.3 1_655 yes
C48 H48B^a O16 0.98 2.54 3.371(13) 142.7 1_556 yes
C49 H49A O21 0.98 2.64 3.436(15) 138.4 . yes
C49 H49B O11 0.98 2.60 3.500(14) 153.2 2_666 yes
C49 H49C O7 0.98 2.60 3.338(14) 132.1 2_666 yes
C51 H51B^a O13 0.98 2.64 3.468(10) 142.8 2_666 yes
C51 H51C^a O18 0.98 2.51 3.387(7) 149.2 2_766 yes
C52 H52B^a O15 0.98 2.57 3.388(8) 140.5 2_666 yes
C54 H54A^a O17 0.98 2.47 3.419(10) 162.0 2_666 yes
C54 H54C^a S21A^a 0.98 2.94 3.781(9) 144.5 2_667 yes
C56 H56A O9 0.98 2.66 3.582(14) 157.5 . yes
C56 H56B O19 0.98 2.49 3.447(13) 164.3 1_455 yes
C57A^a H57A^a O15 0.98 2.57 3.546(12) 171.1 2_665 yes
C57A^a H57C^a O17 0.98 2.26 3.212(9) 165.3 1_545 yes
C58A^a H58A^a Cl4 0.98 2.97 3.913(8) 162.0 1_545 yes
C58A^a H58A^a O18 0.98 2.37 3.208(10) 142.6 1_545 yes
C58A^a H58B^a O6 0.98 2.57 3.398(13) 142.7 2_656 yes
C57B^b H57E^b Cl4 0.98 2.75 3.716(8) 169.6 1_545 yes
C57B^b H57E^b O17 0.98 2.46 3.292(11) 142.5 1_545 yes
C57B^b H57E^b O18 0.98 2.10 3.022(12) 156.8 1_545 yes
C58B^b H58D^b O18 0.98 2.57 3.351(12) 136.5 1_545 yes
C58B^b H58E^b O5 0.98 2.50 3.409(14) 154.8 2_656 yes
C58B^b H58E^b O6 0.98 2.60 3.432(17) 142.9 2_656 yes
C58B^b H58F^b O23 0.98 2.58 3.466(14) 149.7 2_756 yes
C60 H60B^a O7 0.98 2.45 3.355(12) 152.5 . yes
C60 H60C^a O21 0.98 2.58 3.253(11) 126.2 2_666 yes
C61A^a H61A^a S2A^a 0.98 2.22 3.14(2) 156.7 2_666 yes
C61A^a H61B^a O19 0.98 2.62 3.42(2) 139.3 2_666 yes
C61A^a H61C^a S3A^a 0.98 2.90 3.71(3) 140.1 2_666 yes
C62A^a H62A^a O1 0.98 2.27 3.249(17) 172.8 2_666 yes
C62A^a H62C^a S2A^a 0.98 3.01 3.709(17) 128.9 2_666 yes
C61B^b H61E^b O3 0.98 2.60 3.464(15) 146.5 2_666 yes
C61B^b H61F^b O19 0.98 2.60 3.411(11) 140.1 2_666 yes
C62B^b H62D^b O1 0.98 2.46 3.426(18) 166.8 2_666 yes
C62B^b H62F^b O8 0.98 2.41 3.141(12) 131.0 . yes

_refine_diff_density_max         2.741
_refine_diff_density_min         -2.501
_refine_diff_density_rms         0.140



####################################################################### 
# 
# 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_170912mn5_0m_sq_2_2
_database_code_depnum_ccdc_archive 'CCDC 2036136'
loop_
_audit_author_name
_audit_author_address
'Hajime Kamebuchi'
;Nihon University
Japan
;
_audit_update_record             
;
2021-03-11 deposited with the CCDC.	2021-03-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C108 H132 Mn8 N72, 8(Cl O4), 14(C H4 O)'
_chemical_formula_sum            'C122 H188 Cl8 Mn8 N72 O46'
_chemical_formula_weight         4122.55

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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'

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

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   17.046(3)
_cell_length_b                   17.684(3)
_cell_length_c                   18.154(3)
_cell_angle_alpha                68.925(2)
_cell_angle_beta                 70.325(2)
_cell_angle_gamma                70.352(2)
_cell_volume                     4661.7(15)
_cell_formula_units_Z            1
_cell_measurement_temperature    243(2)
_cell_measurement_reflns_used    8107
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      25.68

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_F_000             2128
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.730
_shelx_estimated_absorpt_T_min   0.931
_shelx_estimated_absorpt_T_max   0.964
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6732
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      243(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Bruker TXS fine-focus rotating anode'
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            24745
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.009
_diffrn_reflns_theta_max         26.733
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measured_fraction_theta_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_point_group_measured_fraction_full 0.974
_reflns_number_total             18934
_reflns_number_gt                11608
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 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.

The structure was refined after PLATON/SQUEEZE procedure due to the presence of many heavily disordered solvent molecules. Details of the PLATON/SQUEEZE results are given at the end of this cif file.
;

_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_cell_refinement       'APEX3 (Bruker AXS, 2018)'
_computing_data_reduction        'SAINT (Bruker AXS, 2013)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    'APEX3 (Bruker AXS,2018)'
_computing_publication_material  'APEX3 (Bruker AXS,2018)'
_refine_special_details          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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         18934
_refine_ls_number_parameters     1164
_refine_ls_number_restraints     232
_refine_ls_R_factor_all          0.1231
_refine_ls_R_factor_gt           0.0918
_refine_ls_wR_factor_ref         0.3293
_refine_ls_wR_factor_gt          0.2982
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_restrained_S_all      1.647
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

# start Validation Reply Form
_vrf_PLAT232_170912mn5_0m_sq_2_2 
;
PROBLEM: Hirshfeld Test Diff (M-X)  Mn1      --N2       .       10.7 s.u.  
RESPONSE: This alert is generated because there are many disordered ClO4- in the
structure
;
_vrf_PLAT416_170912mn5_0m_sq_2_2 
;
PROBLEM: Short Intra D-H..H-D       H3       ..H24      .       1.69 Ang.  
RESPONSE: This alert is generated because there are many disordered ClO4- in the
structure
;
_vrf_PLAT934_170912mn5_0m_sq_2_2 
;
PROBLEM: Number of (Iobs-Icalc)/Sigma(W) > 10 Outliers ..          6 Check 
RESPONSE: This alert is generated because there are many disordered ClO4- in the
structure
;
# end Validation Reply Form

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
Mn1 Mn 0.38263(5) 0.85116(4) 0.42614(5) 0.0467(2) Uani 1 1 d . U . . .
Mn2 Mn 0.22624(5) 0.59030(5) 0.75625(5) 0.0553(2) Uani 1 1 d . . . . .
Mn3 Mn 0.62033(5) 0.38860(5) 0.78256(5) 0.0514(2) Uani 1 1 d . . . . .
Mn4 Mn 0.22370(4) 0.34970(5) 0.55139(5) 0.0464(2) Uani 1 1 d . . . . .
N1 N 0.3683(2) 0.7747(2) 0.3596(2) 0.0454(9) Uani 1 1 d . . . . .
N2 N 0.2663(3) 0.9143(3) 0.3939(3) 0.0613(12) Uani 1 1 d . U . . .
N3 N 0.1730(3) 0.9334(3) 0.3268(5) 0.102(2) Uani 1 1 d . . . . .
H3 H 0.149765 0.924760 0.295515 0.123 Uiso 1 1 calc R U . . .
N4 N 0.4439(3) 0.9356(3) 0.3283(3) 0.0577(11) Uani 1 1 d . . . . .
N5 N 0.5649(3) 0.9682(3) 0.2454(3) 0.0705(14) Uani 1 1 d D . . . .
H5 H 0.620062 0.963052 0.226394 0.085 Uiso 1 1 calc R U . . .
N6 N 0.5146(2) 0.7940(2) 0.4217(2) 0.0444(9) Uani 1 1 d . . . . .
N7 N 0.3579(4) 0.9251(3) 0.5121(3) 0.0686(13) Uani 1 1 d . . . . .
N8 N 0.3236(4) 0.9238(3) 0.6413(4) 0.0843(16) Uani 1 1 d . . . . .
H8 H 0.305879 0.905264 0.693863 0.101 Uiso 1 1 calc R U . . .
N9 N 0.3361(3) 0.7716(3) 0.5424(3) 0.0616(12) Uani 1 1 d . U . . .
N10 N 0.2754(3) 0.6842(3) 0.6550(4) 0.0713(15) Uani 1 1 d . . . . .
N13 N 0.1969(3) 0.5048(3) 0.8698(3) 0.0624(12) Uani 1 1 d . . . . .
N14 N 0.2381(3) 0.3956(4) 0.9702(3) 0.0768(15) Uani 1 1 d . . . . .
H14 H 0.273288 0.355470 0.996684 0.092 Uiso 1 1 calc R U . . .
N15 N 0.3514(3) 0.5139(3) 0.7736(3) 0.0544(10) Uani 1 1 d . . . . .
N16 N 0.4857(3) 0.4459(3) 0.7831(2) 0.0504(10) Uani 1 1 d . . . . .
N17 N 0.5534(3) 0.3240(3) 0.8958(3) 0.0705(14) Uani 1 1 d . . . . .
N18 N 0.4339(4) 0.2950(3) 0.9806(3) 0.0819(16) Uani 1 1 d . . . . .
H18 H 0.378704 0.301542 1.000040 0.098 Uiso 1 1 calc R U . . .
N19 N 0.6357(2) 0.3072(2) 0.7073(2) 0.0458(9) Uani 1 1 d . . . . .
N20 N 0.6711(3) 0.4843(3) 0.6803(3) 0.0604(12) Uani 1 1 d . . . . .
N21 N 0.6486(5) 0.4656(4) 0.8371(4) 0.0915(19) Uani 1 1 d . . . . .
N22 N 0.6991(6) 0.5711(5) 0.8234(4) 0.125(3) Uani 1 1 d D . . . .
H22 H 0.720573 0.614509 0.797650 0.150 Uiso 1 1 calc R U . . .
N23 N 0.7389(3) 0.2938(3) 0.7970(3) 0.0675(13) Uani 1 1 d . . . . .
N24 N 0.8423(3) 0.1904(5) 0.7545(4) 0.102(2) Uani 1 1 d . . . . .
H24 H 0.866244 0.150837 0.730324 0.123 Uiso 1 1 calc R U . . .
N25 N 0.0932(4) 0.6334(3) 0.7521(3) 0.0796(16) Uani 1 1 d . . . . .
N26 N -0.0081(4) 0.6329(5) 0.7050(5) 0.129(3) Uani 1 1 d . . . . .
H26A H -0.031754 0.616071 0.680053 0.155 Uiso 1 1 calc R U . . .
N27 N 0.2164(3) 0.5214(3) 0.6823(3) 0.0526(10) Uani 1 1 d . . . . .
N28 N 0.2139(2) 0.4347(2) 0.6192(3) 0.0491(10) Uani 1 1 d . . . . .
N29 N 0.0866(3) 0.4128(3) 0.5786(3) 0.0610(12) Uani 1 1 d . . . . .
N30 N -0.0212(3) 0.4913(4) 0.6523(5) 0.100(2) Uani 1 1 d . . . . .
H30 H -0.045324 0.528742 0.679024 0.120 Uiso 1 1 calc R U . . .
N31 N 0.2765(3) 0.4259(3) 0.4338(3) 0.0571(11) Uani 1 1 d . . . . .
N32 N 0.2109(3) 0.2986(3) 0.4643(4) 0.0708(14) Uani 1 1 d . . . . .
N33 N 0.2365(5) 0.2972(3) 0.3360(4) 0.105(2) Uani 1 1 d D . . . .
H33 H 0.245983 0.317282 0.283328 0.126 Uiso 1 1 calc R U . . .
N34 N 0.3516(2) 0.2755(2) 0.5704(2) 0.0450(9) Uani 1 1 d . . . . .
N35 N 0.1972(3) 0.2441(3) 0.6525(3) 0.0576(11) Uani 1 1 d . . . . .
N36 N 0.2445(3) 0.1308(3) 0.7468(3) 0.0682(13) Uani 1 1 d D . . . .
H36 H 0.281560 0.090062 0.770434 0.082 Uiso 1 1 calc R U . . .
C1 C 0.4067(3) 0.7061(3) 0.3344(3) 0.0489(11) Uani 1 1 d . . . . .
H1 H 0.459028 0.670339 0.345169 0.059 Uiso 1 1 calc R U . . .
C2 C 0.2943(3) 0.7581(3) 0.2900(3) 0.0455(11) Uani 1 1 d . . . . .
C3 C 0.2957(3) 0.8093(3) 0.3307(3) 0.0452(11) Uani 1 1 d . . . . .
C4 C 0.2434(3) 0.8860(3) 0.3502(3) 0.0545(12) Uani 1 1 d . . . . .
C5 C 0.2045(4) 0.9934(4) 0.4017(6) 0.101(3) Uani 1 1 d . . . . .
H5A H 0.179409 0.991595 0.459283 0.121 Uiso 1 1 calc R U . . .
H5AB H 0.233036 1.039591 0.375351 0.121 Uiso 1 1 calc R U . . .
C6 C 0.1401(5) 1.0049(5) 0.3636(7) 0.122(4) Uani 1 1 d . . . . .
H6A H 0.133615 1.058650 0.321622 0.147 Uiso 1 1 calc R U . . .
H6AB H 0.084701 1.002345 0.403296 0.147 Uiso 1 1 calc R U . . .
C7 C 0.4158(4) 1.0161(4) 0.2705(4) 0.0783(19) Uani 1 1 d . . . . .
H7A H 0.383513 1.059175 0.298947 0.094 Uiso 1 1 calc R U . . .
H7AB H 0.379178 1.011058 0.241718 0.094 Uiso 1 1 calc R U . . .
C8 C 0.4973(4) 1.0377(4) 0.2116(4) 0.0714(16) Uani 1 1 d D . . . .
H8A H 0.500398 1.039105 0.156242 0.086 Uiso 1 1 calc R U . . .
H8AB H 0.501770 1.091788 0.210989 0.086 Uiso 1 1 calc R U . . .
C9 C 0.5278(3) 0.9154(3) 0.3091(3) 0.0434(10) Uani 1 1 d . . . . .
C10 C 0.5695(3) 0.8385(3) 0.3606(3) 0.0406(10) Uani 1 1 d . . . . .
C11 C 0.5650(3) 0.7269(3) 0.4608(3) 0.0480(11) Uani 1 1 d . . . . .
H11 H 0.544050 0.685348 0.505815 0.058 Uiso 1 1 calc R U . . .
C12 C 0.6521(3) 0.7953(3) 0.3656(3) 0.0401(10) Uani 1 1 d . . . . .
C13 C 0.3737(7) 1.0015(5) 0.5101(6) 0.105(3) Uani 1 1 d . . . . .
H13A H 0.337103 1.050486 0.480123 0.126 Uiso 1 1 calc R U . . .
H13B H 0.433914 1.002638 0.483695 0.126 Uiso 1 1 calc R U . . .
C14 C 0.3521(6) 1.0014(5) 0.5987(5) 0.101(3) Uani 1 1 d . . . . .
H14A H 0.402742 0.999885 0.613896 0.121 Uiso 1 1 calc R U . . .
H14B H 0.306263 1.050257 0.609537 0.121 Uiso 1 1 calc R U . . .
C15 C 0.3289(4) 0.8864(4) 0.5882(4) 0.0605(14) Uani 1 1 d . . . . .
C16 C 0.3091(4) 0.8075(4) 0.6066(4) 0.0618(15) Uani 1 1 d . . . . .
C17 C 0.3134(4) 0.6982(4) 0.5760(5) 0.0684(17) Uani 1 1 d . . . . .
H17 H 0.323472 0.660471 0.546315 0.082 Uiso 1 1 calc R U . . .
C22 C 0.1154(4) 0.4889(4) 0.9308(4) 0.0748(17) Uani 1 1 d . . . . .
H22A H 0.079583 0.475873 0.906783 0.090 Uiso 1 1 calc R U . . .
H22B H 0.082450 0.537474 0.951454 0.090 Uiso 1 1 calc R U . . .
C23 C 0.1450(4) 0.4151(5) 0.9975(4) 0.0826(19) Uani 1 1 d . . . . .
H23A H 0.125620 0.429295 1.049238 0.099 Uiso 1 1 calc R U . . .
H23B H 0.123071 0.367699 1.004416 0.099 Uiso 1 1 calc R U . . .
C24 C 0.2615(4) 0.4500(3) 0.8968(3) 0.0555(13) Uani 1 1 d . . . . .
C25 C 0.3465(4) 0.4533(3) 0.8474(3) 0.0511(12) Uani 1 1 d . . . . .
C26 C 0.4344(4) 0.5068(3) 0.7386(3) 0.0571(13) Uani 1 1 d . . . . .
H26 H 0.455416 0.541349 0.687237 0.069 Uiso 1 1 calc R U . . .
C27 C 0.4294(4) 0.4109(3) 0.8531(3) 0.0517(12) Uani 1 1 d . . . . .
C28 C 0.4709(4) 0.3424(3) 0.9111(3) 0.0515(12) Uani 1 1 d . . . . .
C29 C 0.5819(5) 0.2529(5) 0.9625(5) 0.095(2) Uani 1 1 d . . . . .
H29A H 0.611414 0.268976 0.990379 0.114 Uiso 1 1 calc R U . . .
H29B H 0.620699 0.205710 0.941927 0.114 Uiso 1 1 calc R U . . .
C30 C 0.4982(5) 0.2307(4) 1.0198(4) 0.087(2) Uani 1 1 d . . . . .
H30A H 0.496597 0.174750 1.022725 0.104 Uiso 1 1 calc R U . . .
H30B H 0.490502 0.233625 1.074732 0.104 Uiso 1 1 calc R U . . .
C31 C 0.6936(4) 0.5388(3) 0.7015(4) 0.0615(15) Uani 1 1 d . . . . .
C32 C 0.6782(5) 0.5251(4) 0.7893(4) 0.0753(18) Uani 1 1 d . . . . .
C33 C 0.6443(9) 0.4639(6) 0.9219(6) 0.146(5) Uani 1 1 d . . . . .
H33A H 0.584855 0.471086 0.954706 0.176 Uiso 1 1 calc R U . . .
H33B H 0.678918 0.410698 0.948685 0.176 Uiso 1 1 calc R U . . .
C34 C 0.6784(8) 0.5330(7) 0.9120(5) 0.140(4) Uani 1 1 d D U . . .
H34A H 0.729989 0.512834 0.932944 0.168 Uiso 1 1 calc R U . . .
H34B H 0.635564 0.572994 0.940319 0.168 Uiso 1 1 calc R U . . .
C35 C 0.7637(3) 0.2416(4) 0.7556(3) 0.0591(14) Uani 1 1 d . . . . .
C36 C 0.8073(4) 0.2759(6) 0.8394(4) 0.089(2) Uani 1 1 d . . . . .
H36A H 0.824080 0.327076 0.830043 0.107 Uiso 1 1 calc R U . . .
H36B H 0.787184 0.252138 0.898193 0.107 Uiso 1 1 calc R U . . .
C37 C 0.8808(6) 0.2146(8) 0.8034(7) 0.134(4) Uani 1 1 d . . . . .
H37A H 0.901629 0.166049 0.845897 0.160 Uiso 1 1 calc R U . . .
H37B H 0.928415 0.240290 0.768518 0.160 Uiso 1 1 calc R U . . .
C38 C 0.0176(6) 0.6973(5) 0.7800(5) 0.112(3) Uani 1 1 d . . . . .
H38A H 0.030949 0.751978 0.760691 0.134 Uiso 1 1 calc R U . . .
H38B H -0.001125 0.681823 0.839590 0.134 Uiso 1 1 calc R U . . .
C39 C -0.0511(7) 0.6994(8) 0.7436(8) 0.162(5) Uani 1 1 d . . . . .
H39A H -0.102907 0.687889 0.785700 0.194 Uiso 1 1 calc R U . . .
H39B H -0.066313 0.753230 0.703852 0.194 Uiso 1 1 calc R U . . .
C40 C 0.0720(4) 0.6007(4) 0.7126(4) 0.0741(17) Uani 1 1 d . . . . .
C41 C 0.1332(3) 0.5348(3) 0.6795(3) 0.0552(13) Uani 1 1 d . . . . .
C42 C 0.2606(3) 0.4616(3) 0.6453(3) 0.0532(12) Uani 1 1 d . . . . .
H42 H 0.320257 0.440141 0.638188 0.064 Uiso 1 1 calc R U . . .
C43 C 0.1313(3) 0.4813(3) 0.6413(3) 0.0526(12) Uani 1 1 d . . . . .
C44 C 0.0650(3) 0.4617(4) 0.6229(3) 0.0598(14) Uani 1 1 d . . . . .
C45 C 0.0078(4) 0.3989(4) 0.5727(5) 0.0799(19) Uani 1 1 d . . . . .
H45A H 0.009112 0.339283 0.591333 0.096 Uiso 1 1 calc R U . . .
H45B H 0.001402 0.421577 0.516618 0.096 Uiso 1 1 calc R U . . .
C46 C -0.0653(4) 0.4465(6) 0.6291(6) 0.111(3) Uani 1 1 d . . . . .
H46A H -0.108956 0.485978 0.600543 0.133 Uiso 1 1 calc R U . . .
H46B H -0.092731 0.407745 0.677261 0.133 Uiso 1 1 calc R U . . .
C47 C 0.3098(4) 0.4935(4) 0.3997(4) 0.0677(17) Uani 1 1 d . . . . .
H47 H 0.318428 0.521866 0.430207 0.081 Uiso 1 1 calc R U . . .
C48 C 0.2745(3) 0.4060(3) 0.3681(4) 0.0551(13) Uani 1 1 d . . . . .
C49 C 0.2399(4) 0.3321(4) 0.3911(4) 0.0643(16) Uani 1 1 d . . . . .
C50 C 0.1791(5) 0.2279(5) 0.4683(6) 0.101(3) Uani 1 1 d . . . . .
H50A H 0.200438 0.176797 0.508300 0.121 Uiso 1 1 calc R U . . .
H50B H 0.116122 0.241350 0.482983 0.121 Uiso 1 1 calc R U . . .
C51 C 0.2131(6) 0.2179(4) 0.3868(6) 0.111(3) Uani 1 1 d D . . . .
H51A H 0.169735 0.208800 0.368838 0.133 Uiso 1 1 calc R U . . .
H51B H 0.263666 0.170553 0.384556 0.133 Uiso 1 1 calc R U . . .
C52 C 0.2629(3) 0.1923(3) 0.6792(3) 0.0459(11) Uani 1 1 d . . . . .
C53 C 0.1183(4) 0.2198(4) 0.7076(4) 0.0715(16) Uani 1 1 d . . . . .
H53A H 0.088715 0.204956 0.678812 0.086 Uiso 1 1 calc R U . . .
H53B H 0.079070 0.265268 0.730512 0.086 Uiso 1 1 calc R U . . .
C54 C 0.1496(4) 0.1443(5) 0.7740(5) 0.087(2) Uani 1 1 d D . . . .
H54A H 0.127558 0.156053 0.827087 0.104 Uiso 1 1 calc R U . . .
H54B H 0.131984 0.095396 0.777773 0.104 Uiso 1 1 calc R U . . .
N11A N 0.2045(8) 0.6938(9) 0.8061(8) 0.082(3) Uani 0.732(16) 1 d . . P A 1
N12A N 0.1921(7) 0.8329(8) 0.7745(8) 0.105(4) Uani 0.732(16) 1 d . . P A 1
H12A H 0.205988 0.880077 0.746809 0.126 Uiso 0.732(16) 1 calc R U P A 1
C18A C 0.2702(12) 0.7572(12) 0.6669(9) 0.063(4) Uani 0.732(16) 1 d . . P A 1
C19A C 0.2220(9) 0.7603(10) 0.7529(11) 0.073(4) Uani 0.732(16) 1 d . . P A 1
C20A C 0.1553(12) 0.7153(14) 0.8827(9) 0.141(7) Uani 0.732(16) 1 d . . P A 1
H20A H 0.190407 0.693431 0.922441 0.169 Uiso 0.732(16) 1 calc R U P A 1
H20B H 0.103644 0.693741 0.906562 0.169 Uiso 0.732(16) 1 calc R U P A 1
C21A C 0.1313(10) 0.8149(10) 0.8544(9) 0.144(7) Uani 0.732(16) 1 d . . P A 1
H21A H 0.071704 0.837537 0.849680 0.173 Uiso 0.732(16) 1 calc R U P A 1
H21B H 0.139890 0.837717 0.892143 0.173 Uiso 0.732(16) 1 calc R U P A 1
N11B N 0.2358(19) 0.6669(18) 0.8208(18) 0.063(7) Uani 0.268(16) 1 d . U P A 2
N12B N 0.237(3) 0.793(2) 0.8118(12) 0.102(12) Uani 0.268(16) 1 d . . P A 2
H12B H 0.236759 0.845155 0.787578 0.123 Uiso 0.268(16) 1 calc R U P A 2
C18B C 0.272(3) 0.747(2) 0.6915(18) 0.035(7) Uani 0.268(16) 1 d . U P A 2
C19B C 0.250(2) 0.733(2) 0.777(3) 0.059(8) Uani 0.268(16) 1 d . . P A 2
C20B C 0.209(2) 0.670(2) 0.9008(19) 0.082(8) Uani 0.268(16) 1 d . U P A 2
H20C H 0.242787 0.621311 0.934039 0.099 Uiso 0.268(16) 1 calc R U P A 2
H20D H 0.148192 0.667906 0.922702 0.099 Uiso 0.268(16) 1 calc R U P A 2
C21B C 0.221(2) 0.7502(19) 0.9025(19) 0.099(11) Uani 0.268(16) 1 d . U P A 2
H21C H 0.168817 0.781239 0.933553 0.118 Uiso 0.268(16) 1 calc R U P A 2
H21D H 0.269933 0.740593 0.923691 0.118 Uiso 0.268(16) 1 calc R U P A 2
Cl1 Cl 0.93370(17) 0.9631(2) 0.3588(2) 0.1378(10) Uani 1 1 d . . . . .
O1 O 0.9554(12) 1.0289(9) 0.3067(12) 0.319(10) Uani 1 1 d . . . . .
O2 O 0.9391(8) 0.9571(13) 0.4350(8) 0.298(9) Uani 1 1 d . . . . .
O3 O 0.9906(5) 0.8936(11) 0.3346(9) 0.281(8) Uani 1 1 d . . . . .
O4 O 0.8535(6) 0.9604(8) 0.3665(11) 0.274(7) Uani 1 1 d . . . . .
Cl2 Cl 0.72909(15) 0.79601(14) 0.84924(14) 0.1149(10) Uani 0.882(3) 1 d D U P .
.
O5 O 0.7698(4) 0.8414(3) 0.7721(3) 0.178(4) Uani 0.882(3) 1 d D U P . .
O6 O 0.6477(3) 0.8464(4) 0.8779(4) 0.241(6) Uani 0.882(3) 1 d D U P . .
O7 O 0.7803(5) 0.7738(6) 0.9047(4) 0.306(8) Uani 0.882(3) 1 d D U P . .
O8 O 0.7187(5) 0.7229(3) 0.8428(5) 0.251(6) Uani 0.882(3) 1 d D U P . .
Cl3 Cl 0.9550(3) 0.3835(3) 0.88099(19) 0.1721(19) Uani 0.840(3) 1 d D U P . .
O9 O 0.9552(7) 0.4665(3) 0.8324(5) 0.329(9) Uani 0.840(3) 1 d D U P . .
O10 O 1.0023(5) 0.3613(6) 0.9397(4) 0.237(6) Uani 0.840(3) 1 d D U P . .
O11 O 0.9931(7) 0.3285(6) 0.8311(5) 0.353(10) Uani 0.840(3) 1 d D U P . .
O12 O 0.8694(3) 0.3777(8) 0.9211(5) 0.282(7) Uani 0.840(3) 1 d D U P . .
Cl4 Cl 0.7227(2) 0.08790(19) 0.10239(17) 0.1156(11) Uani 0.778(3) 1 d D . P . .
O13 O 0.7125(7) 0.1754(2) 0.0698(5) 0.261(7) Uani 0.778(3) 1 d D U P . .
O14 O 0.7077(7) 0.0665(5) 0.18806(19) 0.250(9) Uani 0.778(3) 1 d D . P . .
O15 O 0.8074(3) 0.0465(6) 0.0694(6) 0.354(12) Uani 0.778(3) 1 d D U P . .
O16 O 0.6634(4) 0.0634(5) 0.0823(4) 0.195(5) Uani 0.778(3) 1 d D U P . .
Cl5 Cl 0.500000 0.500000 0.500000 0.0583(4) Uani 1 2 d DS U P . .
O17A O 0.58783(16) 0.4597(5) 0.4953(5) 0.0606(16) Uani 0.251(5) 1 d D U P B -1
O18A O 0.4733(5) 0.4844(6) 0.4423(4) 0.076(3) Uani 0.251(5) 1 d D U P B -1
O19A O 0.4883(6) 0.58687(12) 0.4835(6) 0.148(10) Uani 0.251(5) 1 d D U P B -1
O20A O 0.4509(5) 0.4688(6) 0.5790(2) 0.069(2) Uani 0.251(5) 1 d D U P B -1
O17B O 0.5742(4) 0.4563(5) 0.5300(6) 0.078(2) Uani 0.249(5) 1 d D U P B -2
O18B O 0.4716(6) 0.4444(5) 0.4810(6) 0.102(6) Uani 0.249(5) 1 d D U P B -2
O19B O 0.5199(6) 0.5649(4) 0.4291(4) 0.070(2) Uani 0.249(5) 1 d D U P B -2
O20B O 0.4346(5) 0.5343(6) 0.5598(4) 0.122(7) Uani 0.249(5) 1 d D U P B -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
Mn1 N2 2.084(5) . ?
Mn1 N4 2.090(4) . ?
Mn1 N6 2.120(4) . ?
Mn1 N9 2.133(5) . ?
Mn1 N1 2.224(4) . ?
Mn1 N7 2.230(5) . ?
Mn2 N13 2.087(5) . ?
Mn2 N10 2.131(6) . ?
Mn2 N25 2.154(6) . ?
Mn2 N11B 2.16(3) . ?
Mn2 N15 2.164(5) . ?
Mn2 N27 2.185(5) . ?
Mn2 N11A 2.194(12) . ?
Mn3 N17 2.108(5) . ?
Mn3 N20 2.169(5) . ?
Mn3 N16 2.173(5) . ?
Mn3 N23 2.174(6) . ?
Mn3 N21 2.191(5) . ?
Mn3 N19 2.220(4) . ?
Mn4 N35 2.146(4) . ?
Mn4 N31 2.153(5) . ?
Mn4 N32 2.180(5) . ?
Mn4 N29 2.195(5) . ?
Mn4 N28 2.198(4) . ?
Mn4 N34 2.203(4) . ?
N1 C1 1.331(6) . ?
N1 C3 1.371(6) . ?
N2 C4 1.289(7) . ?
N2 C5 1.462(7) . ?
N3 C4 1.317(7) . ?
N3 C6 1.496(10) . ?
N4 C9 1.305(6) . ?
N4 C7 1.470(7) . ?
N5 C9 1.317(6) . ?
N5 C8 1.483(6) . ?
N6 C11 1.331(6) . ?
N6 C10 1.376(6) . ?
N7 C15 1.307(8) . ?
N7 C13 1.451(8) . ?
N8 C15 1.318(7) . ?
N8 C14 1.465(9) . ?
N9 C17 1.348(8) . ?
N9 C16 1.394(7) . ?
N10 C17 1.329(9) . ?
N10 C18A 1.353(19) . ?
N10 C18B 1.46(3) . ?
N13 C24 1.302(7) . ?
N13 C22 1.497(7) . ?
N14 C24 1.356(7) . ?
N14 C23 1.453(8) . ?
N15 C26 1.325(7) . ?
N15 C25 1.379(6) . ?
N16 C26 1.339(7) . ?
N16 C27 1.390(6) . ?
N17 C28 1.287(7) . ?
N17 C29 1.474(8) . ?
N18 C28 1.323(7) . ?
N18 C30 1.451(8) . ?
N19 C1 1.327(6) 2_666 ?
N19 C2 1.353(6) 2_666 ?
N20 C47 1.314(8) 2_666 ?
N20 C31 1.356(7) . ?
N21 C32 1.233(9) . ?
N21 C33 1.505(9) . ?
N22 C32 1.371(8) . ?
N22 C34 1.471(8) . ?
N23 C35 1.272(7) . ?
N23 C36 1.495(8) . ?
N24 C35 1.340(8) . ?
N24 C37 1.503(9) . ?
N25 C40 1.263(8) . ?
N25 C38 1.479(8) . ?
N26 C40 1.326(8) . ?
N26 C39 1.441(10) . ?
N27 C42 1.331(7) . ?
N27 C41 1.373(7) . ?
N28 C42 1.323(7) . ?
N28 C43 1.378(6) . ?
N29 C44 1.271(7) . ?
N29 C45 1.489(7) . ?
N30 C44 1.369(7) . ?
N30 C46 1.492(10) . ?
N31 C47 1.350(8) . ?
N31 C48 1.373(7) . ?
N32 C49 1.245(8) . ?
N32 C50 1.494(8) . ?
N33 C49 1.374(7) . ?
N33 C51 1.475(8) . ?
N34 C11 1.332(6) 2_666 ?
N34 C12 1.370(6) 2_666 ?
N35 C52 1.298(6) . ?
N35 C53 1.472(7) . ?
N36 C52 1.341(6) . ?
N36 C54 1.484(6) . ?
C2 C3 1.367(6) . ?
C2 C35 1.485(7) 2_666 ?
C3 C4 1.441(7) . ?
C5 C6 1.410(12) . ?
C7 C8 1.511(9) . ?
C9 C10 1.454(6) . ?
C10 C12 1.373(6) . ?
C12 C52 1.450(6) 2_666 ?
C13 C14 1.524(11) . ?
C15 C16 1.443(8) . ?
C16 C18A 1.279(18) . ?
C16 C18B 1.59(3) . ?
C22 C23 1.501(9) . ?
C24 C25 1.432(8) . ?
C25 C27 1.378(8) . ?
C27 C28 1.444(7) . ?
C29 C30 1.536(10) . ?
C31 C48 1.361(8) 2_666 ?
C31 C32 1.467(9) . ?
C33 C34 1.453(14) . ?
C36 C37 1.489(12) . ?
C38 C39 1.511(14) . ?
C40 C41 1.439(8) . ?
C41 C43 1.372(7) . ?
C43 C44 1.453(8) . ?
C45 C46 1.537(11) . ?
C48 C49 1.480(8) . ?
C50 C51 1.448(12) . ?
C53 C54 1.523(9) . ?
N11A C19A 1.28(2) . ?
N11A C20A 1.471(15) . ?
N12A C19A 1.360(17) . ?
N12A C21A 1.468(16) . ?
C18A C19A 1.51(2) . ?
C20A C21A 1.59(2) . ?
N11B C19B 1.21(5) . ?
N11B C20B 1.38(4) . ?
N12B C19B 1.33(4) . ?
N12B C21B 1.51(4) . ?
C18B C19B 1.42(5) . ?
C20B C21B 1.52(4) . ?
Cl1 O1 1.283(12) . ?
Cl1 O4 1.342(9) . ?
Cl1 O2 1.382(11) . ?
Cl1 O3 1.394(11) . ?
Cl2 O8 1.4121(10) . ?
Cl2 O5 1.4141(9) . ?
Cl2 O6 1.4155(9) . ?
Cl2 O7 1.4168(9) . ?
Cl3 O11 1.4136(9) . ?
Cl3 O9 1.4147(10) . ?
Cl3 O10 1.4151(10) . ?
Cl3 O12 1.4154(10) . ?
Cl4 O16 1.4138(9) . ?
Cl4 O14 1.4147(10) . ?
Cl4 O15 1.4148(9) . ?
Cl4 O13 1.4155(10) . ?
Cl5 O20B 1.4111(9) . ?
Cl5 O18A 1.4112(9) 2_666 ?
Cl5 O18A 1.4112(9) . ?
Cl5 O18B 1.4113(9) 2_666 ?
Cl5 O18B 1.4113(9) . ?
Cl5 O19A 1.4115(10) . ?
Cl5 O20A 1.4121(9) . ?
Cl5 O19B 1.4125(9) . ?
Cl5 O17B 1.4130(9) . ?
Cl5 O17B 1.4130(9) 2_666 ?
Cl5 O17A 1.4131(9) 2_666 ?
Cl5 O17A 1.4131(9) . ?

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
N2 Mn1 N4 90.20(17) . . ?
N2 Mn1 N6 163.30(17) . . ?
N4 Mn1 N6 77.16(16) . . ?
N2 Mn1 N9 99.06(18) . . ?
N4 Mn1 N9 165.79(18) . . ?
N6 Mn1 N9 95.51(16) . . ?
N2 Mn1 N1 75.69(16) . . ?
N4 Mn1 N1 99.78(17) . . ?
N6 Mn1 N1 95.52(14) . . ?
N9 Mn1 N1 92.97(16) . . ?
N2 Mn1 N7 93.11(18) . . ?
N4 Mn1 N7 92.6(2) . . ?
N6 Mn1 N7 98.26(17) . . ?
N9 Mn1 N7 76.29(18) . . ?
N1 Mn1 N7 163.24(18) . . ?
N13 Mn2 N10 165.3(2) . . ?
N13 Mn2 N25 91.3(2) . . ?
N10 Mn2 N25 98.9(2) . . ?
N13 Mn2 N11B 86.7(8) . . ?
N10 Mn2 N11B 80.7(8) . . ?
N25 Mn2 N11B 102.8(8) . . ?
N13 Mn2 N15 76.91(17) . . ?
N10 Mn2 N15 94.68(18) . . ?
N25 Mn2 N15 164.2(2) . . ?
N11B Mn2 N15 87.2(8) . . ?
N13 Mn2 N27 97.74(18) . . ?
N10 Mn2 N27 94.98(18) . . ?
N25 Mn2 N27 76.11(19) . . ?
N11B Mn2 N27 175.4(8) . . ?
N15 Mn2 N27 94.81(16) . . ?
N13 Mn2 N11A 94.8(4) . . ?
N10 Mn2 N11A 75.3(4) . . ?
N25 Mn2 N11A 87.6(4) . . ?
N15 Mn2 N11A 103.7(4) . . ?
N27 Mn2 N11A 159.6(4) . . ?
N17 Mn3 N20 164.0(2) . . ?
N17 Mn3 N16 75.77(17) . . ?
N20 Mn3 N16 96.52(16) . . ?
N17 Mn3 N23 90.4(2) . . ?
N20 Mn3 N23 100.03(18) . . ?
N16 Mn3 N23 160.66(17) . . ?
N17 Mn3 N21 92.8(2) . . ?
N20 Mn3 N21 75.0(2) . . ?
N16 Mn3 N21 102.2(2) . . ?
N23 Mn3 N21 91.8(2) . . ?
N17 Mn3 N19 99.95(19) . . ?
N20 Mn3 N19 94.47(16) . . ?
N16 Mn3 N19 93.79(15) . . ?
N23 Mn3 N19 75.09(16) . . ?
N21 Mn3 N19 161.7(2) . . ?
N35 Mn4 N31 162.54(17) . . ?
N35 Mn4 N32 93.3(2) . . ?
N31 Mn4 N32 75.3(2) . . ?
N35 Mn4 N29 89.26(17) . . ?
N31 Mn4 N29 104.25(17) . . ?
N32 Mn4 N29 92.87(19) . . ?
N35 Mn4 N28 98.79(17) . . ?
N31 Mn4 N28 95.31(16) . . ?
N32 Mn4 N28 163.09(19) . . ?
N29 Mn4 N28 75.63(17) . . ?
N35 Mn4 N34 76.22(15) . . ?
N31 Mn4 N34 92.89(15) . . ?
N32 Mn4 N34 101.44(17) . . ?
N29 Mn4 N34 160.05(17) . . ?
N28 Mn4 N34 92.91(14) . . ?
C1 N1 C3 104.9(4) . . ?
C1 N1 Mn1 142.7(3) . . ?
C3 N1 Mn1 112.3(3) . . ?
C4 N2 C5 107.6(5) . . ?
C4 N2 Mn1 118.0(3) . . ?
C5 N2 Mn1 134.0(5) . . ?
C4 N3 C6 107.7(6) . . ?
C9 N4 C7 107.5(4) . . ?
C9 N4 Mn1 116.9(3) . . ?
C7 N4 Mn1 135.5(4) . . ?
C9 N5 C8 108.7(5) . . ?
C11 N6 C10 105.3(4) . . ?
C11 N6 Mn1 140.6(3) . . ?
C10 N6 Mn1 114.1(3) . . ?
C15 N7 C13 107.8(5) . . ?
C15 N7 Mn1 113.5(4) . . ?
C13 N7 Mn1 138.2(5) . . ?
C15 N8 C14 109.9(6) . . ?
C17 N9 C16 104.4(5) . . ?
C17 N9 Mn1 140.5(4) . . ?
C16 N9 Mn1 114.5(4) . . ?
C17 N10 C18A 100.6(8) . . ?
C17 N10 C18B 115.0(14) . . ?
C17 N10 Mn2 140.9(4) . . ?
C18A N10 Mn2 118.6(7) . . ?
C18B N10 Mn2 103.7(13) . . ?
C24 N13 C22 108.5(5) . . ?
C24 N13 Mn2 116.8(4) . . ?
C22 N13 Mn2 134.7(4) . . ?
C24 N14 C23 109.1(5) . . ?
C26 N15 C25 105.9(4) . . ?
C26 N15 Mn2 141.5(4) . . ?
C25 N15 Mn2 112.5(4) . . ?
C26 N16 C27 104.3(4) . . ?
C26 N16 Mn3 141.9(4) . . ?
C27 N16 Mn3 113.7(3) . . ?
C28 N17 C29 109.1(5) . . ?
C28 N17 Mn3 117.8(4) . . ?
C29 N17 Mn3 132.8(4) . . ?
C28 N18 C30 110.7(5) . . ?
C1 N19 C2 104.4(4) 2_666 2_666 ?
C1 N19 Mn3 140.8(3) 2_666 . ?
C2 N19 Mn3 114.2(3) 2_666 . ?
C47 N20 C31 106.1(5) 2_666 . ?
C47 N20 Mn3 139.6(4) 2_666 . ?
C31 N20 Mn3 114.3(4) . . ?
C32 N21 C33 107.6(7) . . ?
C32 N21 Mn3 116.2(4) . . ?
C33 N21 Mn3 136.1(6) . . ?
C32 N22 C34 106.9(7) . . ?
C35 N23 C36 107.0(5) . . ?
C35 N23 Mn3 116.4(4) . . ?
C36 N23 Mn3 136.3(4) . . ?
C35 N24 C37 106.5(6) . . ?
C40 N25 C38 108.2(7) . . ?
C40 N25 Mn2 115.1(4) . . ?
C38 N25 Mn2 136.5(6) . . ?
C40 N26 C39 111.2(8) . . ?
C42 N27 C41 104.2(4) . . ?
C42 N27 Mn2 142.9(4) . . ?
C41 N27 Mn2 112.3(3) . . ?
C42 N28 C43 104.3(4) . . ?
C42 N28 Mn4 142.6(3) . . ?
C43 N28 Mn4 113.0(3) . . ?
C44 N29 C45 109.1(5) . . ?
C44 N29 Mn4 115.2(4) . . ?
C45 N29 Mn4 134.2(4) . . ?
C44 N30 C46 106.1(6) . . ?
C47 N31 C48 103.7(5) . . ?
C47 N31 Mn4 140.7(4) . . ?
C48 N31 Mn4 115.6(4) . . ?
C49 N32 C50 107.3(6) . . ?
C49 N32 Mn4 116.2(4) . . ?
C50 N32 Mn4 136.5(6) . . ?
C49 N33 C51 104.0(6) . . ?
C11 N34 C12 105.5(4) 2_666 2_666 ?
C11 N34 Mn4 141.9(3) 2_666 . ?
C12 N34 Mn4 112.6(3) 2_666 . ?
C52 N35 C53 109.0(4) . . ?
C52 N35 Mn4 115.9(3) . . ?
C53 N35 Mn4 134.6(4) . . ?
C52 N36 C54 108.0(5) . . ?
N19 C1 N1 113.8(4) 2_666 . ?
N19 C2 C3 109.6(4) 2_666 . ?
N19 C2 C35 114.8(4) 2_666 2_666 ?
C3 C2 C35 135.6(5) . 2_666 ?
C2 C3 N1 107.2(4) . . ?
C2 C3 C4 137.9(5) . . ?
N1 C3 C4 114.9(4) . . ?
N2 C4 N3 114.0(5) . . ?
N2 C4 C3 119.0(5) . . ?
N3 C4 C3 127.0(5) . . ?
C6 C5 N2 107.2(6) . . ?
C5 C6 N3 103.1(6) . . ?
N4 C7 C8 105.5(4) . . ?
N5 C8 C7 102.3(4) . . ?
N4 C9 N5 115.8(4) . . ?
N4 C9 C10 116.7(4) . . ?
N5 C9 C10 127.5(4) . . ?
C12 C10 N6 107.9(4) . . ?
C12 C10 C9 137.0(4) . . ?
N6 C10 C9 115.0(4) . . ?
N6 C11 N34 113.2(4) . 2_666 ?
N34 C12 C10 108.1(4) 2_666 . ?
N34 C12 C52 116.4(4) 2_666 2_666 ?
C10 C12 C52 135.5(4) . 2_666 ?
N7 C13 C14 105.9(7) . . ?
N8 C14 C13 101.4(5) . . ?
N7 C15 N8 114.9(5) . . ?
N7 C15 C16 118.6(5) . . ?
N8 C15 C16 126.4(6) . . ?
C18A C16 N9 104.9(9) . . ?
C18A C16 C15 138.8(9) . . ?
N9 C16 C15 116.3(6) . . ?
N9 C16 C18B 112.5(13) . . ?
C15 C16 C18B 130.6(13) . . ?
N10 C17 N9 113.6(5) . . ?
N13 C22 C23 104.1(5) . . ?
N14 C23 C22 104.4(5) . . ?
N13 C24 N14 113.9(5) . . ?
N13 C24 C25 118.1(5) . . ?
N14 C24 C25 128.0(5) . . ?
C27 C25 N15 107.5(5) . . ?
C27 C25 C24 136.9(5) . . ?
N15 C25 C24 115.6(5) . . ?
N15 C26 N16 113.8(5) . . ?
C25 C27 N16 108.5(5) . . ?
C25 C27 C28 137.2(5) . . ?
N16 C27 C28 114.3(5) . . ?
N17 C28 N18 114.2(5) . . ?
N17 C28 C27 118.2(5) . . ?
N18 C28 C27 127.6(5) . . ?
N17 C29 C30 104.0(6) . . ?
N18 C30 C29 101.9(5) . . ?
N20 C31 C48 108.0(5) . 2_666 ?
N20 C31 C32 115.4(6) . . ?
C48 C31 C32 136.6(5) 2_666 . ?
N21 C32 N22 116.1(6) . . ?
N21 C32 C31 119.1(5) . . ?
N22 C32 C31 124.7(7) . . ?
C34 C33 N21 105.7(8) . . ?
C33 C34 N22 103.7(7) . . ?
N23 C35 N24 117.3(5) . . ?
N23 C35 C2 118.9(5) . 2_666 ?
N24 C35 C2 123.8(5) . 2_666 ?
C37 C36 N23 105.3(6) . . ?
C36 C37 N24 102.8(6) . . ?
N25 C38 C39 105.1(7) . . ?
N26 C39 C38 101.0(7) . . ?
N25 C40 N26 114.2(6) . . ?
N25 C40 C41 120.2(6) . . ?
N26 C40 C41 125.5(7) . . ?
C43 C41 N27 108.5(4) . . ?
C43 C41 C40 136.1(5) . . ?
N27 C41 C40 115.3(5) . . ?
N28 C42 N27 114.9(4) . . ?
C41 C43 N28 108.1(4) . . ?
C41 C43 C44 135.7(5) . . ?
N28 C43 C44 116.1(5) . . ?
N29 C44 N30 116.8(5) . . ?
N29 C44 C43 119.4(5) . . ?
N30 C44 C43 123.8(6) . . ?
N29 C45 C46 103.6(5) . . ?
N30 C46 C45 103.7(5) . . ?
N20 C47 N31 113.3(5) 2_666 . ?
C31 C48 N31 108.9(5) 2_666 . ?
C31 C48 C49 137.7(5) 2_666 . ?
N31 C48 C49 113.4(5) . . ?
N32 C49 N33 116.5(6) . . ?
N32 C49 C48 119.5(5) . . ?
N33 C49 C48 124.0(6) . . ?
C51 C50 N32 104.2(7) . . ?
C50 C51 N33 104.5(6) . . ?
N35 C52 N36 115.3(4) . . ?
N35 C52 C12 118.6(4) . 2_666 ?
N36 C52 C12 126.2(4) . 2_666 ?
N35 C53 C54 104.4(5) . . ?
N36 C54 C53 103.2(5) . . ?
C19A N11A C20A 107.7(13) . . ?
C19A N11A Mn2 114.5(10) . . ?
C20A N11A Mn2 135.8(10) . . ?
C19A N12A C21A 105.6(12) . . ?
C16 C18A N10 115.9(11) . . ?
C16 C18A C19A 132.6(15) . . ?
N10 C18A C19A 111.4(13) . . ?
N11A C19A N12A 118.5(14) . . ?
N11A C19A C18A 119.3(14) . . ?
N12A C19A C18A 122.1(15) . . ?
N11A C20A C21A 102.6(12) . . ?
N12A C21A C20A 102.2(9) . . ?
C19B N11B C20B 109(3) . . ?
C19B N11B Mn2 114(3) . . ?
C20B N11B Mn2 135(2) . . ?
C19B N12B C21B 105(3) . . ?
C19B C18B N10 122(3) . . ?
C19B C18B C16 143(3) . . ?
N10 C18B C16 93.9(16) . . ?
N11B C19B N12B 118(4) . . ?
N11B C19B C18B 118(3) . . ?
N12B C19B C18B 123(3) . . ?
N11B C20B C21B 108(3) . . ?
N12B C21B C20B 98(2) . . ?
O1 Cl1 O4 114.3(11) . . ?
O1 Cl1 O2 110.3(12) . . ?
O4 Cl1 O2 106.9(9) . . ?
O1 Cl1 O3 108.2(12) . . ?
O4 Cl1 O3 108.3(7) . . ?
O2 Cl1 O3 108.7(10) . . ?
O8 Cl2 O5 109.73(9) . . ?
O8 Cl2 O6 109.64(9) . . ?
O5 Cl2 O6 109.43(9) . . ?
O8 Cl2 O7 109.47(9) . . ?
O5 Cl2 O7 109.33(9) . . ?
O6 Cl2 O7 109.22(9) . . ?
O11 Cl3 O9 109.56(9) . . ?
O11 Cl3 O10 109.54(9) . . ?
O9 Cl3 O10 109.46(9) . . ?
O11 Cl3 O12 109.50(9) . . ?
O9 Cl3 O12 109.41(9) . . ?
O10 Cl3 O12 109.35(9) . . ?
O16 Cl4 O14 109.57(9) . . ?
O16 Cl4 O15 109.54(9) . . ?
O14 Cl4 O15 109.46(9) . . ?
O16 Cl4 O13 109.48(9) . . ?
O14 Cl4 O13 109.39(9) . . ?
O15 Cl4 O13 109.39(9) . . ?
O18A Cl5 O18A 180.0(7) 2_666 . ?
O18A Cl5 O18B 32.9(5) 2_666 2_666 ?
O18A Cl5 O18B 147.1(5) . 2_666 ?
O20B Cl5 O18B 109.58(8) . . ?
O18B Cl5 O18B 180.0 2_666 . ?
O18A Cl5 O19A 70.44(8) 2_666 . ?
O18A Cl5 O19A 109.56(8) . . ?
O18A Cl5 O20A 70.48(8) 2_666 . ?
O18A Cl5 O20A 109.52(8) . . ?
O19A Cl5 O20A 109.49(8) . . ?
O20B Cl5 O19B 109.49(8) . . ?
O18B Cl5 O19B 70.51(8) 2_666 . ?
O18B Cl5 O19B 109.49(8) . . ?
O20B Cl5 O17B 109.46(8) . . ?
O18B Cl5 O17B 70.56(8) 2_666 . ?
O18B Cl5 O17B 109.44(8) . . ?
O19B Cl5 O17B 109.36(8) . . ?
O18A Cl5 O17B 127.9(5) 2_666 2_666 ?
O18A Cl5 O17B 52.1(5) . 2_666 ?
O19A Cl5 O17B 70.1(6) . 2_666 ?
O20A Cl5 O17B 92.4(5) . 2_666 ?
O18A Cl5 O17A 109.44(8) 2_666 2_666 ?
O18A Cl5 O17A 70.56(8) . 2_666 ?
O19A Cl5 O17A 70.57(8) . 2_666 ?
O20A Cl5 O17A 70.61(8) . 2_666 ?
O18A Cl5 O17A 70.56(8) 2_666 . ?
O18A Cl5 O17A 109.44(8) . . ?
O19A Cl5 O17A 109.43(8) . . ?
O20A Cl5 O17A 109.39(8) . . ?
O17A Cl5 O17A 180.0(8) 2_666 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 N1 C1 N19 -0.9(6) . . . 2_666 ?
Mn1 N1 C1 N19 -178.4(4) . . . 2_666 ?
N19 C2 C3 N1 -0.2(5) 2_666 . . . ?
C35 C2 C3 N1 -179.2(5) 2_666 . . . ?
N19 C2 C3 C4 179.9(6) 2_666 . . . ?
C35 C2 C3 C4 0.9(11) 2_666 . . . ?
C1 N1 C3 C2 0.7(5) . . . . ?
Mn1 N1 C3 C2 179.0(3) . . . . ?
C1 N1 C3 C4 -179.4(4) . . . . ?
Mn1 N1 C3 C4 -1.1(5) . . . . ?
C5 N2 C4 N3 -1.0(8) . . . . ?
Mn1 N2 C4 N3 -174.5(5) . . . . ?
C5 N2 C4 C3 177.9(5) . . . . ?
Mn1 N2 C4 C3 4.4(7) . . . . ?
C6 N3 C4 N2 -2.6(8) . . . . ?
C6 N3 C4 C3 178.6(6) . . . . ?
C2 C3 C4 N2 177.8(6) . . . . ?
N1 C3 C4 N2 -2.1(7) . . . . ?
C2 C3 C4 N3 -3.4(11) . . . . ?
N1 C3 C4 N3 176.7(6) . . . . ?
C4 N2 C5 C6 4.4(9) . . . . ?
Mn1 N2 C5 C6 176.4(6) . . . . ?
N2 C5 C6 N3 -5.6(10) . . . . ?
C4 N3 C6 C5 5.1(10) . . . . ?
C9 N4 C7 C8 2.6(7) . . . . ?
Mn1 N4 C7 C8 -175.7(4) . . . . ?
C9 N5 C8 C7 2.6(7) . . . . ?
N4 C7 C8 N5 -3.1(7) . . . . ?
C7 N4 C9 N5 -1.0(7) . . . . ?
Mn1 N4 C9 N5 177.7(4) . . . . ?
C7 N4 C9 C10 178.1(5) . . . . ?
Mn1 N4 C9 C10 -3.2(6) . . . . ?
C8 N5 C9 N4 -1.1(7) . . . . ?
C8 N5 C9 C10 179.9(5) . . . . ?
C11 N6 C10 C12 0.2(5) . . . . ?
Mn1 N6 C10 C12 179.0(3) . . . . ?
C11 N6 C10 C9 179.8(4) . . . . ?
Mn1 N6 C10 C9 -1.3(5) . . . . ?
N4 C9 C10 C12 -177.5(5) . . . . ?
N5 C9 C10 C12 1.5(9) . . . . ?
N4 C9 C10 N6 3.0(6) . . . . ?
N5 C9 C10 N6 -178.0(5) . . . . ?
C10 N6 C11 N34 -0.1(5) . . . 2_666 ?
Mn1 N6 C11 N34 -178.4(3) . . . 2_666 ?
N6 C10 C12 N34 -0.2(5) . . . 2_666 ?
C9 C10 C12 N34 -179.7(5) . . . 2_666 ?
N6 C10 C12 C52 180.0(5) . . . 2_666 ?
C9 C10 C12 C52 0.4(10) . . . 2_666 ?
C15 N7 C13 C14 1.9(9) . . . . ?
Mn1 N7 C13 C14 -169.2(5) . . . . ?
C15 N8 C14 C13 0.8(8) . . . . ?
N7 C13 C14 N8 -1.5(9) . . . . ?
C13 N7 C15 N8 -1.5(8) . . . . ?
Mn1 N7 C15 N8 172.1(4) . . . . ?
C13 N7 C15 C16 -179.3(6) . . . . ?
Mn1 N7 C15 C16 -5.8(7) . . . . ?
C14 N8 C15 N7 0.4(8) . . . . ?
C14 N8 C15 C16 178.1(6) . . . . ?
C17 N9 C16 C18A -4.0(10) . . . . ?
Mn1 N9 C16 C18A 168.9(9) . . . . ?
C17 N9 C16 C15 177.4(5) . . . . ?
Mn1 N9 C16 C15 -9.7(6) . . . . ?
C17 N9 C16 C18B 5.2(17) . . . . ?
Mn1 N9 C16 C18B 178.1(16) . . . . ?
N7 C15 C16 C18A -167.4(14) . . . . ?
N8 C15 C16 C18A 15.0(16) . . . . ?
N7 C15 C16 N9 10.5(8) . . . . ?
N8 C15 C16 N9 -167.1(5) . . . . ?
N7 C15 C16 C18B -179(2) . . . . ?
N8 C15 C16 C18B 3(2) . . . . ?
C18A N10 C17 N9 4.4(10) . . . . ?
C18B N10 C17 N9 -5.0(19) . . . . ?
Mn2 N10 C17 N9 -175.5(4) . . . . ?
C16 N9 C17 N10 -0.5(6) . . . . ?
Mn1 N9 C17 N10 -170.3(4) . . . . ?
C24 N13 C22 C23 0.0(7) . . . . ?
Mn2 N13 C22 C23 178.6(4) . . . . ?
C24 N14 C23 C22 -0.3(7) . . . . ?
N13 C22 C23 N14 0.2(7) . . . . ?
C22 N13 C24 N14 -0.2(7) . . . . ?
Mn2 N13 C24 N14 -179.1(4) . . . . ?
C22 N13 C24 C25 179.6(5) . . . . ?
Mn2 N13 C24 C25 0.6(6) . . . . ?
C23 N14 C24 N13 0.3(7) . . . . ?
C23 N14 C24 C25 -179.4(5) . . . . ?
C26 N15 C25 C27 -0.6(5) . . . . ?
Mn2 N15 C25 C27 -177.7(3) . . . . ?
C26 N15 C25 C24 179.3(4) . . . . ?
Mn2 N15 C25 C24 2.1(5) . . . . ?
N13 C24 C25 C27 177.9(6) . . . . ?
N14 C24 C25 C27 -2.4(10) . . . . ?
N13 C24 C25 N15 -1.9(7) . . . . ?
N14 C24 C25 N15 177.8(5) . . . . ?
C25 N15 C26 N16 0.3(6) . . . . ?
Mn2 N15 C26 N16 176.1(4) . . . . ?
C27 N16 C26 N15 0.1(6) . . . . ?
Mn3 N16 C26 N15 -178.4(4) . . . . ?
N15 C25 C27 N16 0.6(5) . . . . ?
C24 C25 C27 N16 -179.2(5) . . . . ?
N15 C25 C27 C28 -179.7(6) . . . . ?
C24 C25 C27 C28 0.5(11) . . . . ?
C26 N16 C27 C25 -0.5(5) . . . . ?
Mn3 N16 C27 C25 178.6(3) . . . . ?
C26 N16 C27 C28 179.8(4) . . . . ?
Mn3 N16 C27 C28 -1.2(5) . . . . ?
C29 N17 C28 N18 0.5(8) . . . . ?
Mn3 N17 C28 N18 175.2(4) . . . . ?
C29 N17 C28 C27 179.9(5) . . . . ?
Mn3 N17 C28 C27 -5.4(7) . . . . ?
C30 N18 C28 N17 -3.0(8) . . . . ?
C30 N18 C28 C27 177.6(6) . . . . ?
C25 C27 C28 N17 -175.3(6) . . . . ?
N16 C27 C28 N17 4.3(7) . . . . ?
C25 C27 C28 N18 4.0(10) . . . . ?
N16 C27 C28 N18 -176.3(5) . . . . ?
C28 N17 C29 C30 2.0(8) . . . . ?
Mn3 N17 C29 C30 -171.6(5) . . . . ?
C28 N18 C30 C29 3.9(8) . . . . ?
N17 C29 C30 N18 -3.4(8) . . . . ?
C47 N20 C31 C48 0.6(6) 2_666 . . 2_666 ?
Mn3 N20 C31 C48 179.0(3) . . . 2_666 ?
C47 N20 C31 C32 -179.6(5) 2_666 . . . ?
Mn3 N20 C31 C32 -1.2(6) . . . . ?
C33 N21 C32 N22 0.6(11) . . . . ?
Mn3 N21 C32 N22 -177.4(6) . . . . ?
C33 N21 C32 C31 176.8(7) . . . . ?
Mn3 N21 C32 C31 -1.2(9) . . . . ?
C34 N22 C32 N21 -0.1(11) . . . . ?
C34 N22 C32 C31 -176.1(8) . . . . ?
N20 C31 C32 N21 1.7(9) . . . . ?
C48 C31 C32 N21 -178.6(7) 2_666 . . . ?
N20 C31 C32 N22 177.5(7) . . . . ?
C48 C31 C32 N22 -2.7(12) 2_666 . . . ?
C32 N21 C33 C34 -0.9(12) . . . . ?
Mn3 N21 C33 C34 176.6(7) . . . . ?
N21 C33 C34 N22 0.8(12) . . . . ?
C32 N22 C34 C33 -0.5(12) . . . . ?
C36 N23 C35 N24 -4.4(8) . . . . ?
Mn3 N23 C35 N24 170.7(5) . . . . ?
C36 N23 C35 C2 176.9(5) . . . 2_666 ?
Mn3 N23 C35 C2 -8.0(7) . . . 2_666 ?
C37 N24 C35 N23 -2.4(9) . . . . ?
C37 N24 C35 C2 176.2(7) . . . 2_666 ?
C35 N23 C36 C37 9.4(8) . . . . ?
Mn3 N23 C36 C37 -164.3(6) . . . . ?
N23 C36 C37 N24 -10.2(10) . . . . ?
C35 N24 C37 C36 8.0(10) . . . . ?
C40 N25 C38 C39 -3.7(10) . . . . ?
Mn2 N25 C38 C39 171.8(7) . . . . ?
C40 N26 C39 C38 -3.1(12) . . . . ?
N25 C38 C39 N26 3.9(11) . . . . ?
C38 N25 C40 N26 1.9(9) . . . . ?
Mn2 N25 C40 N26 -174.7(6) . . . . ?
C38 N25 C40 C41 -178.7(6) . . . . ?
Mn2 N25 C40 C41 4.7(8) . . . . ?
C39 N26 C40 N25 0.9(11) . . . . ?
C39 N26 C40 C41 -178.4(9) . . . . ?
C42 N27 C41 C43 0.6(6) . . . . ?
Mn2 N27 C41 C43 -172.1(3) . . . . ?
C42 N27 C41 C40 -177.1(5) . . . . ?
Mn2 N27 C41 C40 10.2(6) . . . . ?
N25 C40 C41 C43 172.8(6) . . . . ?
N26 C40 C41 C43 -7.9(12) . . . . ?
N25 C40 C41 N27 -10.3(9) . . . . ?
N26 C40 C41 N27 169.0(7) . . . . ?
C43 N28 C42 N27 0.0(6) . . . . ?
Mn4 N28 C42 N27 176.2(4) . . . . ?
C41 N27 C42 N28 -0.4(6) . . . . ?
Mn2 N27 C42 N28 168.5(4) . . . . ?
N27 C41 C43 N28 -0.7(6) . . . . ?
C40 C41 C43 N28 176.3(6) . . . . ?
N27 C41 C43 C44 176.5(6) . . . . ?
C40 C41 C43 C44 -6.5(12) . . . . ?
C42 N28 C43 C41 0.4(6) . . . . ?
Mn4 N28 C43 C41 -177.1(3) . . . . ?
C42 N28 C43 C44 -177.4(5) . . . . ?
Mn4 N28 C43 C44 5.1(6) . . . . ?
C45 N29 C44 N30 -1.7(8) . . . . ?
Mn4 N29 C44 N30 -169.5(5) . . . . ?
C45 N29 C44 C43 176.8(5) . . . . ?
Mn4 N29 C44 C43 9.0(7) . . . . ?
C46 N30 C44 N29 6.6(9) . . . . ?
C46 N30 C44 C43 -171.8(6) . . . . ?
C41 C43 C44 N29 173.3(6) . . . . ?
N28 C43 C44 N29 -9.7(7) . . . . ?
C41 C43 C44 N30 -8.3(10) . . . . ?
N28 C43 C44 N30 168.7(6) . . . . ?
C44 N29 C45 C46 -3.8(7) . . . . ?
Mn4 N29 C45 C46 160.7(5) . . . . ?
C44 N30 C46 C45 -8.2(8) . . . . ?
N29 C45 C46 N30 7.2(8) . . . . ?
C48 N31 C47 N20 -0.7(6) . . . 2_666 ?
Mn4 N31 C47 N20 -176.7(4) . . . 2_666 ?
C47 N31 C48 C31 0.3(6) . . . 2_666 ?
Mn4 N31 C48 C31 177.5(3) . . . 2_666 ?
C47 N31 C48 C49 179.8(4) . . . . ?
Mn4 N31 C48 C49 -3.0(5) . . . . ?
C50 N32 C49 N33 -0.7(8) . . . . ?
Mn4 N32 C49 N33 176.4(4) . . . . ?
C50 N32 C49 C48 178.6(5) . . . . ?
Mn4 N32 C49 C48 -4.3(7) . . . . ?
C51 N33 C49 N32 -10.9(8) . . . . ?
C51 N33 C49 C48 169.8(6) . . . . ?
C31 C48 C49 N32 -175.8(6) 2_666 . . . ?
N31 C48 C49 N32 5.0(7) . . . . ?
C31 C48 C49 N33 3.4(10) 2_666 . . . ?
N31 C48 C49 N33 -175.8(5) . . . . ?
C49 N32 C50 C51 12.3(8) . . . . ?
Mn4 N32 C50 C51 -164.0(5) . . . . ?
N32 C50 C51 N33 -17.9(9) . . . . ?
C49 N33 C51 C50 17.6(8) . . . . ?
C53 N35 C52 N36 1.1(7) . . . . ?
Mn4 N35 C52 N36 174.3(4) . . . . ?
C53 N35 C52 C12 -179.6(5) . . . 2_666 ?
Mn4 N35 C52 C12 -6.4(6) . . . 2_666 ?
C54 N36 C52 N35 -3.3(7) . . . . ?
C54 N36 C52 C12 177.6(5) . . . 2_666 ?
C52 N35 C53 C54 1.4(7) . . . . ?
Mn4 N35 C53 C54 -170.0(5) . . . . ?
C52 N36 C54 C53 3.8(7) . . . . ?
N35 C53 C54 N36 -3.1(7) . . . . ?
N9 C16 C18A N10 7.5(16) . . . . ?
C15 C16 C18A N10 -174.4(7) . . . . ?
N9 C16 C18A C19A -176.4(16) . . . . ?
C15 C16 C18A C19A 2(3) . . . . ?
C17 N10 C18A C16 -7.5(15) . . . . ?
Mn2 N10 C18A C16 172.5(9) . . . . ?
C17 N10 C18A C19A 175.6(11) . . . . ?
Mn2 N10 C18A C19A -4.4(16) . . . . ?
C20A N11A C19A N12A -2(2) . . . . ?
Mn2 N11A C19A N12A 164.6(10) . . . . ?
C20A N11A C19A C18A -178.1(13) . . . . ?
Mn2 N11A C19A C18A -11.5(18) . . . . ?
C21A N12A C19A N11A -10.3(19) . . . . ?
C21A N12A C19A C18A 165.6(15) . . . . ?
C16 C18A C19A N11A -165.5(17) . . . . ?
N10 C18A C19A N11A 11(2) . . . . ?
C16 C18A C19A N12A 19(3) . . . . ?
N10 C18A C19A N12A -165.2(13) . . . . ?
C19A N11A C20A C21A 12.3(17) . . . . ?
Mn2 N11A C20A C21A -150.2(12) . . . . ?
C19A N12A C21A C20A 16.4(16) . . . . ?
N11A C20A C21A N12A -17.3(17) . . . . ?
C17 N10 C18B C19B -167(3) . . . . ?
Mn2 N10 C18B C19B 7(4) . . . . ?
C17 N10 C18B C16 7(2) . . . . ?
Mn2 N10 C18B C16 -179.1(12) . . . . ?
N9 C16 C18B C19B 164(5) . . . . ?
C15 C16 C18B C19B -7(6) . . . . ?
N9 C16 C18B N10 -7(2) . . . . ?
C15 C16 C18B N10 -178.0(7) . . . . ?
C20B N11B C19B N12B -2(4) . . . . ?
Mn2 N11B C19B N12B 164(3) . . . . ?
C20B N11B C19B C18B -175(3) . . . . ?
Mn2 N11B C19B C18B -9(4) . . . . ?
C21B N12B C19B N11B 10(5) . . . . ?
C21B N12B C19B C18B -177(3) . . . . ?
N10 C18B C19B N11B 1(5) . . . . ?
C16 C18B C19B N11B -168(4) . . . . ?
N10 C18B C19B N12B -171(3) . . . . ?
C16 C18B C19B N12B 19(7) . . . . ?
C19B N11B C20B C21B -8(4) . . . . ?
Mn2 N11B C20B C21B -169(2) . . . . ?
C19B N12B C21B C20B -13(4) . . . . ?
N11B C20B C21B N12B 13(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C20A^a H20A^a O12 0.98 2.65 3.288(19) 122.8 2_667 yes
N12A^a H12A^a N8 0.87 2.38 3.073(12) 136.4 . yes
C21B^b H21D^b O13 0.98 1.66 2.27(3) 116.2 2_666 yes
N12B^b H12B^b O14 0.87 2.30 2.95(2) 130.7 2_666 yes
N12B^b H12B^b N8 0.87 2.69 3.35(2) 132.9 . yes
C1 H1 O19A^a 0.94 2.53 3.188(10) 127.0 . yes
C1 H1 O19B^b 0.94 2.14 2.971(9) 146.1 . yes
N5 H5 O14 0.87 2.51 3.141(8) 130.3 1_565 yes
N5 H5 O16 0.87 2.60 3.065(8) 114.1 1_565 yes
N5 H5 N36 0.87 2.43 3.154(7) 140.5 2_666 yes
C5 H5A O2 0.98 2.45 3.329(13) 149.3 2_676 yes
C6 H6A O5 0.98 2.58 3.354(11) 136.4 2_676 yes
C42 H42 O20A^a 0.94 2.26 3.088(8) 145.8 . yes
N14 H14 O7 0.87 2.57 3.080(10) 118.1 2_667 yes
N14 H14 N18 0.87 2.54 3.245(8) 138.9 . yes
C17 H17 O17A^a 0.94 2.37 3.205(9) 148.6 2_666 yes
C17 H17 O20B^b 0.94 2.39 2.989(8) 121.5 . yes
N18 H18 N14 0.87 2.52 3.245(8) 141.4 . yes
C53 H53B O11 0.98 2.30 3.226(8) 156.8 1_455 yes
C47 H47 O17A^a 0.94 2.57 3.422(10) 150.6 2_666 yes
C47 H47 O18A^a 0.94 2.56 3.075(8) 114.6 . yes
C47 H47 O17B^b 0.94 2.36 3.166(9) 143.0 2_666 yes
N3 H3 N24 0.87 2.46 3.163(9) 138.3 2_666 yes
N8 H8 N12A^a 0.87 2.44 3.073(12) 130.0 . yes
N8 H8 N12B^b 0.87 2.60 3.35(2) 145.1 . yes
N8 H8 O14 0.87 2.29 3.019(7) 141.1 2_666 yes
C11 H11 O19A^a 0.94 2.45 3.016(7) 119.0 . yes
C11 H11 O18B^b 0.94 2.32 3.035(7) 132.7 2_666 yes
N22 H22 O8 0.87 2.33 2.966(7) 130.4 . yes
N22 H22 N33 0.87 2.39 3.120(10) 141.9 2_666 yes
C22 H22A O10 0.98 2.57 3.359(10) 137.8 1_455 yes
N24 H24 O3 0.87 2.32 2.952(10) 129.3 2_766 yes
N24 H24 N3 0.87 2.45 3.163(9) 139.9 2_666 yes
N30 H30 O9 0.87 2.60 3.041(12) 112.3 1_455 yes
N30 H30 N26 0.87 2.37 3.079(10) 138.5 . yes
C29 H29A O13 0.98 2.41 3.095(11) 126.2 1_556 yes
C26 H26 O18A^a 0.94 2.39 3.099(9) 132.5 2_666 yes
C26 H26 O20B^b 0.94 2.51 3.104(10) 121.5 . yes
N26 H26A N30 0.87 2.37 3.079(10) 138.6 . yes
N33 H33 O8 0.87 2.46 3.197(9) 142.6 2_666 yes
N33 H33 N22 0.87 2.41 3.120(10) 139.4 2_666 yes
N36 H36 O14 0.87 2.55 3.163(10) 127.9 2_656 yes
N36 H36 N5 0.87 2.43 3.154(6) 141.5 2_666 yes
C36 H36A O12 0.98 2.55 3.288(12) 131.8 . yes

_refine_diff_density_max         1.501
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.117




####################################################################### 
# 
# 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_190523_hk_niimh2bizncs_0m_a_sq_2
_database_code_depnum_ccdc_archive 'CCDC 2036135'
loop_
_audit_author_name
_audit_author_address
'Hajime Kamebuchi'
;Nihon University
Japan
;
_audit_update_record             
;
2021-03-11 deposited with the CCDC.	2021-03-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C117 H172 Cl4 N72 Ni8 O28.50'
_chemical_formula_weight         3654.74

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'
N N 0.0061 0.0033 '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'

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

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   14.6815(6)
_cell_length_b                   17.6981(8)
_cell_length_c                   17.8221(8)
_cell_angle_alpha                111.0820(10)
_cell_angle_beta                 98.5660(10)
_cell_angle_gamma                106.1330(10)
_cell_volume                     3987.4(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    7255
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      25.65

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_F_000             1898
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.005
_exptl_absorpt_coefficient_mu    1.080
_shelx_estimated_absorpt_T_min   0.909
_shelx_estimated_absorpt_T_max   0.995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6015
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus tube'
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 7.407
_diffrn_reflns_number            41999
_diffrn_reflns_av_unetI/netI     0.0755
_diffrn_reflns_av_R_equivalents  0.0710
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.190
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_full        25.027
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             13976
_reflns_number_gt                8445
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 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.

The structure was refined after PLATON/SQUEEZE procedure due to the presence of many heavily disordered solvent molecules. Details of the PLATON/SQUEEZE results are given at the end of this cif file.

One may find the values of Ueq and Uvol strange for Cl1-2 and O1-8. The solvent molecules around the complex may have originally been involved in the hydrogen bonding with the ClO4- ions, but they have been removed by the PLATON/SQUEEZE procedure due to their heavy disorder. This may have been reflected in the values of Ueq and Uvol.
;

_computing_data_collection       'Bruker Instrument Service (Bruker AXS, 2018)'
_computing_cell_refinement       'APEX3 (Bruker AXS, 2018)'
_computing_data_reduction        'SAINT (Bruker AXS, 2013)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    'APEX3 (Bruker AXS,2018)'
_computing_publication_material  'APEX3 (Bruker AXS,2018)'
_refine_special_details          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)+(0.1103P)²+12.7373P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13976
_refine_ls_number_parameters     938
_refine_ls_number_restraints     50
_refine_ls_R_factor_all          0.1263
_refine_ls_R_factor_gt           0.0765
_refine_ls_wR_factor_ref         0.2393
_refine_ls_wR_factor_gt          0.1995
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.79923(6) 0.68927(5) 0.78946(5) 0.0360(2) Uani 1 1 d . . . . .
Ni2 Ni 0.85423(6) 0.64971(5) 0.42622(5) 0.0343(2) Uani 1 1 d . . . . .
Ni3 Ni 0.44961(6) 0.71541(5) 0.35063(5) 0.0356(2) Uani 1 1 d . . . . .
Ni4 Ni 0.60752(6) 0.24735(5) 0.28921(5) 0.0333(2) Uani 1 1 d . . . . .
N1 N 0.7806(4) 0.7207(4) 0.9095(3) 0.0412(14) Uani 1 1 d . . . . .
N2 N 0.7027(4) 0.7635(5) 0.9986(4) 0.066(2) Uani 1 1 d D . . . .
H2 H 0.655611 0.780017 1.016445 0.079 Uiso 1 1 calc DR U . . .
N3 N 0.6653(4) 0.7107(3) 0.7728(3) 0.0355(13) Uani 1 1 d . . . . .
N4 N 0.4017(4) 0.7751(4) 0.8363(3) 0.0418(14) Uani 1 1 d . . . . .
N5 N 0.4900(5) 0.8113(6) 0.9598(4) 0.085(3) Uani 1 1 d D . . . .
H5 H 0.539716 0.814974 0.996958 0.102 Uiso 1 1 calc DR U . . .
N6 N 0.5247(4) 0.7331(3) 0.7457(3) 0.0351(12) Uani 1 1 d . . . . .
N7 N 0.9195(4) 0.6531(4) 0.8160(4) 0.0445(14) Uani 1 1 d . . . . .
N8 N 0.9757(5) 0.5486(4) 0.8040(5) 0.082(3) Uani 1 1 d . . . . .
H8 H 0.972494 0.494452 0.787417 0.099 Uiso 1 1 calc DR U . . .
N9 N 0.7292(4) 0.5560(4) 0.7490(3) 0.0376(13) Uani 1 1 d . . . . .
N10 N 0.6878(4) 0.2767(4) 0.6894(3) 0.0420(14) Uani 1 1 d . . . . .
N11 N 0.8433(5) 0.3472(4) 0.7710(5) 0.066(2) Uani 1 1 d . . . . .
H11 H 0.899301 0.391282 0.798827 0.080 Uiso 1 1 calc DR U . . .
N12 N 0.6407(4) 0.4157(3) 0.7045(3) 0.0357(13) Uani 1 1 d . . . . .
N13 N 0.8824(4) 0.8190(4) 0.8224(3) 0.0415(14) Uani 1 1 d . . . . .
N14 N 0.9519(5) 0.9206(4) 0.7850(3) 0.0606(19) Uani 1 1 d . . . . .
H14 H 0.965283 0.943792 0.749908 0.073 Uiso 1 1 calc DR U . . .
N15 N 0.8213(4) 0.6830(3) 0.6734(3) 0.0340(12) Uani 1 1 d . . . . .
N16 N 0.9250(4) 0.7858(3) 0.4906(4) 0.0446(15) Uani 1 1 d . . . . .
N17 N 0.9098(5) 0.8986(4) 0.5897(3) 0.067(2) Uani 1 1 d . . . . .
H17 H 0.897605 0.927116 0.636556 0.080 Uiso 1 1 calc DR U . . .
N18 N 0.8377(4) 0.6695(3) 0.5462(3) 0.0323(12) Uani 1 1 d . . . . .
N19 N 0.8572(4) 0.6491(4) 0.3087(3) 0.0415(14) Uani 1 1 d . . . . .
N20 N 0.7874(6) 0.6474(6) 0.1938(4) 0.095(3) Uani 1 1 d D U . . .
H20C H 0.742405 0.653531 0.160242 0.114 Uiso 1 1 calc DR U . . .
N21 N 0.7214(4) 0.6674(3) 0.3907(3) 0.0358(12) Uani 1 1 d . . . . .
N22 N 0.4846(4) 0.7128(4) 0.2400(3) 0.0386(13) Uani 1 1 d . . . . .
N23 N 0.5883(5) 0.7145(5) 0.1690(4) 0.068(2) Uani 1 1 d D U . . .
H23A H 0.641870 0.708526 0.155331 0.082 Uiso 1 1 calc DR U . . .
N24 N 0.5822(4) 0.6935(3) 0.3661(3) 0.0351(12) Uani 1 1 d . . . . .
N25 N 0.5267(4) 0.8503(4) 0.4146(3) 0.0418(14) Uani 1 1 d . . . . .
N26 N 0.6115(4) 0.9605(4) 0.5396(4) 0.0593(18) Uani 1 1 d . . . . .
H26 H 0.631666 0.987512 0.594574 0.071 Uiso 1 1 calc DR U . . .
N27 N 0.4395(4) 0.7363(3) 0.4712(3) 0.0354(12) Uani 1 1 d . . . . .
N28 N 0.4648(4) 0.8844(3) 0.7440(3) 0.0387(13) Uani 1 1 d . . . . .
N29 N 0.5288(5) 0.9882(4) 0.7069(4) 0.072(2) Uani 1 1 d . . . . .
H29 H 0.548756 1.010738 0.672904 0.086 Uiso 1 1 calc DR U . . .
N30 N 0.4118(4) 0.7503(3) 0.5952(3) 0.0342(12) Uani 1 1 d . . . . .
N31 N 0.9816(4) 0.6122(3) 0.4350(3) 0.0382(13) Uani 1 1 d . . . . .
N32 N 1.0363(4) 0.5059(3) 0.3971(4) 0.0580(18) Uani 1 1 d . . . . .
H32A H 1.031421 0.451282 0.374299 0.070 Uiso 1 1 calc DR U . . .
N33 N 0.7901(4) 0.5171(3) 0.3811(3) 0.0350(12) Uani 1 1 d . . . . .
N34 N 0.7457(4) 0.2361(3) 0.3082(3) 0.0359(12) Uani 1 1 d . . . . .
N35 N 0.9070(4) 0.2932(3) 0.3514(4) 0.0586(18) Uani 1 1 d . . . . .
H35 H 0.965341 0.334792 0.370437 0.070 Uiso 1 1 calc DR U . . .
N36 N 0.7011(4) 0.3761(3) 0.3381(3) 0.0347(12) Uani 1 1 d . . . . .
C1 C 0.8362(6) 0.7323(6) 0.9910(4) 0.054(2) Uani 1 1 d . . . . .
H1A H 0.902496 0.777829 1.009773 0.065 Uiso 1 1 calc R U . . .
H1B H 0.844164 0.677507 0.987440 0.065 Uiso 1 1 calc R U . . .
C2 C 0.7763(7) 0.7591(8) 1.0509(5) 0.081(3) Uani 1 1 d D . . . .
H2A H 0.751146 0.714969 1.071953 0.098 Uiso 1 1 calc R U . . .
H2AB H 0.814378 0.815968 1.098665 0.098 Uiso 1 1 calc R U . . .
C3 C 0.7046(5) 0.7416(4) 0.9185(4) 0.0409(16) Uani 1 1 d . . . . .
C4 C 0.6396(5) 0.7377(4) 0.8458(4) 0.0379(15) Uani 1 1 d . . . . .
C5 C 0.5951(5) 0.7100(4) 0.7167(4) 0.0354(15) Uani 1 1 d . . . . .
H5A H 0.595159 0.694067 0.659796 0.043 Uiso 1 1 calc R U . . .
C6 C 0.5516(5) 0.7521(4) 0.8295(4) 0.0375(15) Uani 1 1 d . . . . .
C7 C 0.4848(5) 0.7789(5) 0.8760(4) 0.0420(17) Uani 1 1 d . . . . .
C8 C 0.3461(6) 0.8031(6) 0.8963(4) 0.059(2) Uani 1 1 d . . . . .
H8A H 0.286972 0.753632 0.887273 0.071 Uiso 1 1 calc R U . . .
H8B H 0.324595 0.849150 0.889679 0.071 Uiso 1 1 calc R U . . .
C9 C 0.4160(7) 0.8375(8) 0.9834(5) 0.091(4) Uani 1 1 d D . . . .
H9A H 0.437815 0.901369 1.013529 0.109 Uiso 1 1 calc R U . . .
H9AB H 0.386565 0.809893 1.017866 0.109 Uiso 1 1 calc R U . . .
C10 C 1.0284(6) 0.6936(6) 0.8426(6) 0.064(2) Uani 1 1 d . . . . .
H10A H 1.051862 0.740743 0.899874 0.077 Uiso 1 1 calc R U . . .
H10B H 1.052106 0.717695 0.803848 0.077 Uiso 1 1 calc R U . . .
C11 C 1.0641(6) 0.6193(6) 0.8398(6) 0.076(3) Uani 1 1 d . . . . .
H11A H 1.110124 0.612820 0.804674 0.092 Uiso 1 1 calc R U . . .
H11B H 1.096552 0.628016 0.896645 0.092 Uiso 1 1 calc R U . . .
C12 C 0.8963(5) 0.5711(5) 0.7972(4) 0.0421(17) Uani 1 1 d . . . . .
C13 C 0.7918(5) 0.5153(4) 0.7641(4) 0.0357(15) Uani 1 1 d . . . . .
C14 C 0.6400(5) 0.4937(4) 0.7136(4) 0.0375(15) Uani 1 1 d . . . . .
H14A H 0.581803 0.503850 0.696583 0.045 Uiso 1 1 calc R U . . .
C15 C 0.7390(5) 0.4295(4) 0.7376(4) 0.0385(16) Uani 1 1 d . . . . .
C16 C 0.7569(5) 0.3513(5) 0.7327(4) 0.0449(17) Uani 1 1 d . . . . .
C17 C 0.7269(7) 0.2108(5) 0.6955(6) 0.064(2) Uani 1 1 d . . . . .
H17A H 0.732746 0.174919 0.640467 0.076 Uiso 1 1 calc R U . . .
H17B H 0.682982 0.172444 0.714511 0.076 Uiso 1 1 calc R U . . .
C18 C 0.8260(7) 0.2592(7) 0.7577(9) 0.104(4) Uani 1 1 d . . . . .
H18A H 0.825341 0.252204 0.810290 0.125 Uiso 1 1 calc R U . . .
H18B H 0.876861 0.239230 0.735040 0.125 Uiso 1 1 calc R U . . .
C19 C 0.9231(6) 0.9007(5) 0.8987(4) 0.055(2) Uani 1 1 d . . . . .
H19A H 0.966269 0.895413 0.943407 0.066 Uiso 1 1 calc R U . . .
H19B H 0.869631 0.917572 0.919520 0.066 Uiso 1 1 calc R U . . .
C20 C 0.9825(7) 0.9668(5) 0.8708(5) 0.068(3) Uani 1 1 d . . . . .
H20A H 0.965569 1.019809 0.888327 0.082 Uiso 1 1 calc R U . . .
H20B H 1.054426 0.983113 0.893168 0.082 Uiso 1 1 calc R U . . .
C21 C 0.8991(5) 0.8358(4) 0.7608(4) 0.0427(17) Uani 1 1 d . . . . .
C22 C 0.8642(5) 0.7645(4) 0.6778(4) 0.0353(15) Uani 1 1 d . . . . .
C23 C 0.8079(5) 0.6295(4) 0.5938(4) 0.0343(15) Uani 1 1 d . . . . .
H23 H 0.779522 0.568119 0.572955 0.041 Uiso 1 1 calc R U . . .
C24 C 0.8709(5) 0.7550(4) 0.5988(4) 0.0379(15) Uani 1 1 d . . . . .
C25 C 0.9056(5) 0.8153(4) 0.5629(4) 0.0441(17) Uani 1 1 d . . . . .
C26 C 0.9523(7) 0.8589(5) 0.4667(5) 0.066(2) Uani 1 1 d . . . . .
H26A H 0.910086 0.843289 0.410623 0.079 Uiso 1 1 calc R U . . .
H26B H 1.022148 0.875550 0.465796 0.079 Uiso 1 1 calc R U . . .
C27 C 0.9359(7) 0.9335(5) 0.5340(5) 0.068(3) Uani 1 1 d . . . . .
H27A H 0.996885 0.985664 0.561553 0.082 Uiso 1 1 calc R U . . .
H27B H 0.882209 0.948784 0.509908 0.082 Uiso 1 1 calc R U . . .
C28 C 0.9176(7) 0.6327(7) 0.2503(5) 0.075(3) Uani 1 1 d . . . . .
H28A H 0.929518 0.578361 0.242682 0.090 Uiso 1 1 calc R U . . .
H28B H 0.982116 0.680977 0.272687 0.090 Uiso 1 1 calc R U . . .
C29 C 0.8621(9) 0.6249(10) 0.1669(7) 0.119(5) Uani 1 1 d D U . . .
H29A H 0.901318 0.666266 0.148137 0.143 Uiso 1 1 calc R U . . .
H29B H 0.838489 0.565112 0.122379 0.143 Uiso 1 1 calc R U . . .
C30 C 0.7827(6) 0.6604(5) 0.2731(4) 0.0440(17) Uani 1 1 d . . . . .
C31 C 0.7081(5) 0.6733(4) 0.3157(4) 0.0373(15) Uani 1 1 d . . . . .
C32 C 0.6440(5) 0.6796(4) 0.4175(4) 0.0367(15) Uani 1 1 d . . . . .
H32 H 0.634229 0.678370 0.468663 0.044 Uiso 1 1 calc R U . . .
C33 C 0.6223(5) 0.6903(4) 0.3007(4) 0.0348(15) Uani 1 1 d . . . . .
C34 C 0.5675(5) 0.7050(4) 0.2356(4) 0.0378(16) Uani 1 1 d . . . . .
C35 C 0.4435(6) 0.7257(6) 0.1677(5) 0.054(2) Uani 1 1 d . . . . .
H35A H 0.427448 0.779099 0.185784 0.064 Uiso 1 1 calc R U . . .
H35B H 0.382826 0.675736 0.130530 0.064 Uiso 1 1 calc R U . . .
C36 C 0.5238(6) 0.7337(6) 0.1227(5) 0.062(2) Uani 1 1 d D U . . .
H36A H 0.499680 0.691327 0.063239 0.074 Uiso 1 1 calc R U . . .
H36B H 0.552478 0.793131 0.126583 0.074 Uiso 1 1 calc R U . . .
C37 C 0.6028(6) 0.9150(5) 0.4002(5) 0.059(2) Uani 1 1 d . . . . .
H37A H 0.572415 0.930833 0.357424 0.071 Uiso 1 1 calc R U . . .
H37B H 0.653376 0.891659 0.381262 0.071 Uiso 1 1 calc R U . . .
C38 C 0.6485(7) 0.9937(5) 0.4854(5) 0.061(2) Uani 1 1 d . . . . .
H38A H 0.721510 1.014188 0.500615 0.073 Uiso 1 1 calc R U . . .
H38B H 0.627070 1.042100 0.485542 0.073 Uiso 1 1 calc R U . . .
C39 C 0.5380(5) 0.8783(4) 0.4939(4) 0.0428(17) Uani 1 1 d . . . . .
C40 C 0.4831(5) 0.8227(4) 0.5269(4) 0.0408(16) Uani 1 1 d . . . . .
C41 C 0.3984(5) 0.6968(4) 0.5158(4) 0.0366(15) Uani 1 1 d . . . . .
H41 H 0.362842 0.636077 0.493094 0.044 Uiso 1 1 calc R U . . .
C42 C 0.4632(5) 0.8301(4) 0.6020(4) 0.0410(16) Uani 1 1 d . . . . .
C43 C 0.4891(5) 0.9019(4) 0.6843(4) 0.0425(17) Uani 1 1 d . . . . .
C44 C 0.5011(6) 0.9671(4) 0.8198(4) 0.0511(19) Uani 1 1 d . . . . .
H44A H 0.556843 0.969539 0.860589 0.061 Uiso 1 1 calc R U . . .
H44B H 0.447877 0.973987 0.846703 0.061 Uiso 1 1 calc R U . . .
C45 C 0.5347(7) 1.0373(5) 0.7888(5) 0.060(2) Uani 1 1 d . . . . .
H45A H 0.490193 1.070635 0.792254 0.072 Uiso 1 1 calc R U . . .
H45B H 0.603088 1.077683 0.820728 0.072 Uiso 1 1 calc R U . . .
C46 C 1.0884(5) 0.6496(5) 0.4435(5) 0.0475(18) Uani 1 1 d . . . . .
H46A H 1.123344 0.696277 0.500402 0.057 Uiso 1 1 calc R U . . .
H46B H 1.098646 0.674067 0.402127 0.057 Uiso 1 1 calc R U . . .
C47 C 1.1260(5) 0.5743(5) 0.4274(5) 0.0492(19) Uani 1 1 d . . . . .
H47A H 1.163660 0.569600 0.385312 0.059 Uiso 1 1 calc R U . . .
H47B H 1.167029 0.579133 0.479542 0.059 Uiso 1 1 calc R U . . .
C48 C 0.9587(5) 0.5289(4) 0.4052(4) 0.0392(16) Uani 1 1 d . . . . .
C49 C 0.8544(5) 0.4747(4) 0.3799(4) 0.0339(14) Uani 1 1 d . . . . .
C50 C 0.7006(5) 0.4571(4) 0.3560(4) 0.0357(15) Uani 1 1 d . . . . .
H50 H 0.641837 0.469791 0.351181 0.043 Uiso 1 1 calc R U . . .
C51 C 0.8005(5) 0.3872(4) 0.3533(4) 0.0349(15) Uani 1 1 d . . . . .
C52 C 0.8191(5) 0.3065(4) 0.3379(4) 0.0381(15) Uani 1 1 d . . . . .
C53 C 0.7815(5) 0.1644(5) 0.2987(5) 0.0519(19) Uani 1 1 d . . . . .
H53A H 0.761485 0.122573 0.239249 0.062 Uiso 1 1 calc R U . . .
H53B H 0.754948 0.133347 0.331720 0.062 Uiso 1 1 calc R U . . .
C54 C 0.8932(5) 0.2071(5) 0.3315(6) 0.059(2) Uani 1 1 d . . . . .
H54A H 0.918613 0.198862 0.381522 0.070 Uiso 1 1 calc R U . . .
H54B H 0.925523 0.184255 0.288069 0.070 Uiso 1 1 calc R U . . .
O1S O 0.500000 0.500000 0.500000 0.175(13) Uiso 0.5 2 d S . P . .
Cl1 Cl 0.8286(4) 1.1451(4) 0.9187(3) 0.168(2) Uani 1 1 d . U . . .
O1 O 0.9215(10) 1.2003(15) 0.9233(12) 0.301(10) Uani 1 1 d . U . . .
O2 O 0.7794(13) 1.0891(14) 0.8408(10) 0.356(13) Uani 1 1 d . U . . .
O3 O 0.7762(11) 1.1886(13) 0.9568(11) 0.275(10) Uani 1 1 d . U . . .
O4 O 0.850(2) 1.1067(15) 0.9759(13) 0.350(13) Uani 1 1 d . U . . .
Cl2 Cl 0.8005(2) 0.95111(15) 1.27872(14) 0.0735(7) Uani 1 1 d . . . . .
O5 O 0.8545(6) 0.9907(5) 1.2351(5) 0.097(2) Uani 1 1 d . . . . .
O6 O 0.7005(6) 0.9285(7) 1.2362(5) 0.135(4) Uani 1 1 d . . . . .
O7 O 0.8132(9) 0.8761(5) 1.2756(6) 0.149(4) Uani 1 1 d . . . . .
O8 O 0.8192(6) 1.0113(5) 1.3617(4) 0.106(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N7 2.086(6) . ?
Ni1 N9 2.086(6) . ?
Ni1 N1 2.088(5) . ?
Ni1 N13 2.089(6) . ?
Ni1 N3 2.102(6) . ?
Ni1 N15 2.109(5) . ?
Ni2 N33 2.056(5) . ?
Ni2 N19 2.098(5) . ?
Ni2 N18 2.101(5) . ?
Ni2 N21 2.101(6) . ?
Ni2 N16 2.112(5) . ?
Ni2 N31 2.154(6) . ?
Ni3 N27 2.082(5) . ?
Ni3 N24 2.087(5) . ?
Ni3 N12 2.091(5) 2_666 ?
Ni3 N10 2.097(6) 2_666 ?
Ni3 N22 2.098(5) . ?
Ni3 N25 2.107(6) . ?
Ni4 N36 2.077(5) . ?
Ni4 N34 2.083(5) . ?
Ni4 N28 2.088(5) 2_666 ?
Ni4 N4 2.103(5) 2_666 ?
Ni4 N6 2.108(5) 2_666 ?
Ni4 N30 2.109(5) 2_666 ?
N1 C3 1.284(9) . ?
N1 C1 1.469(8) . ?
N2 C3 1.346(9) . ?
N2 C2 1.356(7) . ?
N2 H2 0.8800 . ?
N3 C5 1.318(8) . ?
N3 C4 1.365(8) . ?
N4 C7 1.287(9) . ?
N4 C8 1.469(9) . ?
N5 C9 1.360(7) . ?
N5 C7 1.375(9) . ?
N5 H5 0.8800 . ?
N6 C5 1.322(8) . ?
N6 C6 1.373(8) . ?
N7 C12 1.295(9) . ?
N7 C10 1.478(9) . ?
N8 C12 1.336(9) . ?
N8 C11 1.390(10) . ?
N8 H8 0.8800 . ?
N9 C14 1.334(8) . ?
N9 C13 1.367(8) . ?
N10 C16 1.287(9) . ?
N10 C17 1.465(10) . ?
N11 C16 1.380(9) . ?
N11 C18 1.430(11) . ?
N11 H11 0.8800 . ?
N12 C14 1.333(8) . ?
N12 C15 1.391(8) . ?
N13 C21 1.276(9) . ?
N13 C19 1.470(9) . ?
N14 C21 1.353(9) . ?
N14 C20 1.379(9) . ?
N14 H14 0.8800 . ?
N15 C23 1.340(8) . ?
N15 C22 1.372(8) . ?
N16 C25 1.313(9) . ?
N16 C26 1.475(9) . ?
N17 C25 1.357(9) . ?
N17 C27 1.391(8) . ?
N17 H17 0.8800 . ?
N18 C23 1.336(8) . ?
N18 C24 1.357(8) . ?
N19 C30 1.283(9) . ?
N19 C28 1.468(10) . ?
N20 C30 1.362(9) . ?
N20 C29 1.361(8) . ?
N20 H20C 0.8800 . ?
N21 C32 1.338(8) . ?
N21 C31 1.367(8) . ?
N22 C34 1.274(9) . ?
N22 C35 1.461(9) . ?
N23 C34 1.323(8) . ?
N23 C36 1.358(7) . ?
N23 H23A 0.8800 . ?
N24 C32 1.327(8) . ?
N24 C33 1.372(8) . ?
N25 C39 1.286(8) . ?
N25 C37 1.486(9) . ?
N26 C39 1.399(9) . ?
N26 C38 1.401(9) . ?
N26 H26 0.8800 . ?
N27 C41 1.339(8) . ?
N27 C40 1.382(8) . ?
N28 C43 1.283(8) . ?
N28 C44 1.475(8) . ?
N29 C43 1.352(9) . ?
N29 C45 1.379(9) . ?
N29 H29 0.8800 . ?
N30 C41 1.337(8) . ?
N30 C42 1.354(8) . ?
N31 C48 1.295(8) . ?
N31 C46 1.482(9) . ?
N32 C48 1.323(9) . ?
N32 C47 1.387(8) . ?
N32 H32A 0.8800 . ?
N33 C50 1.328(8) . ?
N33 C49 1.357(8) . ?
N34 C52 1.268(8) . ?
N34 C53 1.469(9) . ?
N35 C52 1.376(9) . ?
N35 C54 1.380(9) . ?
N35 H35 0.8800 . ?
N36 C50 1.353(8) . ?
N36 C51 1.388(8) . ?
C1 C2 1.511(11) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2AB 0.9900 . ?
C3 C4 1.458(9) . ?
C4 C6 1.394(9) . ?
C5 H5A 0.9500 . ?
C6 C7 1.446(9) . ?
C8 C9 1.527(11) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9AB 0.9900 . ?
C10 C11 1.533(13) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.464(9) . ?
C13 C15 1.361(9) . ?
C14 H14A 0.9500 . ?
C15 C16 1.455(10) . ?
C17 C18 1.490(13) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.536(11) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.453(9) . ?
C22 C24 1.379(9) . ?
C23 H23 0.9500 . ?
C24 C25 1.446(9) . ?
C26 C27 1.537(11) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.523(13) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.446(9) . ?
C31 C33 1.384(9) . ?
C32 H32 0.9500 . ?
C33 C34 1.455(9) . ?
C35 C36 1.524(11) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 C38 1.534(11) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.442(9) . ?
C40 C42 1.379(9) . ?
C41 H41 0.9500 . ?
C42 C43 1.462(9) . ?
C44 C45 1.525(11) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.532(10) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 C49 1.462(9) . ?
C49 C51 1.388(9) . ?
C50 H50 0.9500 . ?
C51 C52 1.466(9) . ?
C53 C54 1.520(10) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
Cl1 O2 1.321(13) . ?
Cl1 O3 1.324(13) . ?
Cl1 O1 1.411(15) . ?
Cl1 O4 1.455(16) . ?
Cl2 O7 1.374(8) . ?
Cl2 O8 1.407(7) . ?
Cl2 O5 1.411(7) . ?
Cl2 O6 1.419(9) . ?

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
N7 Ni1 N9 79.0(2) . . ?
N7 Ni1 N1 93.9(2) . . ?
N9 Ni1 N1 94.5(2) . . ?
N7 Ni1 N13 95.8(2) . . ?
N9 Ni1 N13 172.8(2) . . ?
N1 Ni1 N13 90.8(2) . . ?
N7 Ni1 N3 169.3(2) . . ?
N9 Ni1 N3 93.3(2) . . ?
N1 Ni1 N3 79.1(2) . . ?
N13 Ni1 N3 92.4(2) . . ?
N7 Ni1 N15 92.1(2) . . ?
N9 Ni1 N15 96.0(2) . . ?
N1 Ni1 N15 168.7(2) . . ?
N13 Ni1 N15 79.0(2) . . ?
N3 Ni1 N15 96.2(2) . . ?
N33 Ni2 N19 94.8(2) . . ?
N33 Ni2 N18 92.7(2) . . ?
N19 Ni2 N18 168.2(2) . . ?
N33 Ni2 N21 94.6(2) . . ?
N19 Ni2 N21 78.8(2) . . ?
N18 Ni2 N21 91.6(2) . . ?
N33 Ni2 N16 171.4(2) . . ?
N19 Ni2 N16 93.5(2) . . ?
N18 Ni2 N16 79.4(2) . . ?
N21 Ni2 N16 89.1(2) . . ?
N33 Ni2 N31 78.2(2) . . ?
N19 Ni2 N31 91.8(2) . . ?
N18 Ni2 N31 98.6(2) . . ?
N21 Ni2 N31 167.8(2) . . ?
N16 Ni2 N31 99.4(2) . . ?
N27 Ni3 N24 95.4(2) . . ?
N27 Ni3 N12 95.3(2) . 2_666 ?
N24 Ni3 N12 95.4(2) . 2_666 ?
N27 Ni3 N10 94.6(2) . 2_666 ?
N24 Ni3 N10 169.0(2) . 2_666 ?
N12 Ni3 N10 79.2(2) 2_666 2_666 ?
N27 Ni3 N22 169.6(2) . . ?
N24 Ni3 N22 79.0(2) . . ?
N12 Ni3 N22 93.9(2) 2_666 . ?
N10 Ni3 N22 91.7(2) 2_666 . ?
N27 Ni3 N25 79.4(2) . . ?
N24 Ni3 N25 90.5(2) . . ?
N12 Ni3 N25 172.5(2) 2_666 . ?
N10 Ni3 N25 95.8(2) 2_666 . ?
N22 Ni3 N25 91.9(2) . . ?
N36 Ni4 N34 78.4(2) . . ?
N36 Ni4 N28 168.6(2) . 2_666 ?
N34 Ni4 N28 92.1(2) . 2_666 ?
N36 Ni4 N4 94.8(2) . 2_666 ?
N34 Ni4 N4 92.2(2) . 2_666 ?
N28 Ni4 N4 91.8(2) 2_666 2_666 ?
N36 Ni4 N6 97.1(2) . 2_666 ?
N34 Ni4 N6 169.8(2) . 2_666 ?
N28 Ni4 N6 93.3(2) 2_666 2_666 ?
N4 Ni4 N6 79.0(2) 2_666 2_666 ?
N36 Ni4 N30 95.54(19) . 2_666 ?
N34 Ni4 N30 95.1(2) . 2_666 ?
N28 Ni4 N30 78.9(2) 2_666 2_666 ?
N4 Ni4 N30 168.3(2) 2_666 2_666 ?
N6 Ni4 N30 94.5(2) 2_666 2_666 ?
C3 N1 C1 108.7(6) . . ?
C3 N1 Ni1 114.2(4) . . ?
C1 N1 Ni1 136.8(5) . . ?
C3 N2 C2 117.2(6) . . ?
C3 N2 H2 121.4 . . ?
C2 N2 H2 121.4 . . ?
C5 N3 C4 104.8(6) . . ?
C5 N3 Ni1 143.1(4) . . ?
C4 N3 Ni1 112.0(4) . . ?
C7 N4 C8 109.2(6) . . ?
C7 N4 Ni4 113.0(4) . 2_666 ?
C8 N4 Ni4 136.7(5) . 2_666 ?
C9 N5 C7 117.9(6) . . ?
C9 N5 H5 121.0 . . ?
C7 N5 H5 121.0 . . ?
C5 N6 C6 105.0(5) . . ?
C5 N6 Ni4 143.1(4) . 2_666 ?
C6 N6 Ni4 111.9(4) . 2_666 ?
C12 N7 C10 108.1(6) . . ?
C12 N7 Ni1 114.1(5) . . ?
C10 N7 Ni1 137.4(5) . . ?
C12 N8 C11 113.2(7) . . ?
C12 N8 H8 123.4 . . ?
C11 N8 H8 123.4 . . ?
C14 N9 C13 105.2(6) . . ?
C14 N9 Ni1 141.2(5) . . ?
C13 N9 Ni1 113.5(4) . . ?
C16 N10 C17 107.4(6) . . ?
C16 N10 Ni3 113.5(5) . 2_666 ?
C17 N10 Ni3 138.1(5) . 2_666 ?
C16 N11 C18 108.3(7) . . ?
C16 N11 H11 125.9 . . ?
C18 N11 H11 125.9 . . ?
C14 N12 C15 104.9(5) . . ?
C14 N12 Ni3 141.9(5) . 2_666 ?
C15 N12 Ni3 112.9(4) . 2_666 ?
C21 N13 C19 108.4(6) . . ?
C21 N13 Ni1 114.4(4) . . ?
C19 N13 Ni1 137.0(5) . . ?
C21 N14 C20 112.5(6) . . ?
C21 N14 H14 123.7 . . ?
C20 N14 H14 123.7 . . ?
C23 N15 C22 104.5(5) . . ?
C23 N15 Ni1 144.5(4) . . ?
C22 N15 Ni1 111.0(4) . . ?
C25 N16 C26 106.7(6) . . ?
C25 N16 Ni2 111.1(4) . . ?
C26 N16 Ni2 135.9(5) . . ?
C25 N17 C27 111.5(6) . . ?
C25 N17 H17 124.2 . . ?
C27 N17 H17 124.2 . . ?
C23 N18 C24 103.8(5) . . ?
C23 N18 Ni2 144.2(4) . . ?
C24 N18 Ni2 112.0(4) . . ?
C30 N19 C28 108.0(6) . . ?
C30 N19 Ni2 113.8(4) . . ?
C28 N19 Ni2 138.0(5) . . ?
C30 N20 C29 119.6(7) . . ?
C30 N20 H20C 120.2 . . ?
C29 N20 H20C 120.2 . . ?
C32 N21 C31 105.1(5) . . ?
C32 N21 Ni2 142.2(4) . . ?
C31 N21 Ni2 112.5(4) . . ?
C34 N22 C35 108.6(6) . . ?
C34 N22 Ni3 114.0(4) . . ?
C35 N22 Ni3 137.1(5) . . ?
C34 N23 C36 117.5(6) . . ?
C34 N23 H23A 121.3 . . ?
C36 N23 H23A 121.3 . . ?
C32 N24 C33 105.1(5) . . ?
C32 N24 Ni3 142.4(4) . . ?
C33 N24 Ni3 112.5(4) . . ?
C39 N25 C37 107.8(6) . . ?
C39 N25 Ni3 112.3(4) . . ?
C37 N25 Ni3 134.8(5) . . ?
C39 N26 C38 110.4(6) . . ?
C39 N26 H26 124.8 . . ?
C38 N26 H26 124.8 . . ?
C41 N27 C40 104.4(5) . . ?
C41 N27 Ni3 142.8(4) . . ?
C40 N27 Ni3 112.5(4) . . ?
C43 N28 C44 107.3(6) . . ?
C43 N28 Ni4 114.5(4) . 2_666 ?
C44 N28 Ni4 138.2(5) . 2_666 ?
C43 N29 C45 113.0(6) . . ?
C43 N29 H29 123.5 . . ?
C45 N29 H29 123.5 . . ?
C41 N30 C42 104.7(5) . . ?
C41 N30 Ni4 142.8(4) . 2_666 ?
C42 N30 Ni4 112.2(4) . 2_666 ?
C48 N31 C46 106.4(6) . . ?
C48 N31 Ni2 112.8(5) . . ?
C46 N31 Ni2 138.2(5) . . ?
C48 N32 C47 114.9(6) . . ?
C48 N32 H32A 122.5 . . ?
C47 N32 H32A 122.5 . . ?
C50 N33 C49 106.0(5) . . ?
C50 N33 Ni2 138.7(5) . . ?
C49 N33 Ni2 115.1(4) . . ?
C52 N34 C53 108.9(5) . . ?
C52 N34 Ni4 115.8(4) . . ?
C53 N34 Ni4 135.3(4) . . ?
C52 N35 C54 112.4(6) . . ?
C52 N35 H35 123.8 . . ?
C54 N35 H35 123.8 . . ?
C50 N36 C51 104.0(5) . . ?
C50 N36 Ni4 142.1(5) . . ?
C51 N36 Ni4 113.7(4) . . ?
N1 C1 C2 105.8(6) . . ?
N1 C1 H1A 110.6 . . ?
C2 C1 H1A 110.6 . . ?
N1 C1 H1B 110.6 . . ?
C2 C1 H1B 110.6 . . ?
H1A C1 H1B 108.7 . . ?
N2 C2 C1 99.4(6) . . ?
N2 C2 H2A 111.9 . . ?
C1 C2 H2A 111.9 . . ?
N2 C2 H2AB 111.9 . . ?
C1 C2 H2AB 111.9 . . ?
H2A C2 H2AB 109.6 . . ?
N1 C3 N2 108.7(6) . . ?
N1 C3 C4 118.5(6) . . ?
N2 C3 C4 132.9(7) . . ?
N3 C4 C6 108.2(6) . . ?
N3 C4 C3 116.0(6) . . ?
C6 C4 C3 135.8(6) . . ?
N3 C5 N6 114.8(5) . . ?
N3 C5 H5A 122.6 . . ?
N6 C5 H5A 122.6 . . ?
N6 C6 C4 107.1(6) . . ?
N6 C6 C7 115.8(6) . . ?
C4 C6 C7 137.1(6) . . ?
N4 C7 N5 107.4(6) . . ?
N4 C7 C6 119.3(6) . . ?
N5 C7 C6 133.3(6) . . ?
N4 C8 C9 106.5(6) . . ?
N4 C8 H8A 110.4 . . ?
C9 C8 H8A 110.4 . . ?
N4 C8 H8B 110.4 . . ?
C9 C8 H8B 110.4 . . ?
H8A C8 H8B 108.6 . . ?
N5 C9 C8 98.1(6) . . ?
N5 C9 H9A 112.2 . . ?
C8 C9 H9A 112.2 . . ?
N5 C9 H9AB 112.2 . . ?
C8 C9 H9AB 112.2 . . ?
H9A C9 H9AB 109.8 . . ?
N7 C10 C11 104.4(7) . . ?
N7 C10 H10A 110.9 . . ?
C11 C10 H10A 110.9 . . ?
N7 C10 H10B 110.9 . . ?
C11 C10 H10B 110.9 . . ?
H10A C10 H10B 108.9 . . ?
N8 C11 C10 101.4(7) . . ?
N8 C11 H11A 111.5 . . ?
C10 C11 H11A 111.5 . . ?
N8 C11 H11B 111.5 . . ?
C10 C11 H11B 111.5 . . ?
H11A C11 H11B 109.3 . . ?
N7 C12 N8 112.1(6) . . ?
N7 C12 C13 118.6(6) . . ?
N8 C12 C13 128.9(7) . . ?
C15 C13 N9 109.0(6) . . ?
C15 C13 C12 136.3(6) . . ?
N9 C13 C12 114.4(6) . . ?
N12 C14 N9 113.3(6) . . ?
N12 C14 H14A 123.4 . . ?
N9 C14 H14A 123.4 . . ?
C13 C15 N12 107.7(6) . . ?
C13 C15 C16 138.3(6) . . ?
N12 C15 C16 114.1(6) . . ?
N10 C16 N11 114.0(7) . . ?
N10 C16 C15 119.6(6) . . ?
N11 C16 C15 126.5(7) . . ?
N10 C17 C18 106.1(7) . . ?
N10 C17 H17A 110.5 . . ?
C18 C17 H17A 110.5 . . ?
N10 C17 H17B 110.5 . . ?
C18 C17 H17B 110.5 . . ?
H17A C17 H17B 108.7 . . ?
N11 C18 C17 103.3(7) . . ?
N11 C18 H18A 111.1 . . ?
C17 C18 H18A 111.1 . . ?
N11 C18 H18B 111.1 . . ?
C17 C18 H18B 111.1 . . ?
H18A C18 H18B 109.1 . . ?
N13 C19 C20 104.0(6) . . ?
N13 C19 H19A 111.0 . . ?
C20 C19 H19A 111.0 . . ?
N13 C19 H19B 111.0 . . ?
C20 C19 H19B 111.0 . . ?
H19A C19 H19B 109.0 . . ?
N14 C20 C19 101.4(6) . . ?
N14 C20 H20A 111.5 . . ?
C19 C20 H20A 111.5 . . ?
N14 C20 H20B 111.5 . . ?
C19 C20 H20B 111.5 . . ?
H20A C20 H20B 109.3 . . ?
N13 C21 N14 112.2(6) . . ?
N13 C21 C22 118.4(6) . . ?
N14 C21 C22 129.3(6) . . ?
N15 C22 C24 107.4(5) . . ?
N15 C22 C21 116.3(6) . . ?
C24 C22 C21 135.9(6) . . ?
N18 C23 N15 114.4(5) . . ?
N18 C23 H23 122.8 . . ?
N15 C23 H23 122.8 . . ?
N18 C24 C22 109.8(5) . . ?
N18 C24 C25 116.2(6) . . ?
C22 C24 C25 134.0(6) . . ?
N16 C25 N17 113.6(6) . . ?
N16 C25 C24 118.3(6) . . ?
N17 C25 C24 127.6(7) . . ?
N16 C26 C27 105.3(6) . . ?
N16 C26 H26A 110.7 . . ?
C27 C26 H26A 110.7 . . ?
N16 C26 H26B 110.7 . . ?
C27 C26 H26B 110.7 . . ?
H26A C26 H26B 108.8 . . ?
N17 C27 C26 102.7(6) . . ?
N17 C27 H27A 111.2 . . ?
C26 C27 H27A 111.2 . . ?
N17 C27 H27B 111.2 . . ?
C26 C27 H27B 111.2 . . ?
H27A C27 H27B 109.1 . . ?
N19 C28 C29 108.1(7) . . ?
N19 C28 H28A 110.1 . . ?
C29 C28 H28A 110.1 . . ?
N19 C28 H28B 110.1 . . ?
C29 C28 H28B 110.1 . . ?
H28A C28 H28B 108.4 . . ?
N20 C29 C28 96.3(7) . . ?
N20 C29 H29A 112.5 . . ?
C28 C29 H29A 112.5 . . ?
N20 C29 H29B 112.5 . . ?
C28 C29 H29B 112.5 . . ?
H29A C29 H29B 110.0 . . ?
N19 C30 N20 107.6(6) . . ?
N19 C30 C31 119.3(6) . . ?
N20 C30 C31 132.7(7) . . ?
N21 C31 C33 107.9(6) . . ?
N21 C31 C30 115.4(6) . . ?
C33 C31 C30 136.6(6) . . ?
N24 C32 N21 113.7(5) . . ?
N24 C32 H32 123.1 . . ?
N21 C32 H32 123.1 . . ?
N24 C33 C31 108.1(5) . . ?
N24 C33 C34 115.4(6) . . ?
C31 C33 C34 136.5(6) . . ?
N22 C34 N23 109.4(6) . . ?
N22 C34 C33 118.8(6) . . ?
N23 C34 C33 131.8(7) . . ?
N22 C35 C36 105.4(6) . . ?
N22 C35 H35A 110.7 . . ?
C36 C35 H35A 110.7 . . ?
N22 C35 H35B 110.7 . . ?
C36 C35 H35B 110.7 . . ?
H35A C35 H35B 108.8 . . ?
N23 C36 C35 98.5(6) . . ?
N23 C36 H36A 112.1 . . ?
C35 C36 H36A 112.1 . . ?
N23 C36 H36B 112.1 . . ?
C35 C36 H36B 112.1 . . ?
H36A C36 H36B 109.7 . . ?
N25 C37 C38 104.9(6) . . ?
N25 C37 H37A 110.8 . . ?
C38 C37 H37A 110.8 . . ?
N25 C37 H37B 110.8 . . ?
C38 C37 H37B 110.8 . . ?
H37A C37 H37B 108.8 . . ?
N26 C38 C37 102.5(6) . . ?
N26 C38 H38A 111.3 . . ?
C37 C38 H38A 111.3 . . ?
N26 C38 H38B 111.3 . . ?
C37 C38 H38B 111.3 . . ?
H38A C38 H38B 109.2 . . ?
N25 C39 N26 113.0(6) . . ?
N25 C39 C40 119.7(6) . . ?
N26 C39 C40 127.1(6) . . ?
C42 C40 N27 107.5(6) . . ?
C42 C40 C39 137.9(6) . . ?
N27 C40 C39 114.6(6) . . ?
N30 C41 N27 114.0(6) . . ?
N30 C41 H41 123.0 . . ?
N27 C41 H41 123.0 . . ?
N30 C42 C40 109.3(6) . . ?
N30 C42 C43 116.1(6) . . ?
C40 C42 C43 134.5(6) . . ?
N28 C43 N29 112.4(6) . . ?
N28 C43 C42 118.2(6) . . ?
N29 C43 C42 129.2(6) . . ?
N28 C44 C45 105.0(6) . . ?
N28 C44 H44A 110.7 . . ?
C45 C44 H44A 110.7 . . ?
N28 C44 H44B 110.7 . . ?
C45 C44 H44B 110.7 . . ?
H44A C44 H44B 108.8 . . ?
N29 C45 C44 101.3(6) . . ?
N29 C45 H45A 111.5 . . ?
C44 C45 H45A 111.5 . . ?
N29 C45 H45B 111.5 . . ?
C44 C45 H45B 111.5 . . ?
H45A C45 H45B 109.3 . . ?
N31 C46 C47 105.7(6) . . ?
N31 C46 H46A 110.6 . . ?
C47 C46 H46A 110.6 . . ?
N31 C46 H46B 110.6 . . ?
C47 C46 H46B 110.6 . . ?
H46A C46 H46B 108.7 . . ?
N32 C47 C46 99.3(6) . . ?
N32 C47 H47A 111.9 . . ?
C46 C47 H47A 111.9 . . ?
N32 C47 H47B 111.9 . . ?
C46 C47 H47B 111.9 . . ?
H47A C47 H47B 109.6 . . ?
N31 C48 N32 112.3(6) . . ?
N31 C48 C49 117.9(6) . . ?
N32 C48 C49 129.6(6) . . ?
N33 C49 C51 108.3(6) . . ?
N33 C49 C48 115.5(6) . . ?
C51 C49 C48 136.2(6) . . ?
N33 C50 N36 113.7(6) . . ?
N33 C50 H50 123.2 . . ?
N36 C50 H50 123.2 . . ?
C49 C51 N36 108.0(6) . . ?
C49 C51 C52 138.3(6) . . ?
N36 C51 C52 113.7(5) . . ?
N34 C52 N35 111.7(6) . . ?
N34 C52 C51 118.3(6) . . ?
N35 C52 C51 130.1(6) . . ?
N34 C53 C54 105.0(6) . . ?
N34 C53 H53A 110.7 . . ?
C54 C53 H53A 110.7 . . ?
N34 C53 H53B 110.7 . . ?
C54 C53 H53B 110.7 . . ?
H53A C53 H53B 108.8 . . ?
N35 C54 C53 102.0(6) . . ?
N35 C54 H54A 111.4 . . ?
C53 C54 H54A 111.4 . . ?
N35 C54 H54B 111.4 . . ?
C53 C54 H54B 111.4 . . ?
H54A C54 H54B 109.2 . . ?
O2 Cl1 O3 112.5(12) . . ?
O2 Cl1 O1 111.6(14) . . ?
O3 Cl1 O1 112.4(14) . . ?
O2 Cl1 O4 115.2(17) . . ?
O3 Cl1 O4 99.3(14) . . ?
O1 Cl1 O4 105.1(14) . . ?
O7 Cl2 O8 111.6(5) . . ?
O7 Cl2 O5 114.7(6) . . ?
O8 Cl2 O5 110.3(5) . . ?
O7 Cl2 O6 107.4(7) . . ?
O8 Cl2 O6 108.3(6) . . ?
O5 Cl2 O6 104.0(5) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C1 H1A O1 0.99 2.54 3.335(16) 137.3 2_777 yes
C46 H46A N35 0.99 2.69 3.409(10) 129.4 2_766 yes
N8 H8 N11 0.88 2.65 3.336(7) 135.8 . yes
C9 H9AB O3 0.99 2.50 3.136(18) 121.5 2_677 yes
C10 H10A O4 0.99 2.62 3.56(2) 159.5 2_777 yes
N11 H11 N8 0.88 2.66 3.336(7) 134.6 . yes
N26 H26 N29 0.88 2.68 3.312(4) 129.6 . yes
N29 H29 N26 0.88 2.62 3.312(4) 136.0 . yes
C45 H45B O2 0.99 2.50 3.34(2) 142.7 . yes
C36 H36B O6 0.99 2.60 3.340(13) 131.7 1_554 yes
N14 H14 O5 0.88 2.51 2.983(10) 114.8 2_777 yes
N14 H14 N17 0.88 2.60 3.301(4) 137.4 . yes

_refine_diff_density_max         1.624
_refine_diff_density_min         -1.616
_refine_diff_density_rms         0.109




