# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2018

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Complex3b
_database_code_depnum_ccdc_archive 'CCDC 1835110'
_audit_update_record             
;
2018-04-05 deposited with the CCDC.
2018-09-04 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT417_Complex3b           
;
PROBLEM: Short Inter D-H..H-D       H3B1     ..H4B1             1.55 Ang.
RESPONSE: This is due to disorder
;
_vrf_PLAT414_Complex3b           
;
PROBLEM: Short Intra D-H..H-X       H4A      ..H12A             1.89 Ang.
RESPONSE: This is due to disorder
;
_vrf_PLAT416_Complex3b           
;
PROBLEM: Short Intra D-H..H-D       H12C     ..H4B2             1.08 Ang.
RESPONSE: This is due to disorder
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H52 N6 Ni4 O12 S2, Cl2, H2 O, C H4 O'
_chemical_formula_sum            'C37 H58 Cl2 N6 Ni4 O14 S2'
_chemical_formula_weight         1180.75

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   11.8297(4)
_cell_length_b                   13.0777(5)
_cell_length_c                   19.8873(5)
_cell_angle_alpha                89.9710(17)
_cell_angle_beta                 74.6770(15)
_cell_angle_gamma                64.9690(12)
_cell_volume                     2666.71(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    295
_cell_measurement_reflns_used    31349
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      30.00

_exptl_crystal_description       prismatic
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_F_000             1224
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    1.630
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.629
_exptl_absorpt_correction_T_max  0.829
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'φ scans and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            31349
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_av_R_equivalents  0.0642
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.516
_diffrn_reflns_theta_max         30.056
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.985
_reflns_number_total             15385
_reflns_number_gt                11442
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_cell_refinement       'Denzo SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction        'Denzo SMN (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP III (Burnett & Johnson, 1996)'
_computing_publication_material  
'SHELXL-2014/6 (Sheldrick, 2014), PARST (Nardelli, 1995), PLATON (Spek, 2009)'
_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)+(0.1220P)²+2.8463P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         15385
_refine_ls_number_parameters     602
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0676
_refine_ls_wR_factor_ref         0.2220
_refine_ls_wR_factor_gt          0.1950
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.059
_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 0.63428(4) 0.39364(4) -0.01476(2) 0.03968(12) Uani 1 1 d . . . . .
Ni2 Ni 0.45495(5) 0.47248(4) 0.13594(2) 0.03999(12) Uani 1 1 d . . . . .
O1A O 0.5531(3) 0.3308(2) 0.06749(13) 0.0445(5) Uani 1 1 d . . . . .
C1A C 0.5546(4) 0.2307(3) 0.0735(2) 0.0448(7) Uani 1 1 d . . . . .
C2A C 0.4806(4) 0.2085(4) 0.1362(2) 0.0519(9) Uani 1 1 d . . . . .
C3A C 0.4863(6) 0.0999(4) 0.1405(3) 0.0637(12) Uani 1 1 d . . . . .
H3A H 0.4368 0.0870 0.1814 0.076 Uiso 1 1 calc R U . . .
C4A C 0.5623(6) 0.0104(4) 0.0866(3) 0.0705(14) Uani 1 1 d . . . . .
C5A C 0.6323(6) 0.0325(4) 0.0265(3) 0.0661(12) Uani 1 1 d . . . . .
H5A H 0.6837 -0.0265 -0.0102 0.079 Uiso 1 1 calc R U . . .
C6A C 0.6304(4) 0.1401(3) 0.0173(2) 0.0537(9) Uani 1 1 d . . . . .
C7A C 0.5695(8) -0.1077(5) 0.0949(4) 0.096(2) Uani 1 1 d . . . . .
H7A1 H 0.5831 -0.1451 0.0499 0.144 Uiso 1 1 calc R U . . .
H7A2 H 0.4894 -0.1012 0.1267 0.144 Uiso 1 1 calc R U . . .
H7A3 H 0.6407 -0.1514 0.1132 0.144 Uiso 1 1 calc R U . . .
C8A C 0.7049(5) 0.1513(4) -0.0511(3) 0.0591(10) Uani 1 1 d . . . . .
H8A H 0.7482 0.0865 -0.0840 0.071 Uiso 1 1 calc R U . . .
O2A O 0.7175(4) 0.2388(3) -0.07086(19) 0.0701(9) Uani 1 1 d . . . . .
C9A C 0.4002(4) 0.2900(4) 0.1982(2) 0.0542(9) Uani 1 1 d . . . . .
H9A H 0.3554 0.2649 0.2349 0.065 Uiso 1 1 calc R U . . .
N1A N 0.3833(3) 0.3923(3) 0.20855(17) 0.0494(7) Uani 1 1 d . . . . .
C10A C 0.2966(5) 0.4656(4) 0.2759(2) 0.0619(11) Uani 1 1 d . . . . .
C11A C 0.2302(5) 0.5873(5) 0.2573(3) 0.0694(13) Uani 1 1 d . . . . .
H11A H 0.1621 0.5929 0.2369 0.083 Uiso 1 1 calc R U . . .
H11B H 0.1899 0.6410 0.2998 0.083 Uiso 1 1 calc R U . . .
O3A O 0.3221(3) 0.6157(3) 0.20874(16) 0.0595(7) Uani 1 1 d . . . . .
H3A1 H 0.3228 0.6865 0.2094 0.071 Uiso 1 1 calc R U . . .
C12A C 0.3812(6) 0.4646(5) 0.3223(2) 0.0674(12) Uani 1 1 d . . . . .
H12A H 0.4436 0.4919 0.2979 0.081 Uiso 1 1 calc R U . . .
H12B H 0.3265 0.5160 0.3652 0.081 Uiso 1 1 calc R U . . .
O4A O 0.4499(4) 0.3532(3) 0.33965(17) 0.0762(10) Uani 1 1 d . . . . .
H4A H 0.5282 0.3359 0.3072 0.091 Uiso 1 1 d . U . . .
C13A C 0.1903(6) 0.4334(6) 0.3156(3) 0.0890(18) Uani 1 1 d . . . . .
H13A H 0.1548 0.4119 0.2829 0.133 Uiso 1 1 calc R U . . .
H13B H 0.1224 0.4972 0.3483 0.133 Uiso 1 1 calc R U . . .
H13C H 0.2265 0.3706 0.3407 0.133 Uiso 1 1 calc R U . . .
C14A C 0.6861(5) 0.5262(4) 0.1111(3) 0.0595(11) Uani 1 1 d . . . . .
N2A N 0.6115(4) 0.4733(3) 0.16698(18) 0.0533(8) Uani 1 1 d . . . . .
H2A1 H 0.5816 0.5142 0.2090 0.064 Uiso 1 1 calc R U . . .
H2A2 H 0.6658 0.4026 0.1703 0.064 Uiso 1 1 calc R U . . .
C15A C 0.8054(5) 0.4320(5) 0.0636(3) 0.0651(11) Uani 1 1 d . . . . .
H15A H 0.8488 0.4653 0.0284 0.078 Uiso 1 1 calc R U . . .
H15B H 0.8643 0.3933 0.0910 0.078 Uiso 1 1 calc R U . . .
O5A O 0.7855(3) 0.3518(3) 0.02938(17) 0.0628(8) Uani 1 1 d . . . . .
H5A1 H 0.8428 0.2754 0.0261 0.075 Uiso 1 1 calc R U . . .
C16A C 0.5877(4) 0.6014(3) 0.0732(2) 0.0447(7) Uani 1 1 d . . . . .
H16A H 0.5241 0.6706 0.1040 0.054 Uiso 1 1 calc R U . . .
H16B H 0.6332 0.6225 0.0316 0.054 Uiso 1 1 calc R U . . .
O6A O 0.5237(2) 0.5414(2) 0.05385(12) 0.0375(5) Uani 1 1 d . . . . .
C17A C 0.7276(6) 0.5998(5) 0.1487(3) 0.0783(15) Uani 1 1 d . . . . .
H17A H 0.7808 0.5548 0.1766 0.117 Uiso 1 1 calc R U . . .
H17B H 0.6516 0.6619 0.1785 0.117 Uiso 1 1 calc R U . . .
H17C H 0.7766 0.6290 0.1146 0.117 Uiso 1 1 calc R U . . .
N3A N 0.2859(3) 0.5218(3) 0.08963(18) 0.0513(7) Uani 1 1 d . . . . .
C18A C 0.2145(4) 0.4810(4) 0.1027(3) 0.0596(10) Uani 1 1 d . . . . .
S1A S 0.11362(19) 0.42468(19) 0.12427(14) 0.1112(7) Uani 1 1 d . . . . .
Ni3 Ni 0.55723(5) -0.03687(5) 0.56258(2) 0.04923(14) Uani 1 1 d . . . . .
Ni4 Ni 0.43161(5) 0.21760(5) 0.54694(2) 0.04634(14) Uani 1 1 d . . . . .
O1B O 0.4181(3) 0.1129(3) 0.61864(13) 0.0508(6) Uani 1 1 d . . . . .
C1B C 0.3336(4) 0.1351(3) 0.68116(17) 0.0444(7) Uani 1 1 d . . . . .
C2B C 0.2374(4) 0.2468(4) 0.70881(18) 0.0475(8) Uani 1 1 d . . . . .
C3B C 0.1474(4) 0.2672(4) 0.7758(2) 0.0551(9) Uani 1 1 d . . . . .
H3B H 0.0839 0.3411 0.7928 0.066 Uiso 1 1 calc R U . . .
C4B C 0.1499(5) 0.1818(5) 0.8169(2) 0.0619(11) Uani 1 1 d . . . . .
C5B C 0.2440(5) 0.0736(5) 0.7898(2) 0.0591(10) Uani 1 1 d . . . . .
H5B H 0.2471 0.0152 0.8171 0.071 Uiso 1 1 calc R U . . .
C6B C 0.3358(4) 0.0460(4) 0.72326(19) 0.0500(8) Uani 1 1 d . . . . .
C7B C 0.0548(6) 0.2080(6) 0.8907(3) 0.0899(19) Uani 1 1 d . . . . .
H7B1 H 0.0030 0.1674 0.8931 0.135 Uiso 1 1 calc R U . . .
H7B2 H -0.0011 0.2882 0.9009 0.135 Uiso 1 1 calc R U . . .
H7B3 H 0.1029 0.1848 0.9245 0.135 Uiso 1 1 calc R U . . .
C8B C 0.4291(5) -0.0722(4) 0.7025(2) 0.0595(10) Uani 1 1 d . . . . .
H8B H 0.4204 -0.1222 0.7346 0.071 Uiso 1 1 calc R U . . .
O2B O 0.5210(4) -0.1156(4) 0.64594(19) 0.0794(11) Uani 1 1 d . . . . .
C9B C 0.2235(4) 0.3482(4) 0.6741(2) 0.0514(9) Uani 1 1 d . . . . .
H9B H 0.1563 0.4168 0.6984 0.062 Uiso 1 1 calc R U . . .
N1B N 0.2936(3) 0.3532(3) 0.61412(16) 0.0475(7) Uani 1 1 d . . . . .
C10B C 0.2692(5) 0.4667(4) 0.5898(2) 0.0534(9) Uani 1 1 d . . . . .
C11B C 0.3019(5) 0.4473(4) 0.5098(2) 0.0627(11) Uani 1 1 d . . . . .
H11C H 0.2322 0.4389 0.4972 0.075 Uiso 1 1 calc R U . . .
H11D H 0.3097 0.5126 0.4899 0.075 Uiso 1 1 calc R U . . .
O3B O 0.4210(3) 0.3478(3) 0.48186(15) 0.0623(8) Uani 1 1 d . . . . .
H3B1 H 0.4852 0.3409 0.4408 0.075 Uiso 1 1 calc R U . . .
C12B C 0.3658(6) 0.5021(5) 0.6092(3) 0.0692(12) Uani 1 1 d . . . A 1
H12C H 0.3500 0.5072 0.6598 0.083 Uiso 1 1 calc R U . A 1
H12D H 0.4539 0.4439 0.5878 0.083 Uiso 1 1 calc R U . A 1
O4B1 O 0.3559(8) 0.6073(6) 0.5873(4) 0.0728(18) Uani 0.5 1 d . . P A 1
H4B1 H 0.4089 0.6230 0.5987 0.109 Uiso 0.5 1 calc R U P A 1
O4B2 O 0.3321(14) 0.5183(11) 0.6865(6) 0.121(4) Uani 0.5 1 d . . P B 2
H4B2 H 0.2715 0.5046 0.7015 0.182 Uiso 0.5 1 d . U P C 2
C13B C 0.1299(6) 0.5579(5) 0.6182(3) 0.0747(14) Uani 1 1 d . . . . .
H13D H 0.0712 0.5290 0.6109 0.112 Uiso 1 1 calc R U . . .
H13E H 0.1194 0.6235 0.5941 0.112 Uiso 1 1 calc R U . . .
H13F H 0.1110 0.5788 0.6675 0.112 Uiso 1 1 calc R U . . .
C14B C 0.7302(5) 0.1068(5) 0.5064(3) 0.0671(12) Uani 1 1 d . . . . .
N2B N 0.6033(6) 0.2190(5) 0.5562(4) 0.0971(18) Uani 1 1 d . . . . .
H2B1 H 0.6074 0.2825 0.5426 0.117 Uiso 1 1 calc R U . . .
H2B2 H 0.6040 0.2170 0.6009 0.117 Uiso 1 1 calc R U . . .
C15B C 0.7766(7) 0.0268(6) 0.5532(3) 0.0850(16) Uani 1 1 d . . . . .
H15C H 0.8504 -0.0406 0.5253 0.102 Uiso 1 1 calc R U . . .
H15D H 0.8085 0.0595 0.5833 0.102 Uiso 1 1 calc R U . . .
O5B O 0.6917(4) -0.0060(4) 0.5944(2) 0.0867(12) Uani 1 1 d . . . . .
H5B1 H 0.6941 -0.0153 0.6404 0.104 Uiso 1 1 calc R U . . .
C16B C 0.6813(4) 0.0684(4) 0.4521(2) 0.0534(9) Uani 1 1 d . . . . .
H16C H 0.6713 0.1196 0.4164 0.064 Uiso 1 1 calc R U . . .
H16D H 0.7441 -0.0075 0.4292 0.064 Uiso 1 1 calc R U . . .
O6B O 0.5608(3) 0.0683(3) 0.48554(13) 0.0498(6) Uani 1 1 d . . . . .
C17B C 0.8368(7) 0.1436(8) 0.4662(4) 0.105(2) Uani 1 1 d . . . . .
H17D H 0.8623 0.1760 0.4994 0.158 Uiso 1 1 calc R U . . .
H17E H 0.8022 0.1990 0.4363 0.158 Uiso 1 1 calc R U . . .
H17F H 0.9113 0.0783 0.4380 0.158 Uiso 1 1 calc R U . . .
N3B N 0.2936(4) 0.1881(3) 0.5036(2) 0.0583(9) Uani 1 1 d . . . . .
C18B C 0.1805(5) 0.2364(4) 0.5184(3) 0.0642(11) Uani 1 1 d . . . . .
S1B S 0.02436(17) 0.3021(2) 0.53940(18) 0.1460(12) Uani 1 1 d . . . . .
Cl1 Cl 0.7381(2) 0.25065(18) 0.26028(11) 0.1104(6) Uani 1 1 d . . . . .
Cl2 Cl 0.3945(3) 0.7660(3) 0.28140(11) 0.1416(10) Uani 1 1 d . . . . .
O1W O 0.8660(10) 0.1672(6) 0.1011(4) 0.169(3) Uani 1 1 d . . . . .
H1W H 0.8240 0.1681 0.1528 0.202 Uiso 1 1 d . U . . .
H2W H 0.9535 0.0919 0.0823 0.202 Uiso 1 1 d . U . . .
C1 C 0.0235(14) 0.9170(16) 0.2847(9) 0.226(9) Uani 1 1 d . . . . .
H1A H 0.0454 0.9064 0.3282 0.339 Uiso 1 1 calc R U . . .
H1B H -0.0074 0.8630 0.2755 0.339 Uiso 1 1 calc R U . . .
H1C H -0.0434 0.9928 0.2880 0.339 Uiso 1 1 calc R U . . .
O1 O 0.1385(17) 0.9003(12) 0.2279(7) 0.320(10) Uani 1 1 d . . . . .
H1 H 0.1593 0.8442 0.2005 0.480 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O2A 2.012(4) . ?
Ni1 O1A 2.027(3) . ?
Ni1 O6A 2.056(2) . ?
Ni1 O6A 2.059(2) 2_665 ?
Ni1 O5A 2.067(3) . ?
Ni1 N3A 2.114(3) 2_665 ?
Ni2 O1A 1.995(3) . ?
Ni2 N1A 2.001(3) . ?
Ni2 O6A 2.014(2) . ?
Ni2 O3A 2.094(3) . ?
Ni2 N2A 2.105(3) . ?
Ni2 N3A 2.268(4) . ?
O1A C1A 1.307(4) . ?
C1A C6A 1.425(6) . ?
C1A C2A 1.430(6) . ?
C2A C3A 1.396(6) . ?
C2A C9A 1.444(7) . ?
C3A C4A 1.388(8) . ?
C3A H3A 0.9300 . ?
C4A C5A 1.371(8) . ?
C4A C7A 1.522(7) . ?
C5A C6A 1.411(6) . ?
C5A H5A 0.9300 . ?
C6A C8A 1.457(7) . ?
C7A H7A1 0.9600 . ?
C7A H7A2 0.9600 . ?
C7A H7A3 0.9600 . ?
C8A O2A 1.266(6) . ?
C8A H8A 0.9300 . ?
C9A N1A 1.276(6) . ?
C9A H9A 0.9300 . ?
N1A C10A 1.486(6) . ?
C10A C13A 1.519(7) . ?
C10A C12A 1.526(7) . ?
C10A C11A 1.543(7) . ?
C11A O3A 1.428(6) . ?
C11A H11A 0.9700 . ?
C11A H11B 0.9700 . ?
O3A H3A1 0.9300 . ?
C12A O4A 1.431(6) . ?
C12A H12A 0.9700 . ?
C12A H12B 0.9700 . ?
O4A H4A 0.912(4) . ?
C13A H13A 0.9600 . ?
C13A H13B 0.9600 . ?
C13A H13C 0.9600 . ?
C14A C15A 1.493(7) . ?
C14A C17A 1.523(6) . ?
C14A C16A 1.545(6) . ?
C14A N2A 1.577(6) . ?
N2A H2A1 0.8900 . ?
N2A H2A2 0.8900 . ?
C15A O5A 1.384(6) . ?
C15A H15A 0.9700 . ?
C15A H15B 0.9700 . ?
O5A H5A1 0.9300 . ?
C16A O6A 1.413(4) . ?
C16A H16A 0.9700 . ?
C16A H16B 0.9700 . ?
O6A Ni1 2.059(2) 2_665 ?
C17A H17A 0.9600 . ?
C17A H17B 0.9600 . ?
C17A H17C 0.9600 . ?
N3A C18A 1.154(6) . ?
N3A Ni1 2.114(3) 2_665 ?
C18A S1A 1.620(5) . ?
Ni3 O2B 1.997(4) . ?
Ni3 O1B 2.023(3) . ?
Ni3 O5B 2.042(4) . ?
Ni3 O6B 2.056(3) 2_656 ?
Ni3 O6B 2.062(3) . ?
Ni3 N3B 2.140(4) 2_656 ?
Ni4 N1B 1.998(3) . ?
Ni4 O1B 1.999(3) . ?
Ni4 O6B 2.032(3) . ?
Ni4 N2B 2.095(5) . ?
Ni4 O3B 2.120(3) . ?
Ni4 N3B 2.198(4) . ?
O1B C1B 1.314(4) . ?
C1B C2B 1.412(6) . ?
C1B C6B 1.430(5) . ?
C2B C3B 1.410(5) . ?
C2B C9B 1.462(6) . ?
C3B C4B 1.377(7) . ?
C3B H3B 0.9300 . ?
C4B C5B 1.372(7) . ?
C4B C7B 1.530(6) . ?
C5B C6B 1.404(5) . ?
C5B H5B 0.9300 . ?
C6B C8B 1.447(7) . ?
C7B H7B1 0.9600 . ?
C7B H7B2 0.9600 . ?
C7B H7B3 0.9600 . ?
C8B O2B 1.266(6) . ?
C8B H8B 0.9300 . ?
C9B N1B 1.280(5) . ?
C9B H9B 0.9300 . ?
N1B C10B 1.495(5) . ?
C10B C13B 1.517(7) . ?
C10B C11B 1.528(6) . ?
C10B C12B 1.533(7) . ?
C11B O3B 1.422(6) . ?
C11B H11C 0.9700 . ?
C11B H11D 0.9700 . ?
O3B H3B1 0.9300 . ?
C12B O4B1 1.409(8) . ?
C12B H12C 0.9700 . ?
C12B H12D 0.9700 . ?
O4B1 H4B1 0.8200 . ?
O4B2 H4B2 0.795(12) . ?
C13B H13D 0.9600 . ?
C13B H13E 0.9600 . ?
C13B H13F 0.9600 . ?
C14B C15B 1.430(9) . ?
C14B C16B 1.527(7) . ?
C14B C17B 1.563(8) . ?
C14B N2B 1.655(8) . ?
N2B H2B1 0.8900 . ?
N2B H2B2 0.8900 . ?
C15B O5B 1.339(8) . ?
C15B H15C 0.9700 . ?
C15B H15D 0.9700 . ?
O5B H5B1 0.9300 . ?
C16B O6B 1.405(5) . ?
C16B H16C 0.9700 . ?
C16B H16D 0.9700 . ?
O6B Ni3 2.056(3) 2_656 ?
C17B H17D 0.9600 . ?
C17B H17E 0.9600 . ?
C17B H17F 0.9600 . ?
N3B C18B 1.164(6) . ?
N3B Ni3 2.140(4) 2_656 ?
C18B S1B 1.604(5) . ?
O1W H1W 1.015(8) . ?
O1W H2W 1.055(9) . ?
C1 O1 1.453(19) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
O1 H1 0.8200 . ?

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
O2A Ni1 O1A 88.86(13) . . ?
O2A Ni1 O6A 168.86(13) . . ?
O1A Ni1 O6A 80.90(10) . . ?
O2A Ni1 O6A 95.40(13) . 2_665 ?
O1A Ni1 O6A 96.60(10) . 2_665 ?
O6A Ni1 O6A 81.55(10) . 2_665 ?
O2A Ni1 O5A 92.32(15) . . ?
O1A Ni1 O5A 85.65(13) . . ?
O6A Ni1 O5A 91.26(12) . . ?
O6A Ni1 O5A 172.00(12) 2_665 . ?
O2A Ni1 N3A 98.93(15) . 2_665 ?
O1A Ni1 N3A 171.71(12) . 2_665 ?
O6A Ni1 N3A 91.53(12) . 2_665 ?
O6A Ni1 N3A 85.54(12) 2_665 2_665 ?
O5A Ni1 N3A 91.18(14) . 2_665 ?
O1A Ni2 N1A 91.59(13) . . ?
O1A Ni2 O6A 82.72(10) . . ?
N1A Ni2 O6A 172.67(12) . . ?
O1A Ni2 O3A 169.45(13) . . ?
N1A Ni2 O3A 82.30(14) . . ?
O6A Ni2 O3A 102.60(11) . . ?
O1A Ni2 N2A 98.70(13) . . ?
N1A Ni2 N2A 102.98(14) . . ?
O6A Ni2 N2A 82.52(12) . . ?
O3A Ni2 N2A 91.07(14) . . ?
O1A Ni2 N3A 89.25(12) . . ?
N1A Ni2 N3A 92.69(13) . . ?
O6A Ni2 N3A 82.67(11) . . ?
O3A Ni2 N3A 82.49(14) . . ?
N2A Ni2 N3A 162.14(14) . . ?
C1A O1A Ni2 129.4(2) . . ?
C1A O1A Ni1 131.5(2) . . ?
Ni2 O1A Ni1 98.86(11) . . ?
O1A C1A C6A 120.7(4) . . ?
O1A C1A C2A 121.4(4) . . ?
C6A C1A C2A 117.9(4) . . ?
C3A C2A C1A 119.4(4) . . ?
C3A C2A C9A 115.6(4) . . ?
C1A C2A C9A 125.0(4) . . ?
C4A C3A C2A 123.2(5) . . ?
C4A C3A H3A 118.4 . . ?
C2A C3A H3A 118.4 . . ?
C5A C4A C3A 117.2(4) . . ?
C5A C4A C7A 121.6(6) . . ?
C3A C4A C7A 121.2(6) . . ?
C4A C5A C6A 123.3(5) . . ?
C4A C5A H5A 118.3 . . ?
C6A C5A H5A 118.3 . . ?
C5A C6A C1A 119.1(4) . . ?
C5A C6A C8A 116.6(4) . . ?
C1A C6A C8A 124.3(4) . . ?
C4A C7A H7A1 109.5 . . ?
C4A C7A H7A2 109.5 . . ?
H7A1 C7A H7A2 109.5 . . ?
C4A C7A H7A3 109.5 . . ?
H7A1 C7A H7A3 109.5 . . ?
H7A2 C7A H7A3 109.5 . . ?
O2A C8A C6A 127.5(4) . . ?
O2A C8A H8A 116.2 . . ?
C6A C8A H8A 116.2 . . ?
C8A O2A Ni1 126.9(3) . . ?
N1A C9A C2A 127.7(4) . . ?
N1A C9A H9A 116.2 . . ?
C2A C9A H9A 116.2 . . ?
C9A N1A C10A 121.0(4) . . ?
C9A N1A Ni2 124.6(3) . . ?
C10A N1A Ni2 114.2(3) . . ?
N1A C10A C13A 115.1(5) . . ?
N1A C10A C12A 108.3(4) . . ?
C13A C10A C12A 110.0(4) . . ?
N1A C10A C11A 106.5(3) . . ?
C13A C10A C11A 107.9(5) . . ?
C12A C10A C11A 108.9(4) . . ?
O3A C11A C10A 111.2(4) . . ?
O3A C11A H11A 109.4 . . ?
C10A C11A H11A 109.4 . . ?
O3A C11A H11B 109.4 . . ?
C10A C11A H11B 109.4 . . ?
H11A C11A H11B 108.0 . . ?
C11A O3A Ni2 109.1(3) . . ?
C11A O3A H3A1 125.4 . . ?
Ni2 O3A H3A1 125.4 . . ?
O4A C12A C10A 112.0(4) . . ?
O4A C12A H12A 109.2 . . ?
C10A C12A H12A 109.2 . . ?
O4A C12A H12B 109.2 . . ?
C10A C12A H12B 109.2 . . ?
H12A C12A H12B 107.9 . . ?
C12A O4A H4A 96.9(3) . . ?
C10A C13A H13A 109.5 . . ?
C10A C13A H13B 109.5 . . ?
H13A C13A H13B 109.5 . . ?
C10A C13A H13C 109.5 . . ?
H13A C13A H13C 109.5 . . ?
H13B C13A H13C 109.5 . . ?
C15A C14A C17A 108.6(4) . . ?
C15A C14A C16A 114.0(4) . . ?
C17A C14A C16A 109.5(4) . . ?
C15A C14A N2A 109.0(4) . . ?
C17A C14A N2A 109.5(4) . . ?
C16A C14A N2A 106.3(3) . . ?
C14A N2A Ni2 109.4(2) . . ?
C14A N2A H2A1 109.8 . . ?
Ni2 N2A H2A1 109.8 . . ?
C14A N2A H2A2 109.8 . . ?
Ni2 N2A H2A2 109.8 . . ?
H2A1 N2A H2A2 108.2 . . ?
O5A C15A C14A 116.0(4) . . ?
O5A C15A H15A 108.3 . . ?
C14A C15A H15A 108.3 . . ?
O5A C15A H15B 108.3 . . ?
C14A C15A H15B 108.3 . . ?
H15A C15A H15B 107.4 . . ?
C15A O5A Ni1 123.1(3) . . ?
C15A O5A H5A1 118.5 . . ?
Ni1 O5A H5A1 118.5 . . ?
O6A C16A C14A 109.8(3) . . ?
O6A C16A H16A 109.7 . . ?
C14A C16A H16A 109.7 . . ?
O6A C16A H16B 109.7 . . ?
C14A C16A H16B 109.7 . . ?
H16A C16A H16B 108.2 . . ?
C16A O6A Ni2 110.8(2) . . ?
C16A O6A Ni1 118.3(2) . . ?
Ni2 O6A Ni1 97.32(10) . . ?
C16A O6A Ni1 126.8(2) . 2_665 ?
Ni2 O6A Ni1 100.19(10) . 2_665 ?
Ni1 O6A Ni1 98.45(10) . 2_665 ?
C14A C17A H17A 109.5 . . ?
C14A C17A H17B 109.5 . . ?
H17A C17A H17B 109.5 . . ?
C14A C17A H17C 109.5 . . ?
H17A C17A H17C 109.5 . . ?
H17B C17A H17C 109.5 . . ?
C18A N3A Ni1 144.4(4) . 2_665 ?
C18A N3A Ni2 122.2(3) . . ?
Ni1 N3A Ni2 90.91(13) 2_665 . ?
N3A C18A S1A 177.7(5) . . ?
O2B Ni3 O1B 89.24(14) . . ?
O2B Ni3 O5B 92.67(19) . . ?
O1B Ni3 O5B 88.48(16) . . ?
O2B Ni3 O6B 95.37(15) . 2_656 ?
O1B Ni3 O6B 96.09(12) . 2_656 ?
O5B Ni3 O6B 170.79(15) . 2_656 ?
O2B Ni3 O6B 169.34(14) . . ?
O1B Ni3 O6B 80.74(11) . . ?
O5B Ni3 O6B 90.70(16) . . ?
O6B Ni3 O6B 82.19(13) 2_656 . ?
O2B Ni3 N3B 95.24(16) . 2_656 ?
O1B Ni3 N3B 175.51(13) . 2_656 ?
O5B Ni3 N3B 91.49(17) . 2_656 ?
O6B Ni3 N3B 83.32(13) 2_656 2_656 ?
O6B Ni3 N3B 94.78(13) . 2_656 ?
N1B Ni4 O1B 91.54(12) . . ?
N1B Ni4 O6B 172.76(12) . . ?
O1B Ni4 O6B 82.05(11) . . ?
N1B Ni4 N2B 102.2(2) . . ?
O1B Ni4 N2B 96.95(18) . . ?
O6B Ni4 N2B 82.0(2) . . ?
N1B Ni4 O3B 79.96(13) . . ?
O1B Ni4 O3B 171.41(12) . . ?
O6B Ni4 O3B 106.36(12) . . ?
N2B Ni4 O3B 86.13(18) . . ?
N1B Ni4 N3B 94.36(14) . . ?
O1B Ni4 N3B 90.62(14) . . ?
O6B Ni4 N3B 82.41(13) . . ?
N2B Ni4 N3B 161.5(2) . . ?
O3B Ni4 N3B 88.83(15) . . ?
C1B O1B Ni4 129.3(3) . . ?
C1B O1B Ni3 130.8(3) . . ?
Ni4 O1B Ni3 99.60(11) . . ?
O1B C1B C2B 121.5(3) . . ?
O1B C1B C6B 120.7(4) . . ?
C2B C1B C6B 117.8(3) . . ?
C3B C2B C1B 119.9(4) . . ?
C3B C2B C9B 114.9(4) . . ?
C1B C2B C9B 125.1(3) . . ?
C4B C3B C2B 122.6(4) . . ?
C4B C3B H3B 118.7 . . ?
C2B C3B H3B 118.7 . . ?
C5B C4B C3B 117.2(4) . . ?
C5B C4B C7B 121.6(5) . . ?
C3B C4B C7B 121.1(5) . . ?
C4B C5B C6B 123.7(4) . . ?
C4B C5B H5B 118.1 . . ?
C6B C5B H5B 118.1 . . ?
C5B C6B C1B 118.8(4) . . ?
C5B C6B C8B 116.9(4) . . ?
C1B C6B C8B 124.3(4) . . ?
C4B C7B H7B1 109.5 . . ?
C4B C7B H7B2 109.5 . . ?
H7B1 C7B H7B2 109.5 . . ?
C4B C7B H7B3 109.5 . . ?
H7B1 C7B H7B3 109.5 . . ?
H7B2 C7B H7B3 109.5 . . ?
O2B C8B C6B 127.6(4) . . ?
O2B C8B H8B 116.2 . . ?
C6B C8B H8B 116.2 . . ?
C8B O2B Ni3 126.8(3) . . ?
N1B C9B C2B 127.3(4) . . ?
N1B C9B H9B 116.3 . . ?
C2B C9B H9B 116.3 . . ?
C9B N1B C10B 119.2(4) . . ?
C9B N1B Ni4 124.5(3) . . ?
C10B N1B Ni4 116.3(2) . . ?
N1B C10B C13B 115.0(4) . . ?
N1B C10B C11B 105.9(3) . . ?
C13B C10B C11B 108.0(4) . . ?
N1B C10B C12B 106.6(4) . . ?
C13B C10B C12B 111.6(4) . . ?
C11B C10B C12B 109.4(4) . . ?
O3B C11B C10B 110.1(4) . . ?
O3B C11B H11C 109.6 . . ?
C10B C11B H11C 109.6 . . ?
O3B C11B H11D 109.6 . . ?
C10B C11B H11D 109.6 . . ?
H11C C11B H11D 108.2 . . ?
C11B O3B Ni4 110.4(2) . . ?
C11B O3B H3B1 124.8 . . ?
Ni4 O3B H3B1 124.8 . . ?
O4B1 C12B C10B 112.6(5) . . ?
O4B1 C12B H12C 109.1 . . ?
C10B C12B H12C 109.1 . . ?
O4B1 C12B H12D 109.1 . . ?
C10B C12B H12D 109.1 . . ?
H12C C12B H12D 107.8 . . ?
C12B O4B1 H4B1 109.5 . . ?
C10B C13B H13D 109.5 . . ?
C10B C13B H13E 109.5 . . ?
H13D C13B H13E 109.5 . . ?
C10B C13B H13F 109.5 . . ?
H13D C13B H13F 109.5 . . ?
H13E C13B H13F 109.5 . . ?
C15B C14B C16B 116.0(5) . . ?
C15B C14B C17B 111.2(6) . . ?
C16B C14B C17B 107.8(5) . . ?
C15B C14B N2B 106.1(4) . . ?
C16B C14B N2B 106.2(4) . . ?
C17B C14B N2B 109.3(5) . . ?
C14B N2B Ni4 109.0(3) . . ?
C14B N2B H2B1 109.9 . . ?
Ni4 N2B H2B1 109.9 . . ?
C14B N2B H2B2 109.9 . . ?
Ni4 N2B H2B2 109.9 . . ?
H2B1 N2B H2B2 108.3 . . ?
O5B C15B C14B 117.2(6) . . ?
O5B C15B H15C 108.0 . . ?
C14B C15B H15C 108.0 . . ?
O5B C15B H15D 108.0 . . ?
C14B C15B H15D 108.0 . . ?
H15C C15B H15D 107.2 . . ?
C15B O5B Ni3 124.2(4) . . ?
C15B O5B H5B1 117.9 . . ?
Ni3 O5B H5B1 117.9 . . ?
O6B C16B C14B 109.4(3) . . ?
O6B C16B H16C 109.8 . . ?
C14B C16B H16C 109.8 . . ?
O6B C16B H16D 109.8 . . ?
C14B C16B H16D 109.8 . . ?
H16C C16B H16D 108.2 . . ?
C16B O6B Ni4 112.3(3) . . ?
C16B O6B Ni3 126.5(2) . 2_656 ?
Ni4 O6B Ni3 100.92(12) . 2_656 ?
C16B O6B Ni3 117.2(3) . . ?
Ni4 O6B Ni3 97.23(11) . . ?
Ni3 O6B Ni3 97.81(13) 2_656 . ?
C14B C17B H17D 109.5 . . ?
C14B C17B H17E 109.5 . . ?
H17D C17B H17E 109.5 . . ?
C14B C17B H17F 109.5 . . ?
H17D C17B H17F 109.5 . . ?
H17E C17B H17F 109.5 . . ?
C18B N3B Ni3 136.4(4) . 2_656 ?
C18B N3B Ni4 130.1(4) . . ?
Ni3 N3B Ni4 93.19(15) 2_656 . ?
N3B C18B S1B 179.4(6) . . ?
H1W O1W H2W 110.1(6) . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C1 O1 H1 109.5 . . ?

_refine_diff_density_max         1.294
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.126

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_Complex3a
_database_code_depnum_ccdc_archive 'CCDC 1835113'
_audit_update_record             
;
2018-04-05 deposited with the CCDC.
2018-09-04 downloaded from the CCDC.
;
_audit_creation_date             2018-03-13
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C36 H52 N6 Ni4 O12 S2, 2(N O3)'
_chemical_formula_sum            'C36 H52 N8 Ni4 O18 S2'
_chemical_formula_weight         1183.74
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.0157(14)
_cell_length_b                   25.622(3)
_cell_length_c                   20.278(2)
_cell_angle_alpha                90
_cell_angle_beta                 95.703(5)
_cell_angle_gamma                90
_cell_volume                     6212.0(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    46969
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      24.870
_cell_measurement_theta_min      2.880
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.322
_exptl_absorpt_correction_T_max  0.799
_exptl_absorpt_correction_T_min  0.679
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.17
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            46969
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        24.870
_diffrn_reflns_theta_max         24.870
_diffrn_reflns_theta_min         2.880
_diffrn_ambient_temperature      300.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine focus sealed tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7847
_reflns_number_total             10793
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_refine_diff_density_max         1.611
_refine_diff_density_min         -1.405
_refine_diff_density_rms         0.146
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         10720
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.1136
_refine_ls_R_factor_gt           0.0915
_refine_ls_restrained_S_all      1.102
_refine_ls_shift/su_max          0.049
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1205P)²+52.2339P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2761
_refine_ls_wR_factor_ref         0.2931
_refine_special_details          ?

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
O5 O 0.0770(6) 0.2998(3) 0.6592(4) 0.072(2) Uani 1 1 d . . . . .
H5 H 0.0608 0.3270 0.6295 0.087 Uiso 1 1 calc R . . . .
O11 O 0.5266(6) 0.2019(3) 0.8290(3) 0.0642(19) Uani 1 1 d . . . . .
H11 H 0.5426 0.1745 0.8585 0.077 Uiso 1 1 calc R . . . .
N2 N 0.0812(6) 0.1938(3) 0.6163(4) 0.057(2) Uani 1 1 d . . . . .
H2A H 0.0678 0.2174 0.5843 0.069 Uiso 1 1 calc R . . . .
H2B H 0.0534 0.1634 0.6012 0.069 Uiso 1 1 calc R . . . .
N5 N 0.5211(6) 0.3071(3) 0.8732(4) 0.057(2) Uani 1 1 d . . . . .
H5A H 0.5499 0.3370 0.8892 0.068 Uiso 1 1 calc R . . . .
H5B H 0.5329 0.2828 0.9046 0.068 Uiso 1 1 calc R . . . .
C31 C 0.1061(7) 0.2025(4) 0.7388(4) 0.049(2) Uani 1 1 d . . . . .
H31A H 0.0819 0.2221 0.7758 0.059 Uiso 1 1 calc R . . . .
H31B H 0.1077 0.1659 0.7508 0.059 Uiso 1 1 calc R . . . .
C30 C 0.0226(8) 0.2107(5) 0.6780(5) 0.065(3) Uani 1 1 d . . . . .
C33 C 0.4975(7) 0.2988(4) 0.7491(4) 0.047(2) Uani 1 1 d . . . . .
H33A H 0.4974 0.3352 0.7361 0.057 Uiso 1 1 calc R . . . .
H33B H 0.5215 0.2782 0.7129 0.057 Uiso 1 1 calc R . . . .
C32 C 0.5790(8) 0.2907(5) 0.8114(5) 0.062(3) Uani 1 1 d . . . . .
C34 C 0.6147(8) 0.2350(5) 0.8187(5) 0.069(3) Uani 1 1 d . . . . .
H34A H 0.6474 0.2241 0.7790 0.083 Uiso 1 1 calc R . . . .
H34B H 0.6719 0.2319 0.8558 0.083 Uiso 1 1 calc R . . . .
C29 C -0.0126(10) 0.2657(6) 0.6699(6) 0.082(4) Uani 1 1 d . . . . .
H29A H -0.0696 0.2684 0.6327 0.098 Uiso 1 1 calc R . . . .
H29B H -0.0458 0.2768 0.7093 0.098 Uiso 1 1 calc R . . . .
C36 C -0.0805(10) 0.1770(6) 0.6832(7) 0.091(4) Uani 1 1 d . . . . .
H36A H -0.0597 0.1408 0.6828 0.136 Uiso 1 1 calc GR . . . .
H36B H -0.1347 0.1840 0.6462 0.136 Uiso 1 1 calc GR . . . .
H36C H -0.1122 0.1848 0.7237 0.136 Uiso 1 1 calc GR . . . .
C35 C 0.6822(10) 0.3235(6) 0.8028(7) 0.089(4) Uani 1 1 d . . . . .
H35A H 0.7314 0.3229 0.8431 0.133 Uiso 1 1 calc GR . . . .
H35B H 0.6601 0.3588 0.7926 0.133 Uiso 1 1 calc GR . . . .
H35C H 0.7203 0.3095 0.7673 0.133 Uiso 1 1 calc GR . . . .
O14 O 0.5521(9) 0.2254(5) 0.9929(4) 0.098(3) Uani 1 1 d . . . . .
O13 O 0.5586(11) 0.1520(5) 0.9419(5) 0.121(4) Uani 1 1 d . . . . .
O15 O 0.5474(10) 0.1513(5) 1.0445(4) 0.121(4) Uani 1 1 d . . . . .
N7 N 0.5523(9) 0.1779(7) 0.9929(5) 0.094(4) Uani 1 1 d . . . . .
O18A O 0.567(2) 0.4500(9) 0.8303(14) 0.175(6) Uani 0.6 1 d D . P . .
N8A N 0.5726(19) 0.4941(9) 0.8560(10) 0.111(7) Uani 0.6 1 d D . P . .
O16A O 0.486(2) 0.5247(9) 0.8513(14) 0.175(6) Uani 0.6 1 d D . P . .
O17A O 0.655(2) 0.5104(9) 0.8885(14) 0.175(6) Uani 0.6 1 d D . P . .
O18B O 0.380(3) 0.0423(12) 0.7594(18) 0.184(10) Uani 0.4 1 d D . P . .
N8B N 0.307(2) 0.0105(10) 0.7701(11) 0.19(3) Uani 0.4 1 d D . P . .
O17B O 0.205(2) 0.0242(13) 0.7605(17) 0.184(10) Uani 0.4 1 d D . P . .
O16B O 0.332(3) -0.0360(11) 0.7819(16) 0.184(10) Uani 0.4 1 d D . P . .
Ni2 Ni 0.25444(9) 0.18675(4) 0.64076(5) 0.0387(3) Uani 1 1 d . . . . .
Ni1 Ni 0.23979(9) 0.29517(4) 0.70268(5) 0.0408(3) Uani 1 1 d . . . . .
Ni3 Ni 0.36266(9) 0.20699(4) 0.78553(5) 0.0387(3) Uani 1 1 d . . . . .
Ni4 Ni 0.34924(8) 0.31579(4) 0.84696(5) 0.0373(3) Uani 1 1 d . . . . .
S2 S -0.0194(2) 0.34379(16) 0.84208(18) 0.0865(10) Uani 1 1 d . . . . .
S1 S 0.6228(2) 0.15467(15) 0.64935(17) 0.0813(9) Uani 1 1 d . . . . .
O12 O 0.3873(4) 0.2835(2) 0.7616(2) 0.0372(12) Uani 1 1 d . . . . .
O6 O 0.2149(4) 0.2188(2) 0.7272(2) 0.0373(12) Uani 1 1 d . . . . .
O1 O 0.2881(5) 0.2611(2) 0.6201(3) 0.0442(14) Uani 1 1 d . . . . .
N3 N 0.4191(6) 0.1786(3) 0.6967(3) 0.0459(17) Uani 1 1 d . . . . .
O7 O 0.3153(5) 0.2417(2) 0.8680(3) 0.0413(13) Uani 1 1 d . . . . .
N4 N 0.2947(5) 0.3416(3) 0.9308(3) 0.0392(15) Uani 1 1 d . . . . .
N1 N 0.3110(6) 0.1613(3) 0.5564(3) 0.0394(15) Uani 1 1 d . . . . .
N6 N 0.1822(6) 0.3236(3) 0.7918(3) 0.0460(17) Uani 1 1 d . . . . .
O3 O 0.2344(6) 0.1060(3) 0.6538(3) 0.0576(17) Uani 1 1 d . . . . .
H3 H 0.1843 0.0900 0.6796 0.069 Uiso 1 1 calc R . . . .
O8 O 0.3264(7) 0.1380(3) 0.8229(4) 0.072(2) Uani 1 1 d . . . . .
O9 O 0.3673(6) 0.3964(3) 0.8310(3) 0.0568(16) Uani 1 1 d . . . . .
H9 H 0.4141 0.4121 0.8030 0.068 Uiso 1 1 calc R . . . .
C14 C 0.2773(7) 0.2223(3) 0.9206(4) 0.0405(19) Uani 1 1 d . . . . .
C9 C 0.3493(8) 0.1908(4) 0.5140(4) 0.047(2) Uani 1 1 d . . . . .
H9A H 0.3764 0.1743 0.4780 0.057 Uiso 1 1 calc R . . . .
C5 C 0.3956(8) 0.2706(4) 0.4591(5) 0.056(2) Uani 1 1 d . . . . .
H5C H 0.4171 0.2488 0.4259 0.067 Uiso 1 1 calc R . . . .
C27 C 0.5049(8) 0.1689(4) 0.6773(4) 0.047(2) Uani 1 1 d . . . . .
C21 C 0.2535(7) 0.3121(3) 0.9735(4) 0.044(2) Uani 1 1 d . . . . .
H21 H 0.2249 0.3289 1.0088 0.053 Uiso 1 1 calc R . . . .
O2 O 0.2769(8) 0.3645(3) 0.6655(4) 0.082(2) Uani 1 1 d . . . . .
C22 C 0.2985(7) 0.3992(3) 0.9408(4) 0.046(2) Uani 1 1 d . . . . .
C6 C 0.3560(8) 0.2478(4) 0.5149(4) 0.048(2) Uani 1 1 d . . . . .
C10 C 0.3085(7) 0.1046(4) 0.5462(4) 0.047(2) Uani 1 1 d . . . . .
C3 C 0.3735(10) 0.3550(4) 0.5013(5) 0.068(3) Uani 1 1 d . . . . .
H3A H 0.3792 0.3910 0.4969 0.081 Uiso 1 1 calc R . . . .
C1 C 0.3243(7) 0.2809(4) 0.5670(4) 0.046(2) Uani 1 1 d . . . . .
C18 C 0.2059(9) 0.2323(4) 1.0282(5) 0.057(2) Uani 1 1 d . . . . .
H18 H 0.1861 0.2542 1.0618 0.069 Uiso 1 1 calc R . . . .
C28 C 0.0983(8) 0.3322(4) 0.8128(4) 0.048(2) Uani 1 1 d . . . . .
C15 C 0.2640(8) 0.1677(4) 0.9286(4) 0.051(2) Uani 1 1 d . . . . .
C16 C 0.2237(9) 0.1483(4) 0.9857(5) 0.062(3) Uani 1 1 d . . . . .
H16 H 0.2167 0.1124 0.9901 0.074 Uiso 1 1 calc R . . . .
C17 C 0.1935(10) 0.1798(4) 1.0363(5) 0.064(3) Uani 1 1 d . . . . .
C2 C 0.3340(9) 0.3358(4) 0.5591(4) 0.053(2) Uani 1 1 d . . . . .
C19 C 0.2464(7) 0.2554(3) 0.9730(4) 0.0427(19) Uani 1 1 d . . . . .
C25 C 0.4105(8) 0.4123(4) 0.9794(5) 0.057(2) Uani 1 1 d . . . . .
H25A H 0.4706 0.3991 0.9555 0.068 Uiso 1 1 calc R . . . .
H25B H 0.4184 0.4500 0.9826 0.068 Uiso 1 1 calc R . . . .
C4 C 0.4044(10) 0.3244(4) 0.4508(5) 0.064(3) Uani 1 1 d . . . . .
O10 O 0.4201(7) 0.3909(3) 1.0436(4) 0.080(2) Uani 1 1 d . . . . .
H10 H 0.4274 0.4144 1.0711 0.120 Uiso 1 1 calc R . . . .
O4 O 0.1883(8) 0.1113(4) 0.4449(4) 0.094(3) Uani 1 1 d . . . . .
H4 H 0.1842 0.0876 0.4175 0.142 Uiso 1 1 calc R . . . .
C26 C 0.2895(10) 0.1297(4) 0.8799(5) 0.061(3) Uani 1 1 d . . . . .
H26 H 0.2781 0.0950 0.8906 0.073 Uiso 1 1 calc R . . . .
C11 C 0.3118(9) 0.0801(4) 0.6157(5) 0.057(2) Uani 1 1 d . . . . .
H11A H 0.2929 0.0434 0.6117 0.069 Uiso 1 1 calc R . . . .
H11B H 0.3867 0.0830 0.6381 0.069 Uiso 1 1 calc R . . . .
C13 C 0.1974(9) 0.0902(4) 0.5082(5) 0.064(3) Uani 1 1 d . . . . .
H13A H 0.1912 0.0525 0.5053 0.077 Uiso 1 1 calc R . . . .
H13B H 0.1367 0.1030 0.5319 0.077 Uiso 1 1 calc R . . . .
C24 C 0.2001(9) 0.4213(4) 0.9743(5) 0.062(3) Uani 1 1 d . . . . .
H24A H 0.1313 0.4078 0.9526 0.094 Uiso 1 1 calc GR . . . .
H24B H 0.2001 0.4587 0.9710 0.094 Uiso 1 1 calc GR . . . .
H24C H 0.2070 0.4112 1.0201 0.094 Uiso 1 1 calc GR . . . .
C12 C 0.4064(9) 0.0829(4) 0.5139(5) 0.062(3) Uani 1 1 d . . . . .
H12A H 0.3993 0.0921 0.4678 0.093 Uiso 1 1 calc GR . . . .
H12B H 0.4074 0.0455 0.5182 0.093 Uiso 1 1 calc GR . . . .
H12C H 0.4747 0.0970 0.5353 0.093 Uiso 1 1 calc GR . . . .
C23 C 0.2939(8) 0.4223(4) 0.8716(5) 0.056(2) Uani 1 1 d . . . . .
H23A H 0.2179 0.4200 0.8507 0.068 Uiso 1 1 calc R . . . .
H23B H 0.3139 0.4590 0.8750 0.068 Uiso 1 1 calc R . . . .
C20 C 0.1490(14) 0.1577(6) 1.0974(6) 0.099(5) Uani 1 1 d . . . . .
H20A H 0.1371 0.1209 1.0918 0.148 Uiso 1 1 calc GR . . . .
H20B H 0.0795 0.1744 1.1040 0.148 Uiso 1 1 calc GR . . . .
H20C H 0.2021 0.1638 1.1352 0.148 Uiso 1 1 calc GR . . . .
C8 C 0.3092(10) 0.3731(4) 0.6082(5) 0.067(3) Uani 1 1 d . . . . .
H8 H 0.3177 0.4080 0.5971 0.080 Uiso 1 1 calc R . . . .
C7 C 0.4478(13) 0.3466(6) 0.3888(6) 0.094(4) Uani 1 1 d . . . . .
H7A H 0.4551 0.3838 0.3931 0.140 Uiso 1 1 calc GR . . . .
H7B H 0.3964 0.3385 0.3510 0.140 Uiso 1 1 calc GR . . . .
H7C H 0.5195 0.3316 0.3833 0.140 Uiso 1 1 calc GR . . . .


_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
O5 C29 1.420(15) . ?
O5 Ni1 2.067(7) . ?
O11 C34 1.388(13) . ?
O11 Ni3 2.080(7) . ?
N2 C30 1.558(12) . ?
N2 Ni2 2.100(7) . ?
N5 C32 1.550(13) . ?
N5 Ni4 2.093(8) . ?
C31 C30 1.525(13) . ?
C31 O6 1.414(9) . ?
C30 C29 1.476(18) . ?
C30 C36 1.523(15) . ?
C33 C32 1.534(12) . ?
C33 O12 1.428(10) . ?
C32 C34 1.495(16) . ?
C32 C35 1.522(14) . ?
O14 N7 1.217(16) . ?
O13 N7 1.238(15) . ?
O15 N7 1.256(15) . ?
O18A N8A 1.244(17) . ?
N8A O16A 1.299(17) . ?
N8A O17A 1.203(17) . ?
O18B N8B 1.234(19) . ?
N8B O17B 1.267(19) . ?
N8B O16B 1.248(19) . ?
Ni2 O6 2.033(5) . ?
Ni2 O1 2.001(6) . ?
Ni2 N3 2.191(7) . ?
Ni2 N1 2.012(7) . ?
Ni2 O3 2.104(7) . ?
Ni1 O12 2.058(5) . ?
Ni1 O6 2.049(6) . ?
Ni1 O1 2.023(6) . ?
Ni1 N6 2.127(7) . ?
Ni1 O2 1.998(9) . ?
Ni3 O12 2.047(6) . ?
Ni3 O6 2.056(5) . ?
Ni3 N3 2.115(7) . ?
Ni3 O7 2.025(5) . ?
Ni3 O8 1.988(8) . ?
Ni4 O12 2.011(5) . ?
Ni4 O7 1.996(6) . ?
Ni4 N4 1.995(7) . ?
Ni4 N6 2.208(7) . ?
Ni4 O9 2.105(7) . ?
S2 C28 1.615(10) . ?
S1 C27 1.618(10) . ?
O1 C1 1.303(10) . ?
N3 C27 1.167(11) . ?
O7 C14 1.300(9) . ?
N4 C21 1.285(11) . ?
N4 C22 1.489(11) . ?
N1 C9 1.266(11) . ?
N1 C10 1.466(11) . ?
N6 C28 1.154(11) . ?
O3 C11 1.429(12) . ?
O8 C26 1.294(12) . ?
O9 C23 1.429(11) . ?
C14 C15 1.421(13) . ?
C14 C19 1.437(11) . ?
C9 C6 1.462(13) . ?
C5 C6 1.397(12) . ?
C5 C4 1.396(15) . ?
C21 C19 1.456(12) . ?
O2 C8 1.279(13) . ?
C22 C25 1.525(12) . ?
C22 C24 1.530(13) . ?
C22 C23 1.519(13) . ?
C6 C1 1.436(12) . ?
C10 C11 1.541(13) . ?
C10 C13 1.519(13) . ?
C10 C12 1.508(13) . ?
C3 C2 1.395(14) . ?
C3 C4 1.370(15) . ?
C1 C2 1.423(13) . ?
C18 C17 1.366(15) . ?
C18 C19 1.396(12) . ?
C15 C16 1.389(12) . ?
C15 C26 1.441(13) . ?
C16 C17 1.381(15) . ?
C17 C20 1.508(14) . ?
C2 C8 1.433(14) . ?
C25 O10 1.408(12) . ?
C4 C7 1.517(14) . ?
O4 C13 1.388(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C29 O5 Ni1 126.9(7) . . ?
C34 O11 Ni3 127.0(7) . . ?
C30 N2 Ni2 110.5(5) . . ?
C32 N5 Ni4 109.5(5) . . ?
O6 C31 C30 111.7(7) . . ?
C31 C30 N2 107.4(7) . . ?
C29 C30 N2 108.8(10) . . ?
C29 C30 C31 112.3(9) . . ?
C29 C30 C36 108.9(10) . . ?
C36 C30 N2 109.5(9) . . ?
C36 C30 C31 110.0(10) . . ?
O12 C33 C32 110.1(7) . . ?
C33 C32 N5 109.2(8) . . ?
C34 C32 N5 109.0(8) . . ?
C34 C32 C33 111.3(9) . . ?
C34 C32 C35 108.0(10) . . ?
C35 C32 N5 112.3(9) . . ?
C35 C32 C33 107.0(8) . . ?
O11 C34 C32 112.5(8) . . ?
O5 C29 C30 113.0(9) . . ?
O14 N7 O13 122.5(13) . . ?
O14 N7 O15 122.9(13) . . ?
O13 N7 O15 114.6(16) . . ?
O18A N8A O16A 121(3) . . ?
O17A N8A O18A 123(3) . . ?
O17A N8A O16A 116(3) . . ?
O18B N8B O17B 119.0(16) . . ?
O18B N8B O16B 120.2(16) . . ?
O16B N8B O17B 120.2(16) . . ?
N2 Ni2 N3 162.5(3) . . ?
N2 Ni2 O3 89.5(3) . . ?
O6 Ni2 N2 81.8(3) . . ?
O6 Ni2 N3 82.4(2) . . ?
O6 Ni2 O3 104.4(2) . . ?
O1 Ni2 N2 94.8(3) . . ?
O1 Ni2 O6 82.3(2) . . ?
O1 Ni2 N3 90.5(3) . . ?
O1 Ni2 N1 92.2(3) . . ?
O1 Ni2 O3 172.5(2) . . ?
N1 Ni2 N2 103.8(3) . . ?
N1 Ni2 O6 172.5(2) . . ?
N1 Ni2 N3 92.6(3) . . ?
N1 Ni2 O3 80.8(3) . . ?
O3 Ni2 N3 87.1(3) . . ?
O5 Ni1 N6 88.2(3) . . ?
O12 Ni1 O5 168.3(3) . . ?
O12 Ni1 N6 83.7(2) . . ?
O6 Ni1 O5 90.2(3) . . ?
O6 Ni1 O12 81.9(2) . . ?
O6 Ni1 N6 93.1(3) . . ?
O1 Ni1 O5 90.5(3) . . ?
O1 Ni1 O12 96.7(2) . . ?
O1 Ni1 O6 81.3(2) . . ?
O1 Ni1 N6 174.3(3) . . ?
O2 Ni1 O5 91.4(4) . . ?
O2 Ni1 O12 97.9(3) . . ?
O2 Ni1 O6 170.0(3) . . ?
O2 Ni1 O1 88.7(3) . . ?
O2 Ni1 N6 96.9(3) . . ?
O11 Ni3 N3 88.2(3) . . ?
O12 Ni3 O11 90.4(3) . . ?
O12 Ni3 O6 82.0(2) . . ?
O12 Ni3 N3 93.5(3) . . ?
O6 Ni3 O11 168.6(3) . . ?
O6 Ni3 N3 83.8(2) . . ?
O7 Ni3 O11 90.6(3) . . ?
O7 Ni3 O12 80.4(2) . . ?
O7 Ni3 O6 96.5(2) . . ?
O7 Ni3 N3 173.9(3) . . ?
O8 Ni3 O11 91.0(3) . . ?
O8 Ni3 O12 169.5(3) . . ?
O8 Ni3 O6 98.1(3) . . ?
O8 Ni3 N3 96.9(3) . . ?
O8 Ni3 O7 89.1(3) . . ?
N5 Ni4 N6 164.4(3) . . ?
N5 Ni4 O9 91.7(3) . . ?
O12 Ni4 N5 82.7(3) . . ?
O12 Ni4 N6 82.8(2) . . ?
O12 Ni4 O9 103.6(2) . . ?
O7 Ni4 N5 93.5(3) . . ?
O7 Ni4 O12 82.0(2) . . ?
O7 Ni4 N6 90.0(3) . . ?
O7 Ni4 O9 172.8(2) . . ?
N4 Ni4 N5 102.6(3) . . ?
N4 Ni4 O12 172.6(3) . . ?
N4 Ni4 O7 92.4(3) . . ?
N4 Ni4 N6 92.4(3) . . ?
N4 Ni4 O9 81.5(3) . . ?
O9 Ni4 N6 86.3(3) . . ?
C33 O12 Ni1 128.1(5) . . ?
C33 O12 Ni3 117.6(5) . . ?
C33 O12 Ni4 109.5(5) . . ?
Ni3 O12 Ni1 98.1(2) . . ?
Ni4 O12 Ni1 100.6(2) . . ?
Ni4 O12 Ni3 98.0(2) . . ?
C31 O6 Ni2 109.0(5) . . ?
C31 O6 Ni1 118.7(5) . . ?
C31 O6 Ni3 128.4(5) . . ?
Ni2 O6 Ni1 97.1(2) . . ?
Ni2 O6 Ni3 100.1(2) . . ?
Ni1 O6 Ni3 98.1(2) . . ?
Ni2 O1 Ni1 99.0(2) . . ?
C1 O1 Ni2 129.3(6) . . ?
C1 O1 Ni1 131.5(6) . . ?
Ni3 N3 Ni2 93.4(3) . . ?
C27 N3 Ni2 129.0(6) . . ?
C27 N3 Ni3 136.8(7) . . ?
Ni4 O7 Ni3 99.3(2) . . ?
C14 O7 Ni3 131.3(5) . . ?
C14 O7 Ni4 129.4(5) . . ?
C21 N4 Ni4 124.0(6) . . ?
C21 N4 C22 120.0(7) . . ?
C22 N4 Ni4 115.9(5) . . ?
C9 N1 Ni2 124.1(6) . . ?
C9 N1 C10 120.0(7) . . ?
C10 N1 Ni2 115.9(5) . . ?
Ni1 N6 Ni4 92.5(3) . . ?
C28 N6 Ni1 138.5(7) . . ?
C28 N6 Ni4 127.8(6) . . ?
C11 O3 Ni2 107.4(5) . . ?
C26 O8 Ni3 126.5(7) . . ?
C23 O9 Ni4 106.8(5) . . ?
O7 C14 C15 121.6(7) . . ?
O7 C14 C19 121.3(8) . . ?
C15 C14 C19 117.1(7) . . ?
N1 C9 C6 127.7(8) . . ?
C6 C5 C4 123.1(9) . . ?
N3 C27 S1 178.9(9) . . ?
N4 C21 C19 127.5(8) . . ?
C8 O2 Ni1 126.5(7) . . ?
N4 C22 C25 107.6(7) . . ?
N4 C22 C24 114.3(8) . . ?
N4 C22 C23 105.2(7) . . ?
C25 C22 C24 111.9(8) . . ?
C23 C22 C25 109.7(8) . . ?
C23 C22 C24 107.8(8) . . ?
C5 C6 C9 115.4(8) . . ?
C5 C6 C1 119.1(9) . . ?
C1 C6 C9 125.4(8) . . ?
N1 C10 C11 106.0(7) . . ?
N1 C10 C13 108.5(8) . . ?
N1 C10 C12 115.0(8) . . ?
C13 C10 C11 107.7(8) . . ?
C12 C10 C11 107.2(8) . . ?
C12 C10 C13 112.0(8) . . ?
C4 C3 C2 124.6(10) . . ?
O1 C1 C6 121.0(8) . . ?
O1 C1 C2 121.0(8) . . ?
C2 C1 C6 118.0(8) . . ?
C17 C18 C19 124.3(9) . . ?
N6 C28 S2 179.6(10) . . ?
C14 C15 C26 123.5(8) . . ?
C16 C15 C14 120.0(9) . . ?
C16 C15 C26 116.5(9) . . ?
C17 C16 C15 123.3(10) . . ?
C18 C17 C16 116.5(9) . . ?
C18 C17 C20 121.3(10) . . ?
C16 C17 C20 122.2(11) . . ?
C3 C2 C1 118.8(9) . . ?
C3 C2 C8 117.4(9) . . ?
C1 C2 C8 123.8(9) . . ?
C14 C19 C21 125.1(8) . . ?
C18 C19 C14 118.7(8) . . ?
C18 C19 C21 116.2(8) . . ?
O10 C25 C22 112.0(8) . . ?
C5 C4 C7 120.4(10) . . ?
C3 C4 C5 116.4(9) . . ?
C3 C4 C7 123.2(11) . . ?
O8 C26 C15 128.0(9) . . ?
O3 C11 C10 110.3(8) . . ?
O4 C13 C10 111.0(9) . . ?
O9 C23 C22 112.5(8) . . ?
O2 C8 C2 128.3(10) . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.267 0.000 0.000 791.1 0.0 ?
2 -0.067 0.500 0.500 791.1 0.0 ?

_olex2_submission_special_instructions 'No special instructions were received'

####################################################################### 
# 
# 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_Complex2
_database_code_depnum_ccdc_archive 'CCDC 1835112'
_audit_update_record             
;
2018-04-05 deposited with the CCDC.
2018-09-04 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT430_Complex2            
;
PROBLEM: Short Inter D...A Contact  O2W      ..O2W              2.77 Ang.
RESPONSE: This is due to disorder
;
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C40 H61 N4 Ni4 O16, (C3 H5 O2), (N O3), (C2 H3 N), (H O), 0.5 O'
_chemical_formula_sum            'C45 H72 N6 Ni4 O22.50'
_chemical_formula_weight         1291.83

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   11.186(3)
_cell_length_b                   12.760(4)
_cell_length_c                   19.351(5)
_cell_angle_alpha                95.105(7)
_cell_angle_beta                 95.350(7)
_cell_angle_gamma                94.242(7)
_cell_volume                     2729.6(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    33595
_cell_measurement_theta_min      1.062
_cell_measurement_theta_max      26.418

_exptl_crystal_description       Block
_exptl_crystal_colour            Green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_F_000             1348
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.17
_exptl_absorpt_coefficient_mu    1.443
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.655
_exptl_absorpt_correction_T_max  0.782
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            33595
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.062
_diffrn_reflns_theta_max         26.418
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measured_fraction_theta_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_point_group_measured_fraction_full 0.983
_reflns_number_total             10741
_reflns_number_gt                9064
_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 SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0717P)²+2.4289P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10741
_refine_ls_number_parameters     797
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0403
_refine_ls_wR_factor_ref         0.1214
_refine_ls_wR_factor_gt          0.1126
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.09
_refine_ls_shift/su_mean         0.009

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
O15A O 0.4980(3) 0.5605(3) 0.1324(2) 0.0246(9) Uani 0.6 1 d . . P . .
H15A H 0.4375 0.5469 0.1520 0.037 Uiso 0.6 1 calc R U P . .
C39 C 0.1709(6) 1.0972(3) 0.3862(2) 0.0567(15) Uani 1 1 d . . . . .
H39A H 0.0875 1.0694 0.3851 0.068 Uiso 1 1 calc R U . . .
H39B H 0.1917 1.1407 0.4300 0.068 Uiso 1 1 calc R U . . .
O13 O 0.1813(3) 1.1586(3) 0.33289(17) 0.0612(9) Uani 1 1 d . . . . .
H13 H 0.1368 1.2066 0.3367 0.092 Uiso 1 1 calc R U . . .
H12B H 0.632(3) 0.663(3) 0.1414(17) 0.014(8) Uiso 1 1 d . . . . .
H11A H 0.556(4) 0.907(3) 0.202(2) 0.031(10) Uiso 1 1 d . . . . .
H12A H 0.593(3) 0.638(3) 0.217(2) 0.032(10) Uiso 1 1 d . . . . .
H11B H 0.655(4) 0.832(3) 0.228(2) 0.038(11) Uiso 1 1 d . . . . .
H6 H -0.187(3) 0.645(3) 0.0925(18) 0.018(9) Uiso 1 1 d . . . . .
H8 H -0.172(5) 0.505(4) 0.193(3) 0.075(17) Uiso 1 1 d . . . . .
H16 H 0.028(4) 0.383(4) 0.413(2) 0.055(14) Uiso 1 1 d . . . . .
H5 H 0.020(5) 0.899(4) 0.395(3) 0.061(15) Uiso 1 1 d . . . . .
H14 H -0.167(3) 0.533(3) -0.052(2) 0.042(12) Uiso 1 1 d D . . . .
H15E H -0.167(3) 0.673(3) 0.4230(19) 0.026(10) Uiso 1 1 d . . . . .
H15D H -0.137(3) 0.580(3) 0.4684(19) 0.018(8) Uiso 1 1 d . . . . .
H15C H -0.261(4) 0.572(3) 0.417(2) 0.034(10) Uiso 1 1 d . . . . .
H16A H -0.193(3) 0.378(2) 0.3690(16) 0.011(8) Uiso 1 1 d . . . . .
H28B H -0.027(3) 0.597(3) 0.0210(19) 0.018(6) Uiso 1 1 d . . . . .
H16B H -0.077(3) 0.391(3) 0.3257(19) 0.023(9) Uiso 1 1 d . . . . .
H28A H 0.046(3) 0.626(3) -0.0420(17) 0.018(6) Uiso 1 1 d . . . . .
H7 H 0.312(4) 0.655(2) 0.0678(17) 0.036(11) Uiso 1 1 d D . . . .
H2 H -0.100(3) 0.766(3) 0.2641(19) 0.023(9) Uiso 1 1 d . . . . .
H4 H 0.067(3) 0.5776(19) 0.1311(17) 0.022(10) Uiso 1 1 d D . . . .
H1WA H 0.159(6) 0.407(4) 0.336(2) 0.11(2) Uiso 1 1 d D . . . .
O20 O 0.2782(2) 0.5444(2) 0.00424(12) 0.0353(6) Uani 1 1 d . . . . .
O17 O 0.8791(2) 0.9249(2) 0.42535(14) 0.0433(7) Uani 1 1 d . . . . .
O18 O 0.7906(2) 0.8221(2) 0.33805(13) 0.0366(6) Uani 1 1 d . . . . .
N5 N 0.7834(3) 0.8818(2) 0.39076(16) 0.0305(7) Uani 1 1 d . . . . .
C41 C 0.2717(3) 0.5562(3) -0.05966(17) 0.0272(8) Uani 1 1 d . . . . .
C40 C 0.4881(3) 0.6531(3) 0.53404(17) 0.0303(8) Uani 1 1 d . . . . .
H40A H 0.5693 0.6798 0.5297 0.046 Uiso 1 1 calc R U . . .
H40B H 0.4865 0.5797 0.5416 0.046 Uiso 1 1 calc R U . . .
H40C H 0.4583 0.6917 0.5728 0.046 Uiso 1 1 calc R U . . .
C42A C 0.3541(8) 0.6457(7) -0.0767(4) 0.0259(14) Uani 0.5 1 d . . P A 1
H42A H 0.4361 0.6333 -0.0607 0.031 Uiso 0.5 1 calc R U P A 1
H42B H 0.3348 0.7100 -0.0510 0.031 Uiso 0.5 1 calc R U P A 1
C42B C 0.2970(8) 0.6705(7) -0.0880(4) 0.0259(14) Uani 0.5 1 d . . P A 2
H42C H 0.2221 0.7040 -0.0931 0.031 Uiso 0.5 1 calc R U P A 2
H42D H 0.3523 0.7147 -0.0539 0.031 Uiso 0.5 1 calc R U P A 2
O21 O 0.2210(2) 0.48829(17) -0.10557(11) 0.0198(5) Uani 1 1 d . . . . .
O19 O 0.6840(3) 0.9008(3) 0.40978(17) 0.0515(8) Uani 1 1 d . . . . .
C43 C 0.3480(4) 0.6628(3) -0.1548(2) 0.0448(11) Uani 1 1 d . . . . .
H43A H 0.3988 0.6162 -0.1776 0.067 Uiso 1 1 calc R U . A 1
H43B H 0.3750 0.7346 -0.1598 0.067 Uiso 1 1 calc R U . A 1
H43C H 0.2664 0.6481 -0.1755 0.067 Uiso 1 1 calc R U . A 1
O1W O 0.1598(3) 0.3692(2) 0.37594(15) 0.0451(7) Uani 1 1 d D . . . .
N6 N 0.6001(3) 0.1559(3) 0.2930(2) 0.0490(9) Uani 1 1 d . . . . .
C44 C 0.6662(4) 0.1541(3) 0.3402(2) 0.0399(10) Uani 1 1 d . . . . .
C45 C 0.7511(5) 0.1549(4) 0.4030(2) 0.0591(13) Uani 1 1 d . . . . .
H45A H 0.8027 0.2193 0.4087 0.089 Uiso 1 1 calc R U . . .
H45B H 0.7990 0.0958 0.3982 0.089 Uiso 1 1 calc R U . . .
H45C H 0.7070 0.1502 0.4430 0.089 Uiso 1 1 calc R U . . .
O2W O 0.5342(10) 0.5996(9) -0.0179(6) 0.111(3) Uiso 0.5 1 d . . P . .
O15B O 0.6450(6) 0.8815(5) 0.1317(3) 0.0317(14) Uani 0.4 1 d . . P . .
H15B H 0.6785 0.8332 0.1130 0.048 Uiso 0.4 1 calc R U P . .
Ni1 Ni 0.10364(3) 0.85642(3) 0.27823(2) 0.01456(11) Uani 1 1 d . . . . .
Ni4 Ni 0.03699(3) 0.60604(3) 0.25256(2) 0.01352(10) Uani 1 1 d . . . . .
Ni3 Ni 0.24370(3) 0.68993(3) 0.18779(2) 0.01279(10) Uani 1 1 d . . . . .
Ni2 Ni -0.01472(3) 0.77043(3) 0.14188(2) 0.01312(10) Uani 1 1 d . . . . .
O1 O 0.15614(18) 0.83705(16) 0.18000(10) 0.0136(4) Uani 1 1 d . . . . .
O2 O -0.03474(19) 0.75039(16) 0.24360(10) 0.0151(4) Uani 1 1 d . . . . .
O4 O 0.07155(18) 0.63457(16) 0.15475(10) 0.0132(4) Uani 1 1 d D . . . .
O3 O 0.18841(18) 0.70657(16) 0.28618(10) 0.0141(4) Uani 1 1 d . . . . .
O11 O 0.29150(19) 0.54112(16) 0.19452(10) 0.0172(4) Uani 1 1 d . . . . .
O12 O 0.14103(19) 0.47558(17) 0.25182(10) 0.0172(4) Uani 1 1 d . . . . .
N2 N 0.0227(2) 0.79329(19) 0.04384(12) 0.0140(5) Uani 1 1 d . . . . .
O10 O -0.0892(2) 0.91346(17) 0.15122(11) 0.0195(5) Uani 1 1 d . . . . .
N4 N 0.0033(2) 0.5890(2) 0.35122(12) 0.0160(5) Uani 1 1 d . . . . .
N3 N 0.4121(2) 0.7448(2) 0.22656(12) 0.0151(5) Uani 1 1 d . . . . .
O5 O 0.0852(2) 0.86683(19) 0.38283(11) 0.0226(5) Uani 1 1 d . . . . .
O8 O -0.1277(2) 0.51824(18) 0.23512(11) 0.0196(5) Uani 1 1 d . . . . .
O6 O -0.17643(19) 0.70772(19) 0.09042(11) 0.0165(4) Uani 1 1 d . . . . .
O9 O 0.0078(2) 0.98358(17) 0.25383(11) 0.0200(5) Uani 1 1 d . . . . .
O14 O -0.1129(2) 0.56133(17) -0.07296(11) 0.0185(5) Uani 1 1 d D . . . .
O7 O 0.3145(2) 0.70682(18) 0.09559(11) 0.0174(5) Uani 1 1 d D . . . .
N1 N 0.2466(2) 0.9585(2) 0.30929(13) 0.0172(5) Uani 1 1 d . . . . .
C10 C 0.4297(3) 0.7654(3) 0.10398(15) 0.0184(6) Uani 1 1 d . . . . .
H10A H 0.4184 0.8396 0.1007 0.022 Uiso 1 1 calc R U . . .
H10B H 0.4757 0.7419 0.0663 0.022 Uiso 1 1 calc R U . . .
C26 C -0.0671(3) 0.7379(2) -0.01116(15) 0.0159(6) Uani 1 1 d . . . . .
C14 C -0.1959(3) 0.5532(3) 0.29149(15) 0.0209(7) Uani 1 1 d . . . . .
H14A H -0.2718 0.5103 0.2890 0.025 Uiso 1 1 calc R U . . .
H14B H -0.2128 0.6262 0.2886 0.025 Uiso 1 1 calc R U . . .
O16 O -0.0504(2) 0.3983(2) 0.42713(12) 0.0311(6) Uani 1 1 d . . . . .
C33 C 0.2380(3) 0.4686(2) 0.22409(15) 0.0173(6) Uani 1 1 d . . . . .
C30 C 0.2538(3) 1.0017(3) 0.38358(15) 0.0217(7) Uani 1 1 d . . . . .
C7 C 0.4527(3) 0.7472(2) 0.29104(15) 0.0166(6) Uani 1 1 d . . . . .
H7A H 0.5333 0.7710 0.3025 0.020 Uiso 1 1 calc R U . . .
C3 C 0.2859(3) 0.6375(3) 0.46148(15) 0.0203(7) Uani 1 1 d . . . . .
H3 H 0.2525 0.6107 0.4992 0.024 Uiso 1 1 calc R U . . .
C9 C 0.5018(3) 0.7532(3) 0.17407(15) 0.0178(6) Uani 1 1 d . . . . .
C31 C 0.1905(3) 0.9185(3) 0.42315(16) 0.0233(7) Uani 1 1 d . . . . .
H31A H 0.2460 0.8663 0.4348 0.028 Uiso 1 1 calc R U . . .
H31B H 0.1677 0.9521 0.4664 0.028 Uiso 1 1 calc R U . . .
C21 C 0.3734(3) 1.0566(3) 0.15775(16) 0.0200(7) Uani 1 1 d . . . . .
H21 H 0.4298 1.1040 0.1849 0.024 Uiso 1 1 calc R U . . .
C22 C 0.2990(3) 0.9881(2) 0.19107(15) 0.0173(6) Uani 1 1 d . . . . .
C24 C 0.1091(3) 0.8556(2) 0.02860(15) 0.0170(6) Uani 1 1 d . . . . .
H24 H 0.1150 0.8611 -0.0186 0.020 Uiso 1 1 calc R U . . .
C1 C 0.2597(3) 0.6890(2) 0.34359(14) 0.0152(6) Uani 1 1 d . . . . .
C28 C -0.0307(3) 0.6244(2) -0.02316(15) 0.0165(6) Uani 1 1 d . . . . .
C8 C 0.0823(3) 0.6101(3) 0.40403(15) 0.0190(6) Uani 1 1 d . . . . .
H8A H 0.0573 0.6011 0.4478 0.023 Uiso 1 1 calc R U . . .
C5 C 0.4564(3) 0.7055(3) 0.41114(16) 0.0199(7) Uani 1 1 d . . . . .
H5A H 0.5385 0.7258 0.4142 0.024 Uiso 1 1 calc R U . . .
C11 C 0.5947(3) 0.8477(3) 0.19198(18) 0.0247(7) Uani 1 1 d . . . . .
C6 C 0.3846(3) 0.7162(2) 0.34874(15) 0.0171(6) Uani 1 1 d . . . . .
C37 C -0.1428(3) 1.0792(3) 0.19779(18) 0.0267(7) Uani 1 1 d . . . . .
H37A H -0.1547 1.0950 0.1496 0.032 Uiso 1 1 calc R U . . .
H37B H -0.2215 1.0597 0.2122 0.032 Uiso 1 1 calc R U . . .
C19 C 0.2772(3) 0.9892(2) 0.04726(15) 0.0182(6) Uani 1 1 d . . . . .
H19 H 0.2683 0.9905 -0.0009 0.022 Uiso 1 1 calc R U . . .
C2 C 0.2093(3) 0.6474(2) 0.40091(15) 0.0175(6) Uani 1 1 d . . . . .
C27 C -0.1877(3) 0.7393(2) 0.02103(15) 0.0173(6) Uani 1 1 d . . . . .
H27A H -0.2146 0.8100 0.0221 0.021 Uiso 1 1 calc R U . . .
H27B H -0.2480 0.6919 -0.0078 0.021 Uiso 1 1 calc R U . . .
C36 C -0.0686(3) 0.9844(2) 0.20081(16) 0.0185(6) Uani 1 1 d . . . . .
C12 C 0.5651(3) 0.6504(3) 0.16847(19) 0.0259(8) Uani 1 1 d . . . . .
C20 C 0.3663(3) 1.0565(2) 0.08591(16) 0.0196(7) Uani 1 1 d . . . . .
C17 C 0.2150(3) 0.9136(2) 0.15039(15) 0.0151(6) Uani 1 1 d . . . . .
C29 C -0.0785(3) 0.7886(3) -0.08009(16) 0.0224(7) Uani 1 1 d . . . . .
H29A H -0.0904 0.8621 -0.0710 0.034 Uiso 1 1 calc R U . . .
H29B H -0.1460 0.7539 -0.1099 0.034 Uiso 1 1 calc R U . . .
H29C H -0.0062 0.7815 -0.1026 0.034 Uiso 1 1 calc R U . . .
C25 C 0.3126(3) 1.0039(2) 0.26782(16) 0.0196(7) Uani 1 1 d . . . . .
H25 H 0.3754 1.0516 0.2884 0.023 Uiso 1 1 calc R U . . .
C18 C 0.1997(3) 0.9190(2) 0.07742(15) 0.0165(6) Uani 1 1 d . . . . .
C4 C 0.4093(3) 0.6660(3) 0.46772(16) 0.0222(7) Uani 1 1 d . . . . .
C23 C 0.4519(3) 1.1273(3) 0.05095(17) 0.0251(7) Uani 1 1 d . . . . .
H23A H 0.4358 1.1135 0.0012 0.038 Uiso 1 1 calc R U . . .
H23B H 0.5334 1.1134 0.0648 0.038 Uiso 1 1 calc R U . . .
H23C H 0.4409 1.1999 0.0646 0.038 Uiso 1 1 calc R U . . .
C13 C -0.1195(3) 0.5418(3) 0.35962(15) 0.0202(7) Uani 1 1 d . . . . .
C15 C -0.1760(3) 0.5952(3) 0.42095(17) 0.0265(8) Uani 1 1 d . . . . .
C34 C 0.3036(3) 0.3689(3) 0.22863(17) 0.0248(7) Uani 1 1 d . . . . .
H34A H 0.3296 0.3470 0.1835 0.030 Uiso 1 1 calc R U . . .
H34B H 0.2494 0.3125 0.2414 0.030 Uiso 1 1 calc R U . . .
C35 C 0.4130(4) 0.3893(4) 0.2832(2) 0.0433(10) Uani 1 1 d . . . . .
H35A H 0.4682 0.4429 0.2693 0.065 Uiso 1 1 calc R U . . .
H35B H 0.4524 0.3254 0.2868 0.065 Uiso 1 1 calc R U . . .
H35C H 0.3872 0.4125 0.3275 0.065 Uiso 1 1 calc R U . . .
C38 C -0.0904(4) 1.1786(3) 0.2417(2) 0.0376(9) Uani 1 1 d . . . . .
H38A H -0.0781 1.1646 0.2897 0.056 Uiso 1 1 calc R U . . .
H38B H -0.1450 1.2328 0.2372 0.056 Uiso 1 1 calc R U . . .
H38C H -0.0147 1.2018 0.2261 0.056 Uiso 1 1 calc R U . . .
C16 C -0.1148(3) 0.4228(3) 0.36523(17) 0.0264(7) Uani 1 1 d . . . . .
C32 C 0.3822(4) 1.0293(3) 0.41704(18) 0.0361(9) Uani 1 1 d . . . . .
H32A H 0.4299 0.9713 0.4071 0.054 Uiso 1 1 calc R U . . .
H32B H 0.3817 1.0431 0.4666 0.054 Uiso 1 1 calc R U . . .
H32C H 0.4161 1.0910 0.3986 0.054 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O15A C12 1.414(5) . ?
C39 O13 1.359(5) . ?
C39 C30 1.585(6) . ?
O20 C41 1.255(4) . ?
O17 N5 1.269(4) . ?
O18 N5 1.230(4) . ?
N5 O19 1.238(4) . ?
C41 O21 1.248(4) . ?
C41 C42A 1.493(9) . ?
C41 C42B 1.618(9) . ?
C40 C4 1.516(4) . ?
C42A C43 1.541(9) . ?
C42B C43 1.459(9) . ?
N6 C44 1.124(5) . ?
C44 C45 1.469(6) . ?
O15B C11 1.427(7) . ?
Ni1 N1 1.997(3) . ?
Ni1 O2 2.003(2) . ?
Ni1 O1 2.0409(19) . ?
Ni1 O5 2.047(2) . ?
Ni1 O9 2.074(2) . ?
Ni1 O3 2.207(2) . ?
Ni1 Ni2 2.9217(8) . ?
Ni4 N4 2.008(2) . ?
Ni4 O4 2.025(2) . ?
Ni4 O3 2.064(2) . ?
Ni4 O8 2.067(2) . ?
Ni4 O2 2.077(2) . ?
Ni4 O12 2.100(2) . ?
Ni4 Ni3 2.9113(8) . ?
Ni3 N3 2.012(3) . ?
Ni3 O11 2.022(2) . ?
Ni3 O4 2.026(2) . ?
Ni3 O7 2.040(2) . ?
Ni3 O3 2.0541(19) . ?
Ni3 O1 2.191(2) . ?
Ni2 N2 2.022(2) . ?
Ni2 O2 2.038(2) . ?
Ni2 O6 2.052(2) . ?
Ni2 O10 2.062(2) . ?
Ni2 O4 2.068(2) . ?
Ni2 O1 2.075(2) . ?
O1 C17 1.338(3) . ?
O3 C1 1.351(4) . ?
O11 C33 1.272(4) . ?
O12 C33 1.259(4) . ?
N2 C24 1.278(4) . ?
N2 C26 1.484(4) . ?
O10 C36 1.252(4) . ?
N4 C8 1.282(4) . ?
N4 C13 1.487(4) . ?
N3 C7 1.284(4) . ?
N3 C9 1.498(4) . ?
O5 C31 1.432(4) . ?
O8 C14 1.446(3) . ?
O6 C27 1.433(4) . ?
O9 C36 1.274(4) . ?
O14 C28 1.417(4) . ?
O7 C10 1.429(4) . ?
N1 C25 1.286(4) . ?
N1 C30 1.486(4) . ?
C10 C9 1.539(4) . ?
C26 C29 1.532(4) . ?
C26 C28 1.537(4) . ?
C26 C27 1.539(4) . ?
C14 C13 1.527(4) . ?
O16 C16 1.411(4) . ?
C33 C34 1.520(4) . ?
C30 C32 1.523(5) . ?
C30 C31 1.533(5) . ?
C7 C6 1.475(4) . ?
C3 C4 1.392(5) . ?
C3 C2 1.406(4) . ?
C9 C11 1.525(5) . ?
C9 C12 1.536(5) . ?
C21 C20 1.385(4) . ?
C21 C22 1.403(4) . ?
C22 C17 1.415(4) . ?
C22 C25 1.473(4) . ?
C24 C18 1.462(4) . ?
C1 C6 1.407(4) . ?
C1 C2 1.416(4) . ?
C8 C2 1.474(4) . ?
C5 C4 1.378(4) . ?
C5 C6 1.410(4) . ?
C37 C38 1.510(5) . ?
C37 C36 1.519(4) . ?
C19 C20 1.382(4) . ?
C19 C18 1.403(4) . ?
C20 C23 1.515(4) . ?
C17 C18 1.415(4) . ?
C13 C15 1.527(4) . ?
C13 C16 1.536(5) . ?
C34 C35 1.531(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
O13 C39 C30 113.4(3) . . ?
O18 N5 O19 120.6(3) . . ?
O18 N5 O17 119.4(3) . . ?
O19 N5 O17 120.0(3) . . ?
O21 C41 O20 123.1(3) . . ?
O21 C41 C42A 122.0(4) . . ?
O20 C41 C42A 113.4(4) . . ?
O21 C41 C42B 113.0(4) . . ?
O20 C41 C42B 122.1(4) . . ?
C41 C42A C43 114.7(6) . . ?
C43 C42B C41 112.2(6) . . ?
N6 C44 C45 178.0(5) . . ?
N1 Ni1 O2 177.08(9) . . ?
N1 Ni1 O1 90.96(9) . . ?
O2 Ni1 O1 86.52(8) . . ?
N1 Ni1 O5 82.51(10) . . ?
O2 Ni1 O5 99.71(9) . . ?
O1 Ni1 O5 168.29(9) . . ?
N1 Ni1 O9 88.27(10) . . ?
O2 Ni1 O9 93.27(9) . . ?
O1 Ni1 O9 91.67(8) . . ?
O5 Ni1 O9 97.82(9) . . ?
N1 Ni1 O3 99.64(9) . . ?
O2 Ni1 O3 78.54(8) . . ?
O1 Ni1 O3 81.36(8) . . ?
O5 Ni1 O3 90.12(9) . . ?
O9 Ni1 O3 169.49(8) . . ?
N1 Ni1 Ni2 133.86(7) . . ?
O2 Ni1 Ni2 44.17(6) . . ?
O1 Ni1 Ni2 45.24(6) . . ?
O5 Ni1 Ni2 143.20(7) . . ?
O9 Ni1 Ni2 80.80(6) . . ?
O3 Ni1 Ni2 88.71(5) . . ?
N4 Ni4 O4 175.90(9) . . ?
N4 Ni4 O3 91.33(9) . . ?
O4 Ni4 O3 86.18(8) . . ?
N4 Ni4 O8 79.83(10) . . ?
O4 Ni4 O8 102.28(9) . . ?
O3 Ni4 O8 169.25(8) . . ?
N4 Ni4 O2 97.86(9) . . ?
O4 Ni4 O2 78.51(8) . . ?
O3 Ni4 O2 80.26(8) . . ?
O8 Ni4 O2 94.80(9) . . ?
N4 Ni4 O12 90.77(9) . . ?
O4 Ni4 O12 92.52(8) . . ?
O3 Ni4 O12 90.61(9) . . ?
O8 Ni4 O12 95.57(9) . . ?
O2 Ni4 O12 167.53(8) . . ?
N4 Ni4 Ni3 134.43(8) . . ?
O4 Ni4 Ni3 44.07(6) . . ?
O3 Ni4 Ni3 44.88(5) . . ?
O8 Ni4 Ni3 145.06(6) . . ?
O2 Ni4 Ni3 87.65(6) . . ?
O12 Ni4 Ni3 79.88(6) . . ?
N3 Ni3 O11 89.01(9) . . ?
N3 Ni3 O4 176.54(8) . . ?
O11 Ni3 O4 90.82(9) . . ?
N3 Ni3 O7 81.77(9) . . ?
O11 Ni3 O7 94.73(9) . . ?
O4 Ni3 O7 101.68(8) . . ?
N3 Ni3 O3 90.13(9) . . ?
O11 Ni3 O3 94.82(8) . . ?
O4 Ni3 O3 86.44(8) . . ?
O7 Ni3 O3 167.36(9) . . ?
N3 Ni3 O1 101.45(9) . . ?
O11 Ni3 O1 168.86(8) . . ?
O4 Ni3 O1 78.51(8) . . ?
O7 Ni3 O1 90.60(8) . . ?
O3 Ni3 O1 81.46(8) . . ?
N3 Ni3 Ni4 132.54(7) . . ?
O11 Ni3 Ni4 81.53(6) . . ?
O4 Ni3 Ni4 44.05(6) . . ?
O7 Ni3 Ni4 145.05(6) . . ?
O3 Ni3 Ni4 45.16(6) . . ?
O1 Ni3 Ni4 88.49(5) . . ?
N2 Ni2 O2 174.36(9) . . ?
N2 Ni2 O6 82.08(9) . . ?
O2 Ni2 O6 103.40(9) . . ?
N2 Ni2 O10 90.67(9) . . ?
O2 Ni2 O10 90.94(8) . . ?
O6 Ni2 O10 87.44(9) . . ?
N2 Ni2 O4 99.35(9) . . ?
O2 Ni2 O4 78.45(8) . . ?
O6 Ni2 O4 100.66(9) . . ?
O10 Ni2 O4 167.85(8) . . ?
N2 Ni2 O1 89.79(9) . . ?
O2 Ni2 O1 84.72(8) . . ?
O6 Ni2 O1 171.86(8) . . ?
O10 Ni2 O1 92.96(9) . . ?
O4 Ni2 O1 80.31(8) . . ?
N2 Ni2 Ni1 131.91(7) . . ?
O2 Ni2 Ni1 43.22(6) . . ?
O6 Ni2 Ni1 143.53(6) . . ?
O10 Ni2 Ni1 80.42(6) . . ?
O4 Ni2 Ni1 87.74(6) . . ?
O1 Ni2 Ni1 44.31(5) . . ?
C17 O1 Ni1 123.42(17) . . ?
C17 O1 Ni2 123.27(18) . . ?
Ni1 O1 Ni2 90.45(8) . . ?
C17 O1 Ni3 116.77(17) . . ?
Ni1 O1 Ni3 99.05(8) . . ?
Ni2 O1 Ni3 97.70(8) . . ?
Ni1 O2 Ni2 92.61(9) . . ?
Ni1 O2 Ni4 103.76(10) . . ?
Ni2 O2 Ni4 100.89(9) . . ?
Ni4 O4 Ni3 91.88(8) . . ?
Ni4 O4 Ni2 101.63(8) . . ?
Ni3 O4 Ni2 103.38(9) . . ?
C1 O3 Ni3 122.49(17) . . ?
C1 O3 Ni4 120.13(18) . . ?
Ni3 O3 Ni4 89.96(8) . . ?
C1 O3 Ni1 121.70(17) . . ?
Ni3 O3 Ni1 98.12(8) . . ?
Ni4 O3 Ni1 97.39(8) . . ?
C33 O11 Ni3 127.05(19) . . ?
C33 O12 Ni4 125.6(2) . . ?
C24 N2 C26 121.2(2) . . ?
C24 N2 Ni2 124.8(2) . . ?
C26 N2 Ni2 113.74(18) . . ?
C36 O10 Ni2 127.2(2) . . ?
C8 N4 C13 120.7(2) . . ?
C8 N4 Ni4 123.9(2) . . ?
C13 N4 Ni4 115.29(19) . . ?
C7 N3 C9 117.8(3) . . ?
C7 N3 Ni3 124.3(2) . . ?
C9 N3 Ni3 115.57(18) . . ?
C31 O5 Ni1 111.79(18) . . ?
C14 O8 Ni4 105.95(18) . . ?
C27 O6 Ni2 109.70(18) . . ?
C36 O9 Ni1 125.36(19) . . ?
C10 O7 Ni3 113.13(17) . . ?
C25 N1 C30 119.4(3) . . ?
C25 N1 Ni1 124.4(2) . . ?
C30 N1 Ni1 114.3(2) . . ?
O7 C10 C9 112.7(2) . . ?
N2 C26 C29 115.3(2) . . ?
N2 C26 C28 106.3(2) . . ?
C29 C26 C28 110.4(2) . . ?
N2 C26 C27 104.6(2) . . ?
C29 C26 C27 109.2(3) . . ?
C28 C26 C27 110.7(2) . . ?
O8 C14 C13 107.2(3) . . ?
O12 C33 O11 125.5(3) . . ?
O12 C33 C34 119.3(3) . . ?
O11 C33 C34 115.1(3) . . ?
N1 C30 C32 113.6(3) . . ?
N1 C30 C31 107.4(3) . . ?
C32 C30 C31 109.7(3) . . ?
N1 C30 C39 106.5(3) . . ?
C32 C30 C39 114.4(3) . . ?
C31 C30 C39 104.7(3) . . ?
N3 C7 C6 126.7(3) . . ?
C4 C3 C2 123.1(3) . . ?
N3 C9 C11 113.0(2) . . ?
N3 C9 C12 108.5(2) . . ?
C11 C9 C12 110.1(3) . . ?
N3 C9 C10 106.6(2) . . ?
C11 C9 C10 108.9(3) . . ?
C12 C9 C10 109.6(3) . . ?
O5 C31 C30 111.7(3) . . ?
C20 C21 C22 122.5(3) . . ?
C21 C22 C17 119.4(3) . . ?
C21 C22 C25 115.4(3) . . ?
C17 C22 C25 125.1(3) . . ?
N2 C24 C18 126.9(3) . . ?
O3 C1 C6 120.5(3) . . ?
O3 C1 C2 120.6(3) . . ?
C6 C1 C2 118.8(3) . . ?
O14 C28 C26 112.0(2) . . ?
N4 C8 C2 125.2(3) . . ?
C4 C5 C6 122.3(3) . . ?
O15B C11 C9 112.2(4) . . ?
C1 C6 C5 119.9(3) . . ?
C1 C6 C7 125.3(3) . . ?
C5 C6 C7 114.6(3) . . ?
C38 C37 C36 116.1(3) . . ?
C20 C19 C18 122.9(3) . . ?
C3 C2 C1 118.6(3) . . ?
C3 C2 C8 114.8(3) . . ?
C1 C2 C8 126.6(3) . . ?
O6 C27 C26 111.3(2) . . ?
O10 C36 O9 125.9(3) . . ?
O10 C36 C37 116.9(3) . . ?
O9 C36 C37 117.2(3) . . ?
O15A C12 C9 116.9(3) . . ?
C19 C20 C21 117.2(3) . . ?
C19 C20 C23 121.2(3) . . ?
C21 C20 C23 121.6(3) . . ?
O1 C17 C18 121.0(3) . . ?
O1 C17 C22 120.6(3) . . ?
C18 C17 C22 118.3(3) . . ?
N1 C25 C22 126.8(3) . . ?
C19 C18 C17 119.1(3) . . ?
C19 C18 C24 115.4(3) . . ?
C17 C18 C24 125.5(3) . . ?
C5 C4 C3 117.3(3) . . ?
C5 C4 C40 121.6(3) . . ?
C3 C4 C40 121.1(3) . . ?
N4 C13 C15 113.5(3) . . ?
N4 C13 C14 105.9(2) . . ?
C15 C13 C14 109.9(3) . . ?
N4 C13 C16 109.2(3) . . ?
C15 C13 C16 111.5(3) . . ?
C14 C13 C16 106.6(3) . . ?
C33 C34 C35 110.0(3) . . ?
O16 C16 C13 113.9(3) . . ?

_refine_diff_density_max         1.985
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.103

####################################################################### 
# 
# 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_Complex1
_database_code_depnum_ccdc_archive 'CCDC 1835111'
_audit_update_record             
;
2018-04-05 deposited with the CCDC.
2018-09-04 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C38 H56 N4 Ni4 O16, C2 H3 O2, N O3, H2 O, O, H O'
_chemical_formula_sum            'C40 H65 N5 Ni4 O24'
_chemical_formula_weight         1234.78
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.6627(6)
_cell_length_b                   12.5163(6)
_cell_length_c                   19.6420(9)
_cell_angle_alpha                92.6980(10)
_cell_angle_beta                 96.2000(10)
_cell_angle_gamma                90.0900(10)
_cell_volume                     2847.2(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    34906
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.321
_cell_measurement_theta_min      1.629
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.381
_exptl_absorpt_correction_T_max  0.780
_exptl_absorpt_correction_T_min  0.656
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1282
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            34906
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.321
_diffrn_reflns_theta_min         1.629
_diffrn_ambient_temperature      293.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9138
_reflns_number_total             11167
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_refine_diff_density_max         2.552
_refine_diff_density_min         -1.093
_refine_diff_density_rms         0.119
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     691
_refine_ls_number_reflns         11167
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0555
_refine_ls_restrained_S_all      1.184
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0985P)²+4.4085P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1610
_refine_ls_wR_factor_ref         0.1686
_refine_special_details          ?

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
C22 C 0.8418(3) 0.7362(3) 0.3554(2) 0.0182(8) Uani 1 1 d . . . . .
C27 C 0.8850(3) 0.7188(3) 0.4241(2) 0.0200(8) Uani 1 1 d . . . . .
C24 C 0.9763(3) 0.8864(3) 0.3588(2) 0.0242(9) Uani 1 1 d . . . . .
H24 H 1.0061 0.9427 0.3368 0.029 Uiso 1 1 calc R . . . .
C25 C 1.0175(3) 0.8708(3) 0.4268(2) 0.0264(9) Uani 1 1 d . . . . .
C30 C 0.7656(3) 0.4634(3) 0.4876(2) 0.0195(8) Uani 1 1 d . . . . .
C28 C 0.8702(4) 0.8396(3) 0.2494(2) 0.0254(9) Uani 1 1 d . . . . .
H28 H 0.9008 0.9022 0.2349 0.030 Uiso 1 1 calc R . . . .
C31 C 0.7702(4) 0.3589(3) 0.4425(2) 0.0249(9) Uani 1 1 d . . . . .
H31A H 0.8499 0.3427 0.4365 0.030 Uiso 1 1 calc R . . . .
H31B H 0.7392 0.3004 0.4656 0.030 Uiso 1 1 calc R . . . .
C29 C 0.8489(3) 0.6319(3) 0.4644(2) 0.0211(8) Uani 1 1 d . . . . .
H29 H 0.8726 0.6365 0.5112 0.025 Uiso 1 1 calc R . . . .
C23 C 0.8918(3) 0.8205(3) 0.3224(2) 0.0223(8) Uani 1 1 d . . . . .
C34 C 0.3239(3) 0.7068(3) 0.3024(2) 0.0238(9) Uani 1 1 d . . . . .
C33 C 0.6435(3) 0.4815(3) 0.5081(2) 0.0199(8) Uani 1 1 d . . . . .
H33A H 0.6398 0.5519 0.5306 0.024 Uiso 1 1 calc R . . . .
H33B H 0.5889 0.4794 0.4672 0.024 Uiso 1 1 calc R . . . .
C32 C 0.8522(4) 0.4569(4) 0.5517(2) 0.0281(9) Uani 1 1 d . . . . .
H32A H 0.9291 0.4643 0.5392 0.042 Uiso 1 1 calc GR . . . .
H32B H 0.8442 0.3890 0.5715 0.042 Uiso 1 1 calc GR . . . .
H32C H 0.8375 0.5132 0.5844 0.042 Uiso 1 1 calc GR . . . .
C26 C 0.9704(3) 0.7872(3) 0.4582(2) 0.0239(9) Uani 1 1 d . . . . .
H26 H 0.9963 0.7758 0.5037 0.029 Uiso 1 1 calc R . . . .
O14 O 0.6116(2) 0.4033(2) 0.55278(15) 0.0234(6) Uani 1 1 d D . . . .
C36 C 0.9329(3) 0.5004(3) 0.2664(2) 0.0250(9) Uani 1 1 d . . . . .
C39 C 1.1142(4) 0.9402(4) 0.4637(3) 0.0332(10) Uani 1 1 d . . . . .
H39A H 1.1117 0.9383 0.5123 0.050 Uiso 1 1 calc GR . . . .
H39B H 1.1048 1.0125 0.4499 0.050 Uiso 1 1 calc GR . . . .
H39C H 1.1871 0.9136 0.4522 0.050 Uiso 1 1 calc GR . . . .
C37 C 1.0474(4) 0.4505(4) 0.2542(3) 0.0371(11) Uani 1 1 d . . . . .
H37A H 1.0668 0.3976 0.2873 0.056 Uiso 1 1 calc GR . . . .
H37B H 1.1062 0.5049 0.2586 0.056 Uiso 1 1 calc GR . . . .
H37C H 1.0418 0.4173 0.2089 0.056 Uiso 1 1 calc GR . . . .
C35 C 0.2022(4) 0.7481(4) 0.3069(3) 0.0388(12) Uani 1 1 d . . . . .
H35A H 0.1831 0.7976 0.2716 0.058 Uiso 1 1 calc GR . . . .
H35B H 0.1979 0.7835 0.3509 0.058 Uiso 1 1 calc GR . . . .
H35C H 0.1487 0.6891 0.3009 0.058 Uiso 1 1 calc GR . . . .
C38 C 0.3660(7) 0.9814(6) 0.0300(3) 0.072(2) Uani 1 1 d . . . . .
H38A H 0.2871 0.9943 0.0375 0.107 Uiso 1 1 calc GR . . . .
H38B H 0.3690 0.9493 -0.0151 0.107 Uiso 1 1 calc GR . . . .
H38C H 0.4078 1.0479 0.0342 0.107 Uiso 1 1 calc GR . . . .
O20 O 0.5153(2) 0.7411(2) 0.53440(15) 0.0264(6) Uani 1 1 d . . . . .
C40 C 0.5600(4) 0.7286(3) 0.5950(2) 0.0247(9) Uani 1 1 d . . . . .
O18 O 0.7395(5) 0.3196(4) 0.1658(3) 0.0813(16) Uani 1 1 d . . . . .
C41 C 0.6855(4) 0.7586(4) 0.6135(3) 0.0335(10) Uani 1 1 d . . . . .
H41A H 0.7272 0.7440 0.5746 0.050 Uiso 1 1 calc GR . . . .
H41B H 0.7173 0.7175 0.6510 0.050 Uiso 1 1 calc GR . . . .
H41C H 0.6916 0.8334 0.6267 0.050 Uiso 1 1 calc GR . . . .
N5 N 0.6938(7) 0.2238(6) 0.1613(4) 0.088(2) Uani 1 1 d . . . . .
O23 O 0.5045(3) 0.6950(2) 0.64098(16) 0.0309(7) Uani 1 1 d . . . . .
O19 O 0.6715(8) 0.1832(6) 0.1019(4) 0.136(3) Uani 1 1 d . . . . .
O1W O 0.7689(3) 0.4512(3) 0.05629(19) 0.0473(9) Uani 1 1 d D . . . .
O2W O 0.0121(5) 0.6075(8) 0.9786(4) 0.143(3) Uani 1 1 d . . . . .
O3W O 0.8205 0.2805 0.2934 0.0749(14) Uani 1 1 d D . . . .
O6 O 0.7062(2) 0.3680(2) 0.37707(14) 0.0222(6) Uani 1 1 d . . . . .
H6 H 0.6627 0.3134 0.3530 0.027 Uiso 1 1 calc R . . . .
O15 O 0.4229(4) 0.9353(3) 0.4245(2) 0.0580(11) Uani 1 1 d . . . . .
H15 H 0.4429 0.8738 0.4158 0.087 Uiso 1 1 calc GR . . . .
O17 O 0.6665(8) 0.1772(5) 0.2090(4) 0.134(3) Uani 1 1 d . . . . .
H7 H 0.588(4) 0.780(4) 0.466(2) 0.045(16) Uiso 1 1 d D . . . .
H8 H 0.431(5) 0.362(4) 0.279(2) 0.051(18) Uiso 1 1 d D . . . .
H2 H 0.685(6) 0.458(5) 0.217(3) 0.09(3) Uiso 1 1 d D . . . .
H4 H 0.499(4) 0.575(6) 0.369(4) 0.09(3) Uiso 1 1 d D . . . .
H5 H 0.746(5) 0.580(3) 0.101(3) 0.06(2) Uiso 1 1 d D . . . .
H14 H 0.576(4) 0.354(3) 0.529(2) 0.030(13) Uiso 1 1 d D . . . .
H1WA H 0.7744 0.3883 0.0864 0.049(11) Uiso 1 1 d D . . . .
H1WB H 0.8433 0.4398 0.0489 0.049(11) Uiso 1 1 d D . . . .
H3W H 0.8243 0.2361 0.2534 0.13(4) Uiso 1 1 d D . . . .
Ni3 Ni 0.57794(4) 0.73708(4) 0.33445(2) 0.01708(14) Uani 1 1 d . . . . .
Ni2 Ni 0.72436(4) 0.52088(4) 0.34327(2) 0.01689(14) Uani 1 1 d . . . . .
Ni1 Ni 0.73661(4) 0.64150(4) 0.22038(3) 0.02001(14) Uani 1 1 d . . . . .
Ni4 Ni 0.48962(4) 0.55337(4) 0.24857(2) 0.01993(14) Uani 1 1 d . . . . .
O4 O 0.5589(2) 0.5797(2) 0.34749(14) 0.0175(5) Uani 1 1 d D . . . .
O2 O 0.6582(2) 0.5061(2) 0.24327(14) 0.0207(6) Uani 1 1 d D . . . .
O1 O 0.7529(2) 0.6794(2) 0.32371(13) 0.0174(5) Uani 1 1 d . . . . .
O3 O 0.5628(2) 0.7001(2) 0.23092(14) 0.0207(6) Uani 1 1 d . . . . .
O9 O 0.8937(2) 0.5684(2) 0.22393(15) 0.0259(6) Uani 1 1 d . . . . .
O12 O 0.3359(2) 0.6221(2) 0.26731(15) 0.0256(6) Uani 1 1 d . . . . .
N2 N 0.7880(3) 0.5501(3) 0.44168(17) 0.0190(7) Uani 1 1 d . . . . .
O10 O 0.8848(2) 0.4718(2) 0.31661(15) 0.0256(6) Uani 1 1 d . . . . .
O11 O 0.4050(2) 0.7632(2) 0.33393(15) 0.0239(6) Uani 1 1 d . . . . .
N3 N 0.5953(3) 0.8927(3) 0.31769(18) 0.0222(7) Uani 1 1 d . . . . .
O7 O 0.6295(2) 0.7914(2) 0.43348(14) 0.0202(6) Uani 1 1 d D . . . .
O5 O 0.7086(3) 0.6333(3) 0.11532(15) 0.0301(7) Uani 1 1 d D . . . .
N1 N 0.8136(3) 0.7792(3) 0.20328(18) 0.0253(8) Uani 1 1 d . . . . .
N4 N 0.4363(3) 0.5346(3) 0.14798(18) 0.0286(8) Uani 1 1 d . . . . .
O8 O 0.4164(3) 0.4033(3) 0.24685(15) 0.0287(7) Uani 1 1 d D . . . .
C19 C 0.7320(4) 0.7325(4) 0.0858(2) 0.0354(11) Uani 1 1 d . . . . .
H19A H 0.6614 0.7735 0.0799 0.043 Uiso 1 1 calc R . . . .
H19B H 0.7571 0.7178 0.0408 0.043 Uiso 1 1 calc R . . . .
C15 C 0.6713(3) 0.8995(3) 0.4376(2) 0.0211(8) Uani 1 1 d . . . . .
H15A H 0.7537 0.8995 0.4345 0.025 Uiso 1 1 calc R . . . .
H15B H 0.6582 0.9329 0.4816 0.025 Uiso 1 1 calc R . . . .
C1 C 0.5122(4) 0.7668(4) 0.1848(2) 0.0267(9) Uani 1 1 d . . . . .
C14 C 0.6113(4) 0.9651(3) 0.3801(2) 0.0243(9) Uani 1 1 d . . . . .
C7 C 0.4245(4) 0.6108(4) 0.1068(2) 0.0330(10) Uani 1 1 d . . . . .
H7A H 0.3971 0.5922 0.0615 0.040 Uiso 1 1 calc R . . . .
C18 C 0.8257(4) 0.7999(4) 0.1305(2) 0.0311(10) Uani 1 1 d . . . . .
C6 C 0.5232(4) 0.8777(4) 0.1949(2) 0.0312(10) Uani 1 1 d . . . . .
O13 O 0.9664(4) 0.6520(4) 0.1114(2) 0.0625(11) Uani 1 1 d . . . . .
H13 H 0.9562 0.6275 0.1483 0.094 Uiso 1 1 calc R . . . .
C3 C 0.4060(5) 0.7965(5) 0.0741(3) 0.0457(13) Uani 1 1 d . . . . .
H3 H 0.3660 0.7688 0.0336 0.055 Uiso 1 1 calc R . . . .
C9 C 0.3932(4) 0.4258(4) 0.1253(2) 0.0355(11) Uani 1 1 d . . . . .
C8 C 0.5688(4) 0.9342(4) 0.2599(2) 0.0303(10) Uani 1 1 d . . . . .
H8A H 0.5794 1.0077 0.2586 0.036 Uiso 1 1 calc R . . . .
C17 C 0.4933(4) 1.0039(4) 0.3989(3) 0.0402(12) Uani 1 1 d . . . . .
C21 C 0.9490(5) 0.7635(4) 0.1148(3) 0.0435(13) Uani 1 1 d . . . . .
H21A H 0.9641 0.7916 0.0714 0.052 Uiso 1 1 calc R . . . .
H21B H 1.0051 0.7954 0.1500 0.052 Uiso 1 1 calc R . . . .
C13 C 0.4428(5) 0.3860(5) 0.0598(3) 0.0450(13) Uani 1 1 d . . . . .
H13A H 0.4111 0.4268 0.0222 0.067 Uiso 1 1 calc GR . . . .
H13B H 0.4234 0.3118 0.0504 0.067 Uiso 1 1 calc GR . . . .
H13C H 0.5252 0.3943 0.0658 0.067 Uiso 1 1 calc GR . . . .
C10 C 0.4361(4) 0.3530(4) 0.1822(2) 0.0362(11) Uani 1 1 d . . . . .
H10A H 0.3956 0.2849 0.1757 0.043 Uiso 1 1 calc R . . . .
H10B H 0.5179 0.3397 0.1811 0.043 Uiso 1 1 calc R . . . .
C2 C 0.4497(4) 0.7247(4) 0.1234(2) 0.0321(10) Uani 1 1 d . . . . .
O16 O 0.2115(5) 0.3360(6) 0.0952(3) 0.107(2) Uani 1 1 d . . . . .
H16 H 0.1411 0.3418 0.0906 0.160 Uiso 1 1 calc R . . . .
C5 C 0.4786(5) 0.9452(4) 0.1435(3) 0.0423(12) Uani 1 1 d . . . . .
H5A H 0.4892 1.0187 0.1506 0.051 Uiso 1 1 calc R . . . .
C16 C 0.6846(5) 1.0640(4) 0.3721(3) 0.0403(12) Uani 1 1 d . . . . .
H16A H 0.7527 1.0431 0.3516 0.060 Uiso 1 1 calc GR . . . .
H16B H 0.7062 1.0985 0.4163 0.060 Uiso 1 1 calc GR . . . .
H16C H 0.6408 1.1127 0.3433 0.060 Uiso 1 1 calc GR . . . .
C20 C 0.8106(5) 0.9171(4) 0.1139(3) 0.0420(12) Uani 1 1 d . . . . .
H20A H 0.7442 0.9452 0.1334 0.063 Uiso 1 1 calc GR . . . .
H20B H 0.8001 0.9229 0.0651 0.063 Uiso 1 1 calc GR . . . .
H20C H 0.8779 0.9569 0.1328 0.063 Uiso 1 1 calc GR . . . .
C11 C 0.2605(4) 0.4320(6) 0.1159(3) 0.0564(17) Uani 1 1 d . . . . .
H11A H 0.2333 0.4560 0.1590 0.068 Uiso 1 1 calc R . . . .
H11B H 0.2368 0.4841 0.0823 0.068 Uiso 1 1 calc R . . . .
C4 C 0.4200(5) 0.9065(5) 0.0830(3) 0.0490(14) 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
C22 C27 1.416(6) . ?
C22 C23 1.420(6) . ?
C22 O1 1.336(4) . ?
C27 C29 1.463(6) . ?
C27 C26 1.404(5) . ?
C24 C25 1.392(6) . ?
C24 C23 1.398(6) . ?
C25 C26 1.381(6) . ?
C25 C39 1.521(6) . ?
C30 C31 1.549(5) . ?
C30 C33 1.535(5) . ?
C30 C32 1.531(6) . ?
C30 N2 1.484(5) . ?
C28 C23 1.461(6) . ?
C28 N1 1.278(6) . ?
C31 O6 1.425(5) . ?
C29 N2 1.280(5) . ?
C34 C35 1.522(6) . ?
C34 O12 1.253(5) . ?
C34 O11 1.267(5) . ?
C33 O14 1.419(5) . ?
C36 C37 1.512(6) . ?
C36 O9 1.271(5) . ?
C36 O10 1.251(5) . ?
C38 C4 1.521(7) . ?
O20 C40 1.264(5) . ?
C40 C41 1.511(6) . ?
C40 O23 1.254(5) . ?
O18 N5 1.308(8) . ?
N5 O19 1.250(9) . ?
N5 O17 1.199(9) . ?
O6 Ni2 2.072(3) . ?
O15 C17 1.339(7) . ?
Ni3 Ni4 2.9061(7) . ?
Ni3 O4 2.014(3) . ?
Ni3 O1 2.193(3) . ?
Ni3 O3 2.053(3) . ?
Ni3 O11 2.043(3) . ?
Ni3 N3 2.004(3) . ?
Ni3 O7 2.056(3) . ?
Ni2 Ni1 2.9229(7) . ?
Ni2 O4 2.075(3) . ?
Ni2 O2 2.031(3) . ?
Ni2 O1 2.071(3) . ?
Ni2 N2 2.011(3) . ?
Ni2 O10 2.083(3) . ?
Ni1 O2 2.017(3) . ?
Ni1 O1 2.051(3) . ?
Ni1 O3 2.184(3) . ?
Ni1 O9 2.045(3) . ?
Ni1 O5 2.052(3) . ?
Ni1 N1 2.000(4) . ?
Ni4 O4 2.034(3) . ?
Ni4 O2 2.066(3) . ?
Ni4 O3 2.083(3) . ?
Ni4 O12 2.051(3) . ?
Ni4 N4 2.009(4) . ?
Ni4 O8 2.059(3) . ?
O3 C1 1.350(5) . ?
N3 C14 1.485(5) . ?
N3 C8 1.279(6) . ?
O7 C15 1.434(5) . ?
O5 C19 1.432(6) . ?
N1 C18 1.485(5) . ?
N4 C7 1.278(6) . ?
N4 C9 1.483(6) . ?
O8 C10 1.433(5) . ?
C19 C18 1.549(7) . ?
C15 C14 1.534(6) . ?
C1 C6 1.396(7) . ?
C1 C2 1.419(6) . ?
C14 C17 1.536(6) . ?
C14 C16 1.527(6) . ?
C7 C2 1.469(7) . ?
C18 C21 1.567(7) . ?
C18 C20 1.524(7) . ?
C6 C8 1.476(7) . ?
C6 C5 1.404(6) . ?
O13 C21 1.410(7) . ?
C3 C2 1.408(7) . ?
C3 C4 1.387(8) . ?
C9 C13 1.529(7) . ?
C9 C10 1.519(7) . ?
C9 C11 1.541(7) . ?
O16 C11 1.355(8) . ?
C5 C4 1.371(8) . ?

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
C27 C22 C23 117.7(3) . . ?
O1 C22 C27 121.3(3) . . ?
O1 C22 C23 120.9(3) . . ?
C22 C27 C29 125.1(3) . . ?
C26 C27 C22 119.8(4) . . ?
C26 C27 C29 115.1(4) . . ?
C25 C24 C23 122.4(4) . . ?
C24 C25 C39 121.0(4) . . ?
C26 C25 C24 117.3(4) . . ?
C26 C25 C39 121.6(4) . . ?
C33 C30 C31 110.6(3) . . ?
C32 C30 C31 109.4(3) . . ?
C32 C30 C33 110.2(3) . . ?
N2 C30 C31 104.7(3) . . ?
N2 C30 C33 106.6(3) . . ?
N2 C30 C32 115.2(3) . . ?
N1 C28 C23 126.7(4) . . ?
O6 C31 C30 111.5(3) . . ?
N2 C29 C27 126.5(4) . . ?
C22 C23 C28 124.9(4) . . ?
C24 C23 C22 120.0(4) . . ?
C24 C23 C28 114.8(4) . . ?
O12 C34 C35 118.0(4) . . ?
O12 C34 O11 125.7(4) . . ?
O11 C34 C35 116.3(4) . . ?
O14 C33 C30 112.1(3) . . ?
C25 C26 C27 122.7(4) . . ?
O9 C36 C37 116.2(4) . . ?
O10 C36 C37 118.2(4) . . ?
O10 C36 O9 125.6(4) . . ?
O20 C40 C41 118.5(4) . . ?
O23 C40 O20 123.1(4) . . ?
O23 C40 C41 118.4(4) . . ?
O19 N5 O18 115.8(8) . . ?
O17 N5 O18 124.5(8) . . ?
O17 N5 O19 119.5(8) . . ?
C31 O6 Ni2 110.0(2) . . ?
O4 Ni3 Ni4 44.39(8) . . ?
O4 Ni3 O1 78.90(10) . . ?
O4 Ni3 O3 87.19(11) . . ?
O4 Ni3 O11 92.14(11) . . ?
O4 Ni3 O7 100.72(11) . . ?
O1 Ni3 Ni4 88.30(7) . . ?
O3 Ni3 Ni4 45.79(8) . . ?
O3 Ni3 O1 80.08(10) . . ?
O3 Ni3 O7 166.15(11) . . ?
O11 Ni3 Ni4 80.36(8) . . ?
O11 Ni3 O1 168.61(11) . . ?
O11 Ni3 O3 92.58(11) . . ?
O11 Ni3 O7 98.42(11) . . ?
N3 Ni3 Ni4 133.50(10) . . ?
N3 Ni3 O4 177.86(13) . . ?
N3 Ni3 O1 101.07(12) . . ?
N3 Ni3 O3 90.70(13) . . ?
N3 Ni3 O11 87.62(12) . . ?
N3 Ni3 O7 81.42(13) . . ?
O7 Ni3 Ni4 144.57(8) . . ?
O7 Ni3 O1 90.22(10) . . ?
O6 Ni2 Ni1 143.20(8) . . ?
O6 Ni2 O4 101.07(11) . . ?
O6 Ni2 O10 86.52(11) . . ?
O4 Ni2 Ni1 87.99(8) . . ?
O4 Ni2 O10 167.29(11) . . ?
O2 Ni2 O6 103.03(11) . . ?
O2 Ni2 Ni1 43.58(8) . . ?
O2 Ni2 O4 78.28(11) . . ?
O2 Ni2 O1 85.21(11) . . ?
O2 Ni2 O10 90.13(11) . . ?
O1 Ni2 O6 171.76(11) . . ?
O1 Ni2 Ni1 44.56(7) . . ?
O1 Ni2 O4 80.42(10) . . ?
O1 Ni2 O10 93.54(11) . . ?
N2 Ni2 O6 81.96(12) . . ?
N2 Ni2 Ni1 132.12(10) . . ?
N2 Ni2 O4 99.31(12) . . ?
N2 Ni2 O2 174.75(12) . . ?
N2 Ni2 O1 89.80(12) . . ?
N2 Ni2 O10 91.80(12) . . ?
O10 Ni2 Ni1 79.94(8) . . ?
O2 Ni1 Ni2 43.97(8) . . ?
O2 Ni1 O1 86.12(11) . . ?
O2 Ni1 O3 79.29(11) . . ?
O2 Ni1 O9 92.02(11) . . ?
O2 Ni1 O5 101.24(12) . . ?
O1 Ni1 Ni2 45.13(7) . . ?
O1 Ni1 O3 80.35(10) . . ?
O1 Ni1 O5 168.87(12) . . ?
O3 Ni1 Ni2 88.74(7) . . ?
O9 Ni1 Ni2 81.10(8) . . ?
O9 Ni1 O1 93.60(11) . . ?
O9 Ni1 O3 169.67(11) . . ?
O9 Ni1 O5 94.46(12) . . ?
O5 Ni1 Ni2 144.16(10) . . ?
O5 Ni1 O3 92.72(12) . . ?
N1 Ni1 Ni2 133.12(10) . . ?
N1 Ni1 O2 176.64(13) . . ?
N1 Ni1 O1 90.60(12) . . ?
N1 Ni1 O3 99.48(13) . . ?
N1 Ni1 O9 88.88(13) . . ?
N1 Ni1 O5 81.90(14) . . ?
O4 Ni4 Ni3 43.83(8) . . ?
O4 Ni4 O2 78.41(11) . . ?
O4 Ni4 O3 85.85(11) . . ?
O4 Ni4 O12 92.63(11) . . ?
O4 Ni4 O8 104.06(11) . . ?
O2 Ni4 Ni3 88.15(8) . . ?
O2 Ni4 O3 80.56(11) . . ?
O3 Ni4 Ni3 44.94(7) . . ?
O12 Ni4 Ni3 80.99(8) . . ?
O12 Ni4 O2 169.05(11) . . ?
O12 Ni4 O3 92.61(11) . . ?
O12 Ni4 O8 90.53(12) . . ?
N4 Ni4 Ni3 132.50(12) . . ?
N4 Ni4 O4 173.94(13) . . ?
N4 Ni4 O2 97.23(13) . . ?
N4 Ni4 O3 89.29(13) . . ?
N4 Ni4 O12 91.20(13) . . ?
N4 Ni4 O8 80.59(14) . . ?
O8 Ni4 Ni3 145.59(9) . . ?
O8 Ni4 O2 97.71(12) . . ?
O8 Ni4 O3 169.47(11) . . ?
Ni3 O4 Ni2 103.18(12) . . ?
Ni3 O4 Ni4 91.78(11) . . ?
Ni4 O4 Ni2 101.30(12) . . ?
Ni2 O2 Ni4 101.68(12) . . ?
Ni1 O2 Ni2 92.45(11) . . ?
Ni1 O2 Ni4 103.01(13) . . ?
C22 O1 Ni3 118.2(2) . . ?
C22 O1 Ni2 122.5(2) . . ?
C22 O1 Ni1 122.5(2) . . ?
Ni2 O1 Ni3 97.34(10) . . ?
Ni1 O1 Ni3 99.66(11) . . ?
Ni1 O1 Ni2 90.31(10) . . ?
Ni3 O3 Ni1 99.91(11) . . ?
Ni3 O3 Ni4 89.27(11) . . ?
Ni4 O3 Ni1 96.97(11) . . ?
C1 O3 Ni3 122.0(3) . . ?
C1 O3 Ni1 119.8(2) . . ?
C1 O3 Ni4 122.2(2) . . ?
C36 O9 Ni1 126.6(3) . . ?
C34 O12 Ni4 126.0(3) . . ?
C30 N2 Ni2 114.1(2) . . ?
C29 N2 C30 120.7(3) . . ?
C29 N2 Ni2 125.1(3) . . ?
C36 O10 Ni2 126.7(3) . . ?
C34 O11 Ni3 126.9(3) . . ?
C14 N3 Ni3 115.4(3) . . ?
C8 N3 Ni3 124.4(3) . . ?
C8 N3 C14 118.2(3) . . ?
C15 O7 Ni3 112.6(2) . . ?
C19 O5 Ni1 112.8(3) . . ?
C28 N1 Ni1 124.9(3) . . ?
C28 N1 C18 117.5(4) . . ?
C18 N1 Ni1 116.3(3) . . ?
C7 N4 Ni4 124.6(3) . . ?
C7 N4 C9 120.1(4) . . ?
C9 N4 Ni4 114.6(3) . . ?
C10 O8 Ni4 105.8(3) . . ?
O5 C19 C18 112.5(4) . . ?
O7 C15 C14 111.7(3) . . ?
O3 C1 C6 121.4(4) . . ?
O3 C1 C2 120.0(4) . . ?
C6 C1 C2 118.5(4) . . ?
N3 C14 C15 106.7(3) . . ?
N3 C14 C17 109.7(3) . . ?
N3 C14 C16 113.7(4) . . ?
C15 C14 C17 110.4(4) . . ?
C16 C14 C15 108.9(3) . . ?
C16 C14 C17 107.5(4) . . ?
N4 C7 C2 126.8(4) . . ?
N1 C18 C19 107.2(3) . . ?
N1 C18 C21 108.2(4) . . ?
N1 C18 C20 113.5(4) . . ?
C19 C18 C21 110.4(4) . . ?
C20 C18 C19 108.9(4) . . ?
C20 C18 C21 108.7(4) . . ?
C1 C6 C8 125.0(4) . . ?
C1 C6 C5 120.3(4) . . ?
C5 C6 C8 114.4(4) . . ?
C4 C3 C2 123.1(5) . . ?
N4 C9 C13 111.4(4) . . ?
N4 C9 C10 106.2(3) . . ?
N4 C9 C11 106.7(4) . . ?
C13 C9 C11 112.5(4) . . ?
C10 C9 C13 108.0(4) . . ?
C10 C9 C11 111.8(4) . . ?
N3 C8 C6 126.9(4) . . ?
O15 C17 C14 119.3(4) . . ?
O13 C21 C18 115.3(4) . . ?
O8 C10 C9 109.0(4) . . ?
C1 C2 C7 125.3(4) . . ?
C3 C2 C1 118.4(5) . . ?
C3 C2 C7 116.2(4) . . ?
C4 C5 C6 122.3(5) . . ?
O16 C11 C9 111.8(6) . . ?
C3 C4 C38 121.3(5) . . ?
C5 C4 C38 121.3(6) . . ?
C5 C4 C3 117.3(5) . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 504.7 0.0 ?



