# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

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

data_hang66_0m_sq
_database_code_depnum_ccdc_archive 'CCDC 1562140'
_audit_update_record             
;
2017-09-28 deposited with the CCDC.
2018-01-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H68 N5 Ni4 O14 S5'
_chemical_formula_weight         1478.33

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   13.2812(6)
_cell_length_b                   22.1310(9)
_cell_length_c                   27.4033(12)
_cell_angle_alpha                90
_cell_angle_beta                 103.714(2)
_cell_angle_gamma                90
_cell_volume                     7824.9(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    190(2)
_cell_measurement_reflns_used    9846
_cell_measurement_theta_min      3.43
_cell_measurement_theta_max      44.56

_exptl_crystal_description       green
_exptl_crystal_colour            block
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_F_000             3068
_exptl_transmission_factor_min   0.636
_exptl_transmission_factor_max   0.716
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    2.783
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6216
_exptl_absorpt_correction_T_max  0.7488
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      190(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            36232
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.596
_diffrn_reflns_theta_max         44.610
_diffrn_reflns_theta_full        44.610
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             6169
_reflns_number_gt                5297
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0851P)²+43.0392P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6169
_refine_ls_number_parameters     787
_refine_ls_number_restraints     330
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0604
_refine_ls_wR_factor_ref         0.1726
_refine_ls_wR_factor_gt          0.1659
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.101
_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 0.48334(10) 0.51130(6) 0.18262(5) 0.0301(4) Uani 1 1 d . . . . .
Ni2 Ni 0.59903(11) 0.39957(6) 0.26913(5) 0.0354(4) Uani 1 1 d . . . . .
Ni3 Ni 0.49098(10) 0.29045(6) 0.20703(5) 0.0318(4) Uani 1 1 d . . . . .
Ni4 Ni 0.34948(10) 0.38379(6) 0.10417(5) 0.0311(4) Uani 1 1 d . . . . .
S1 S 0.36609(17) 0.57595(9) 0.21089(8) 0.0372(6) Uani 1 1 d . . . . .
S2 S 0.5730(2) 0.41550(10) 0.35366(8) 0.0504(7) Uani 1 1 d . . . . .
S3 S 0.37597(18) 0.22705(9) 0.24392(8) 0.0411(6) Uani 1 1 d . . . . .
S4 S 0.16978(17) 0.38513(9) 0.09833(9) 0.0417(6) Uani 1 1 d . . . . .
S5 S 0.59184(17) 0.39521(9) 0.14896(8) 0.0344(6) Uani 1 1 d . . . . .
O1 O 0.3530(4) 0.4614(2) 0.14901(18) 0.0315(14) Uani 1 1 d . . . . .
O2 O 0.5014(4) 0.4713(2) 0.2499(2) 0.0320(14) Uani 1 1 d . . . . .
O3 O 0.4746(4) 0.3459(2) 0.2626(2) 0.0351(14) Uani 1 1 d . . . . .
O4 O 0.3554(4) 0.3228(2) 0.16177(18) 0.0302(14) Uani 1 1 d . . . . .
O5 O 0.5902(4) 0.4603(2) 0.15943(19) 0.0359(14) Uani 1 1 d . . . . .
O6 O 0.5818(4) 0.3632(2) 0.19579(18) 0.0320(14) Uani 1 1 d . . . . .
O7 O 0.5025(4) 0.3778(2) 0.10856(18) 0.0336(14) Uani 1 1 d . . . . .
O8 O 0.6871(4) 0.3785(2) 0.1359(2) 0.0446(16) Uani 1 1 d . . . . .
O9 O 0.3356(4) 0.4408(3) 0.04233(19) 0.0446(16) Uani 1 1 d . . . . .
O10 O 0.5095(5) 0.2328(3) 0.1534(2) 0.0519(17) Uani 1 1 d . . . . .
O11 O 0.6173(5) 0.2498(2) 0.2525(2) 0.0389(15) Uani 1 1 d . . . . .
O12 O 0.6911(4) 0.3297(3) 0.2988(2) 0.0407(15) Uani 1 1 d . . . . .
O13 O 0.8947(4) 0.0745(2) 0.2941(2) 0.0357(14) Uani 1 1 d . . . . .
O14 O 0.9939(5) 0.0753(2) 0.3707(2) 0.0363(14) Uani 1 1 d . . . . .
N1 N 0.3653(6) 0.5243(3) 0.0017(3) 0.052(2) Uani 1 1 d . . . . .
N2 N 0.7215(6) 0.4571(3) 0.2675(3) 0.045(2) Uani 1 1 d . . . . .
N3 N 0.8317(5) 0.1896(3) 0.5522(3) 0.0320(17) Uani 1 1 d . U . . .
N4 N 0.8189(7) 0.2947(4) 0.5345(3) 0.061(2) Uani 1 1 d . . . . .
N5 N 0.6042(14) 0.1826(10) 0.1106(7) 0.205(7) Uani 1 1 d . U . . .
C1 C 0.2616(7) 0.4827(4) 0.1536(3) 0.032(2) Uani 1 1 d . U . . .
C2 C 0.1678(7) 0.4534(4) 0.1319(3) 0.036(2) Uani 1 1 d . U . . .
C3 C 0.0733(7) 0.4772(4) 0.1365(3) 0.047(3) Uani 1 1 d . U . . .
H3A H 0.011495 0.457085 0.119966 0.057 Uiso 1 1 calc R U . . .
C4 C 0.0649(7) 0.5289(4) 0.1639(4) 0.046(2) Uani 1 1 d . U . . .
C5 C 0.1573(7) 0.5577(4) 0.1853(3) 0.041(2) Uani 1 1 d . U . . .
H5A H 0.155674 0.593859 0.203777 0.049 Uiso 1 1 calc R U . . .
C6 C 0.2516(6) 0.5358(4) 0.1805(3) 0.036(2) Uani 1 1 d . U . . .
C7 C 0.4616(7) 0.4965(4) 0.2842(3) 0.035(2) Uani 1 1 d . U . . .
C8 C 0.3941(7) 0.5465(4) 0.2732(3) 0.037(2) Uani 1 1 d . U . . .
C9 C 0.3546(7) 0.5747(4) 0.3096(4) 0.050(3) Uani 1 1 d . U . . .
H9A H 0.310676 0.608793 0.300665 0.060 Uiso 1 1 calc R U . . .
C10 C 0.3771(8) 0.5546(4) 0.3585(4) 0.056(3) Uani 1 1 d . U . . .
C11 C 0.4427(8) 0.5054(4) 0.3703(4) 0.055(3) Uani 1 1 d . U . . .
H11A H 0.460339 0.491024 0.403916 0.066 Uiso 1 1 calc R U . . .
C12 C 0.4838(7) 0.4763(4) 0.3340(3) 0.042(2) Uani 1 1 d . U . . .
C13 C 0.4591(7) 0.3214(4) 0.3034(4) 0.040(2) Uani 1 1 d . U . . .
C14 C 0.4076(7) 0.2660(4) 0.3021(3) 0.040(2) Uani 1 1 d . U . . .
C15 C 0.3901(8) 0.2411(4) 0.3461(4) 0.060(3) Uani 1 1 d . U . . .
H15A H 0.354035 0.203813 0.344196 0.073 Uiso 1 1 calc R U . . .
C16 C 0.4237(8) 0.2692(5) 0.3930(4) 0.061(3) Uani 1 1 d . U . . .
C17 C 0.4774(8) 0.3230(5) 0.3942(4) 0.058(3) Uani 1 1 d . U . . .
H17A H 0.502770 0.342742 0.425536 0.070 Uiso 1 1 calc R U . . .
C18 C 0.4950(7) 0.3488(4) 0.3507(3) 0.046(2) Uani 1 1 d . U . . .
C19 C 0.2675(7) 0.3069(4) 0.1726(3) 0.034(2) Uani 1 1 d . U . . .
C20 C 0.1718(7) 0.3307(4) 0.1465(3) 0.042(2) Uani 1 1 d . U . . .
C21 C 0.0798(8) 0.3140(4) 0.1571(4) 0.063(3) Uani 1 1 d . U . . .
H21A H 0.017346 0.331184 0.137943 0.075 Uiso 1 1 calc R U . . .
C22 C 0.0744(9) 0.2728(5) 0.1947(5) 0.074(3) Uani 1 1 d . U . . .
C23 C 0.1688(8) 0.2479(4) 0.2209(4) 0.057(3) Uani 1 1 d . U . . .
H23A H 0.169030 0.219440 0.246869 0.069 Uiso 1 1 calc R U . . .
C24 C 0.2615(7) 0.2638(4) 0.2099(3) 0.040(2) Uani 1 1 d . U . . .
C25 C 0.7427(9) 0.5041(5) 0.3082(4) 0.081(3) Uani 1 1 d . . . . .
H25A H 0.678681 0.526157 0.308044 0.122 Uiso 1 1 calc R U . . .
H25B H 0.767974 0.484417 0.340812 0.122 Uiso 1 1 calc R U . . .
H25C H 0.795271 0.532349 0.302153 0.122 Uiso 1 1 calc R U . . .
C26 C 0.8164(9) 0.4256(5) 0.2686(4) 0.085(4) Uani 1 1 d . . . . .
H26A H 0.804200 0.394603 0.242241 0.127 Uiso 1 1 calc R U . . .
H26B H 0.868577 0.454237 0.262764 0.127 Uiso 1 1 calc R U . . .
H26C H 0.841281 0.406306 0.301423 0.127 Uiso 1 1 calc R U . . .
C27 C 0.3424(9) 0.4964(5) -0.0476(4) 0.068(3) Uani 1 1 d . U . . .
H27A H 0.351554 0.526110 -0.072643 0.102 Uiso 1 1 calc R U . . .
H27B H 0.389488 0.462265 -0.047477 0.102 Uiso 1 1 calc R U . . .
H27C H 0.270628 0.481861 -0.055834 0.102 Uiso 1 1 calc R U . . .
C28 C 0.3933(9) 0.5892(5) 0.0033(4) 0.083(4) Uani 1 1 d . U . . .
H28A H 0.393726 0.603153 -0.030563 0.124 Uiso 1 1 calc R U . . .
H28B H 0.342481 0.612594 0.016182 0.124 Uiso 1 1 calc R U . . .
H28C H 0.462344 0.594838 0.025504 0.124 Uiso 1 1 calc R U . . .
C29 C 0.3597(7) 0.4953(5) 0.0434(4) 0.052(3) Uani 1 1 d . . . . .
C31 C 0.6785(7) 0.2737(5) 0.2892(3) 0.034(2) Uani 1 1 d . . . . .
C32 C 0.7431(6) 0.2333(4) 0.3267(3) 0.033(2) Uani 1 1 d . U . . .
C33 C 0.7548(7) 0.2474(4) 0.3769(4) 0.043(2) Uani 1 1 d . U . . .
H33A H 0.720941 0.282060 0.385762 0.051 Uiso 1 1 calc R U . . .
C34 C 0.8153(7) 0.2118(4) 0.4151(3) 0.035(2) Uani 1 1 d . . . . .
C35 C 0.8694(6) 0.1633(4) 0.4010(3) 0.037(2) Uani 1 1 d . . . . .
H35A H 0.915014 0.140413 0.426234 0.045 Uiso 1 1 calc R U . . .
C36 C 0.8579(6) 0.1479(4) 0.3509(3) 0.031(2) Uani 1 1 d . . . . .
C37 C 0.7921(6) 0.1821(4) 0.3141(3) 0.033(2) Uani 1 1 d . . . . .
H37A H 0.780470 0.170362 0.279880 0.040 Uiso 1 1 calc R U . . .
C38 C 0.8188(6) 0.2257(4) 0.4686(3) 0.037(2) Uani 1 1 d . . . . .
C39 C 0.8277(6) 0.1802(4) 0.5033(4) 0.041(2) Uani 1 1 d . . . . .
H39A H 0.831338 0.139814 0.492212 0.049 Uiso 1 1 calc R U . . .
C40 C 0.8245(7) 0.2473(5) 0.5644(4) 0.052(3) Uani 1 1 d . . . . .
H40A H 0.823263 0.255389 0.598306 0.062 Uiso 1 1 calc R U . . .
C41 C 0.8157(8) 0.2832(5) 0.4868(4) 0.055(3) Uani 1 1 d . . . . .
H41A H 0.811106 0.316256 0.464200 0.066 Uiso 1 1 calc R U . . .
C42 C -0.0422(7) 0.5541(4) 0.1679(4) 0.061(3) Uani 1 1 d . . . . .
C43 C -0.1233(7) 0.5052(5) 0.1599(4) 0.070(3) Uani 1 1 d . . . . .
H43A H -0.101217 0.473153 0.184805 0.105 Uiso 1 1 calc R U . . .
H43B H -0.189210 0.522207 0.163536 0.105 Uiso 1 1 calc R U . . .
H43C H -0.132188 0.488313 0.126039 0.105 Uiso 1 1 calc R U . . .
C44 C -0.0735(10) 0.6041(6) 0.1302(6) 0.129(6) Uani 1 1 d . . . . .
H44A H -0.019637 0.635333 0.136199 0.193 Uiso 1 1 calc R U . . .
H44B H -0.082054 0.587823 0.096246 0.193 Uiso 1 1 calc R U . . .
H44C H -0.139077 0.621718 0.133743 0.193 Uiso 1 1 calc R U . . .
C45 C -0.0346(9) 0.5815(6) 0.2209(5) 0.110(4) Uani 1 1 d . . . . .
H45A H -0.014288 0.549886 0.246365 0.165 Uiso 1 1 calc R U . . .
H45B H 0.017347 0.613802 0.227107 0.165 Uiso 1 1 calc R U . . .
H45C H -0.102111 0.598072 0.222629 0.165 Uiso 1 1 calc R U . . .
C46 C 0.3352(8) 0.5902(4) 0.3986(3) 0.081(3) Uani 1 1 d D . . . .
C47 C 0.2178(7) 0.5987(6) 0.3798(5) 0.128(5) Uani 1 1 d D . . . .
H47A H 0.202990 0.619688 0.347352 0.192 Uiso 1 1 calc R U . . .
H47B H 0.183769 0.559161 0.375788 0.192 Uiso 1 1 calc R U . . .
H47C H 0.191683 0.622815 0.404154 0.192 Uiso 1 1 calc R U . . .
C48 C 0.3868(8) 0.6528(4) 0.4049(4) 0.093(4) Uani 1 1 d D . . . .
H48A H 0.371150 0.673828 0.372453 0.140 Uiso 1 1 calc R U . . .
H48B H 0.360239 0.676462 0.429333 0.140 Uiso 1 1 calc R U . . .
H48C H 0.462038 0.648102 0.416771 0.140 Uiso 1 1 calc R U . . .
C49 C 0.3598(13) 0.5577(6) 0.4491(4) 0.199(9) Uani 1 1 d D . . . .
H49A H 0.434930 0.552487 0.460796 0.299 Uiso 1 1 calc R U . . .
H49B H 0.334039 0.581621 0.473704 0.299 Uiso 1 1 calc R U . . .
H49C H 0.326125 0.517967 0.445338 0.299 Uiso 1 1 calc R U . . .
C50 C 0.4073(11) 0.2409(5) 0.4425(4) 0.085(3) Uani 1 1 d . . . . .
C51 C 0.3403(12) 0.1857(6) 0.4326(4) 0.110(5) Uani 1 1 d . . . . .
H51A H 0.372126 0.155802 0.414602 0.166 Uiso 1 1 calc R U . . .
H51B H 0.333154 0.168531 0.464604 0.166 Uiso 1 1 calc R U . . .
H51C H 0.271683 0.196688 0.412202 0.166 Uiso 1 1 calc R U . . .
C52 C 0.3585(12) 0.2880(6) 0.4707(5) 0.119(5) Uani 1 1 d . . . . .
H52A H 0.402812 0.323889 0.476989 0.178 Uiso 1 1 calc R U . . .
H52B H 0.289948 0.299163 0.450318 0.178 Uiso 1 1 calc R U . . .
H52C H 0.351419 0.271006 0.502721 0.178 Uiso 1 1 calc R U . . .
C53 C 0.5176(11) 0.2246(6) 0.4756(4) 0.103(4) Uani 1 1 d . . . . .
H53A H 0.560403 0.261170 0.481763 0.154 Uiso 1 1 calc R U . . .
H53B H 0.510753 0.207784 0.507762 0.154 Uiso 1 1 calc R U . . .
H53C H 0.550426 0.194756 0.457999 0.154 Uiso 1 1 calc R U . . .
C54 C -0.0217(8) 0.2590(4) 0.2148(5) 0.114(4) Uani 1 1 d D . . . .
C55 C -0.1150(9) 0.2951(5) 0.1870(6) 0.167(7) Uani 1 1 d D . . . .
H55A H -0.099458 0.338362 0.190906 0.250 Uiso 1 1 calc R U . . .
H55B H -0.131040 0.284474 0.151286 0.250 Uiso 1 1 calc R U . . .
H55C H -0.174768 0.285750 0.200902 0.250 Uiso 1 1 calc R U . . .
C56 C -0.0029(12) 0.2749(8) 0.2718(5) 0.212(9) Uani 1 1 d D . . . .
H56A H 0.057022 0.252246 0.290859 0.317 Uiso 1 1 calc R U . . .
H56B H 0.010435 0.318333 0.276517 0.317 Uiso 1 1 calc R U . . .
H56C H -0.064419 0.264161 0.283865 0.317 Uiso 1 1 calc R U . . .
C57 C -0.0436(8) 0.1913(4) 0.2095(5) 0.107(5) Uani 1 1 d D . . . .
H57A H 0.017337 0.168812 0.227629 0.160 Uiso 1 1 calc R U . . .
H57B H -0.103047 0.181461 0.223455 0.160 Uiso 1 1 calc R U . . .
H57C H -0.059320 0.180186 0.173839 0.160 Uiso 1 1 calc R U . . .
C58 C 0.9177(7) 0.0962(4) 0.3374(4) 0.035(2) Uani 1 1 d . . . . .
C59 C 0.5853(15) 0.2267(8) 0.1427(6) 0.132(6) Uani 1 1 d . U . . .
C60 C 0.721(2) 0.1574(12) 0.1108(10) 0.263(9) Uani 1 1 d . U . . .
H60A H 0.715498 0.126309 0.084909 0.395 Uiso 1 1 calc R U . . .
H60B H 0.763481 0.190854 0.103946 0.395 Uiso 1 1 calc R U . . .
H60C H 0.752011 0.140017 0.143807 0.395 Uiso 1 1 calc R U . . .
C61 C 0.542(2) 0.1239(13) 0.1063(11) 0.263(9) Uani 1 1 d . U . . .
H61A H 0.562979 0.096805 0.082320 0.395 Uiso 1 1 calc R U . . .
H61B H 0.554544 0.104308 0.139299 0.395 Uiso 1 1 calc R U . . .
H61C H 0.467721 0.133039 0.094668 0.395 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 O2 2.007(5) . ?
Ni1 O5 2.030(5) . ?
Ni1 O1 2.076(5) . ?
Ni1 O14 2.108(5) 2_655 ?
Ni1 O13 2.121(5) 2_655 ?
Ni1 S1 2.376(2) . ?
Ni1 C58 2.430(9) 2_655 ?
Ni2 O3 2.008(6) . ?
Ni2 O12 2.019(6) . ?
Ni2 O2 2.038(5) . ?
Ni2 N2 2.074(7) . ?
Ni2 O6 2.126(5) . ?
Ni2 S2 2.447(3) . ?
Ni3 O10 2.005(6) . ?
Ni3 O3 2.008(5) . ?
Ni3 O11 2.045(6) . ?
Ni3 O4 2.058(5) . ?
Ni3 O6 2.078(5) . ?
Ni3 S3 2.461(2) . ?
Ni4 O7 2.011(5) . ?
Ni4 O4 2.063(5) . ?
Ni4 O9 2.086(6) . ?
Ni4 O1 2.105(5) . ?
Ni4 N3 2.137(7) 4_565 ?
Ni4 S4 2.354(2) . ?
S1 C8 1.781(9) . ?
S1 C6 1.787(9) . ?
S2 C12 1.789(9) . ?
S2 C18 1.794(9) . ?
S3 C14 1.773(9) . ?
S3 C24 1.781(9) . ?
S4 C2 1.772(9) . ?
S4 C20 1.781(9) . ?
S5 O8 1.443(6) . ?
S5 O7 1.469(5) . ?
S5 O5 1.470(5) . ?
S5 O6 1.499(5) . ?
O1 C1 1.337(9) . ?
O2 C7 1.307(9) . ?
O3 C13 1.303(10) . ?
O4 C19 1.318(9) . ?
O9 C29 1.246(11) . ?
O10 C59 1.121(18) . ?
O11 C31 1.252(10) . ?
O12 C31 1.269(10) . ?
O13 C58 1.250(10) . ?
O14 C58 1.278(10) . ?
N1 C29 1.329(11) . ?
N1 C27 1.448(11) . ?
N1 C28 1.483(12) . ?
N2 C26 1.434(12) . ?
N2 C25 1.502(12) . ?
N3 C40 1.329(11) . ?
N3 C39 1.344(10) . ?
N4 C40 1.321(11) . ?
N4 C41 1.323(11) . ?
N5 C59 1.38(2) . ?
N5 C61 1.53(3) . ?
N5 C60 1.64(3) . ?
C1 C2 1.405(11) . ?
C1 C6 1.410(11) . ?
C2 C3 1.394(12) . ?
C3 C4 1.386(12) . ?
C3 H3A 0.9500 . ?
C4 C5 1.384(11) . ?
C4 C42 1.557(13) . ?
C5 C6 1.377(11) . ?
C5 H5A 0.9500 . ?
C7 C12 1.401(11) . ?
C7 C8 1.412(12) . ?
C8 C9 1.382(12) . ?
C9 C10 1.375(12) . ?
C9 H9A 0.9500 . ?
C10 C11 1.385(13) . ?
C10 C46 1.559(13) . ?
C11 C12 1.399(12) . ?
C11 H11A 0.9500 . ?
C13 C14 1.400(12) . ?
C13 C18 1.408(12) . ?
C14 C15 1.393(12) . ?
C15 C16 1.401(13) . ?
C15 H15A 0.9500 . ?
C16 C17 1.385(13) . ?
C16 C50 1.557(14) . ?
C17 C18 1.391(12) . ?
C17 H17A 0.9500 . ?
C19 C20 1.405(12) . ?
C19 C24 1.414(12) . ?
C20 C21 1.372(12) . ?
C21 C22 1.390(14) . ?
C21 H21A 0.9500 . ?
C22 C23 1.401(14) . ?
C22 C54 1.537(15) . ?
C23 C24 1.381(12) . ?
C23 H23A 0.9500 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C31 C32 1.475(12) . ?
C32 C33 1.383(11) . ?
C32 C37 1.391(11) . ?
C33 C34 1.400(11) . ?
C33 H33A 0.9500 . ?
C34 C35 1.396(11) . ?
C34 C38 1.486(12) . ?
C35 C36 1.389(11) . ?
C35 H35A 0.9500 . ?
C36 C37 1.392(11) . ?
C36 C58 1.487(12) . ?
C37 H37A 0.9500 . ?
C38 C39 1.371(11) . ?
C38 C41 1.372(12) . ?
C39 H39A 0.9500 . ?
C40 H40A 0.9500 . ?
C41 H41A 0.9500 . ?
C42 C44 1.501(15) . ?
C42 C43 1.507(13) . ?
C42 C45 1.555(15) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 C49 1.525(8) . ?
C46 C47 1.533(9) . ?
C46 C48 1.537(8) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 C51 1.498(16) . ?
C50 C52 1.528(16) . ?
C50 C53 1.571(17) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 C55 1.520(9) . ?
C54 C57 1.526(9) . ?
C54 C56 1.562(9) . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ni1 O5 95.8(2) . . ?
O2 Ni1 O1 94.5(2) . . ?
O5 Ni1 O1 97.8(2) . . ?
O2 Ni1 O14 158.1(2) . 2_655 ?
O5 Ni1 O14 86.0(2) . 2_655 ?
O1 Ni1 O14 106.9(2) . 2_655 ?
O2 Ni1 O13 95.6(2) . 2_655 ?
O5 Ni1 O13 85.4(2) . 2_655 ?
O1 Ni1 O13 169.0(2) . 2_655 ?
O14 Ni1 O13 62.7(2) 2_655 2_655 ?
O2 Ni1 S1 84.90(17) . . ?
O5 Ni1 S1 176.39(17) . . ?
O1 Ni1 S1 85.60(16) . . ?
O14 Ni1 S1 91.95(16) 2_655 . ?
O13 Ni1 S1 91.00(16) 2_655 . ?
O2 Ni1 C58 126.6(3) . 2_655 ?
O5 Ni1 C58 84.5(2) . 2_655 ?
O1 Ni1 C58 138.6(3) . 2_655 ?
O14 Ni1 C58 31.7(3) 2_655 2_655 ?
O13 Ni1 C58 30.9(2) 2_655 2_655 ?
S1 Ni1 C58 92.3(2) . 2_655 ?
O3 Ni2 O12 89.4(2) . . ?
O3 Ni2 O2 88.7(2) . . ?
O12 Ni2 O2 171.1(2) . . ?
O3 Ni2 N2 173.7(3) . . ?
O12 Ni2 N2 94.3(3) . . ?
O2 Ni2 N2 88.3(3) . . ?
O3 Ni2 O6 77.9(2) . . ?
O12 Ni2 O6 90.6(2) . . ?
O2 Ni2 O6 97.5(2) . . ?
N2 Ni2 O6 96.9(2) . . ?
O3 Ni2 S2 82.61(17) . . ?
O12 Ni2 S2 86.38(17) . . ?
O2 Ni2 S2 84.76(17) . . ?
N2 Ni2 S2 102.7(2) . . ?
O6 Ni2 S2 160.31(16) . . ?
O10 Ni3 O3 177.9(2) . . ?
O10 Ni3 O11 86.6(3) . . ?
O3 Ni3 O11 91.6(2) . . ?
O10 Ni3 O4 91.3(2) . . ?
O3 Ni3 O4 90.4(2) . . ?
O11 Ni3 O4 173.8(2) . . ?
O10 Ni3 O6 102.0(2) . . ?
O3 Ni3 O6 79.0(2) . . ?
O11 Ni3 O6 90.6(2) . . ?
O4 Ni3 O6 95.5(2) . . ?
O10 Ni3 S3 97.7(2) . . ?
O3 Ni3 S3 81.23(17) . . ?
O11 Ni3 S3 89.89(17) . . ?
O4 Ni3 S3 84.63(16) . . ?
O6 Ni3 S3 160.25(16) . . ?
O7 Ni4 O4 93.3(2) . . ?
O7 Ni4 O9 88.9(2) . . ?
O4 Ni4 O9 175.6(2) . . ?
O7 Ni4 O1 97.8(2) . . ?
O4 Ni4 O1 95.46(19) . . ?
O9 Ni4 O1 88.1(2) . . ?
O7 Ni4 N3 86.6(2) . 4_565 ?
O4 Ni4 N3 89.5(2) . 4_565 ?
O9 Ni4 N3 86.8(3) . 4_565 ?
O1 Ni4 N3 173.2(2) . 4_565 ?
O7 Ni4 S4 176.93(17) . . ?
O4 Ni4 S4 85.08(17) . . ?
O9 Ni4 S4 92.55(17) . . ?
O1 Ni4 S4 84.92(16) . . ?
N3 Ni4 S4 90.80(18) 4_565 . ?
C8 S1 C6 103.0(4) . . ?
C8 S1 Ni1 95.0(3) . . ?
C6 S1 Ni1 95.7(3) . . ?
C12 S2 C18 105.7(4) . . ?
C12 S2 Ni2 93.2(3) . . ?
C18 S2 Ni2 92.8(3) . . ?
C14 S3 C24 103.9(4) . . ?
C14 S3 Ni3 93.1(3) . . ?
C24 S3 Ni3 93.5(3) . . ?
C2 S4 C20 101.0(4) . . ?
C2 S4 Ni4 96.6(3) . . ?
C20 S4 Ni4 96.0(3) . . ?
O8 S5 O7 110.2(3) . . ?
O8 S5 O5 110.7(3) . . ?
O7 S5 O5 110.9(3) . . ?
O8 S5 O6 110.7(3) . . ?
O7 S5 O6 107.5(3) . . ?
O5 S5 O6 106.7(3) . . ?
C1 O1 Ni1 116.8(5) . . ?
C1 O1 Ni4 116.6(5) . . ?
Ni1 O1 Ni4 126.4(3) . . ?
C7 O2 Ni1 119.4(5) . . ?
C7 O2 Ni2 119.2(5) . . ?
Ni1 O2 Ni2 120.8(3) . . ?
C13 O3 Ni2 117.7(5) . . ?
C13 O3 Ni3 117.7(5) . . ?
Ni2 O3 Ni3 101.2(2) . . ?
C19 O4 Ni3 117.8(5) . . ?
C19 O4 Ni4 118.2(5) . . ?
Ni3 O4 Ni4 123.9(3) . . ?
S5 O5 Ni1 130.5(3) . . ?
S5 O6 Ni3 131.7(3) . . ?
S5 O6 Ni2 128.3(3) . . ?
Ni3 O6 Ni2 95.1(2) . . ?
S5 O7 Ni4 130.7(3) . . ?
C29 O9 Ni4 126.4(6) . . ?
C59 O10 Ni3 122.8(9) . . ?
C31 O11 Ni3 125.8(5) . . ?
C31 O12 Ni2 128.8(5) . . ?
C58 O13 Ni1 88.3(5) . 2_645 ?
C58 O14 Ni1 88.2(5) . 2_645 ?
C29 N1 C27 123.6(8) . . ?
C29 N1 C28 120.4(8) . . ?
C27 N1 C28 116.0(8) . . ?
C26 N2 C25 108.2(8) . . ?
C26 N2 Ni2 113.0(6) . . ?
C25 N2 Ni2 114.8(6) . . ?
C40 N3 C39 114.3(7) . . ?
C40 N3 Ni4 124.5(6) . 4_666 ?
C39 N3 Ni4 121.2(6) . 4_666 ?
C40 N4 C41 116.4(8) . . ?
C59 N5 C61 118.2(19) . . ?
C59 N5 C60 123.5(19) . . ?
C61 N5 C60 101.8(18) . . ?
O1 C1 C2 122.1(7) . . ?
O1 C1 C6 123.0(7) . . ?
C2 C1 C6 115.0(8) . . ?
C3 C2 C1 120.9(8) . . ?
C3 C2 S4 119.6(7) . . ?
C1 C2 S4 119.5(7) . . ?
C4 C3 C2 123.4(8) . . ?
C4 C3 H3A 118.3 . . ?
C2 C3 H3A 118.3 . . ?
C5 C4 C3 115.6(8) . . ?
C5 C4 C42 122.6(8) . . ?
C3 C4 C42 121.7(8) . . ?
C6 C5 C4 122.1(8) . . ?
C6 C5 H5A 118.9 . . ?
C4 C5 H5A 118.9 . . ?
C5 C6 C1 122.9(8) . . ?
C5 C6 S1 118.2(7) . . ?
C1 C6 S1 118.8(7) . . ?
O2 C7 C12 122.5(8) . . ?
O2 C7 C8 121.7(8) . . ?
C12 C7 C8 115.8(8) . . ?
C9 C8 C7 122.0(8) . . ?
C9 C8 S1 119.9(7) . . ?
C7 C8 S1 118.0(7) . . ?
C10 C9 C8 121.8(9) . . ?
C10 C9 H9A 119.1 . . ?
C8 C9 H9A 119.1 . . ?
C9 C10 C11 117.4(9) . . ?
C9 C10 C46 119.5(9) . . ?
C11 C10 C46 122.9(9) . . ?
C10 C11 C12 121.8(9) . . ?
C10 C11 H11A 119.1 . . ?
C12 C11 H11A 119.1 . . ?
C11 C12 C7 121.2(8) . . ?
C11 C12 S2 118.4(7) . . ?
C7 C12 S2 120.3(7) . . ?
O3 C13 C14 121.2(8) . . ?
O3 C13 C18 121.5(8) . . ?
C14 C13 C18 117.3(8) . . ?
C15 C14 C13 120.3(8) . . ?
C15 C14 S3 122.2(7) . . ?
C13 C14 S3 117.3(7) . . ?
C14 C15 C16 122.4(9) . . ?
C14 C15 H15A 118.8 . . ?
C16 C15 H15A 118.8 . . ?
C17 C16 C15 117.0(9) . . ?
C17 C16 C50 120.1(10) . . ?
C15 C16 C50 122.8(10) . . ?
C16 C17 C18 121.5(9) . . ?
C16 C17 H17A 119.3 . . ?
C18 C17 H17A 119.3 . . ?
C17 C18 C13 121.5(9) . . ?
C17 C18 S2 120.8(7) . . ?
C13 C18 S2 117.5(7) . . ?
O4 C19 C20 121.8(8) . . ?
O4 C19 C24 123.2(8) . . ?
C20 C19 C24 114.9(8) . . ?
C21 C20 C19 122.3(8) . . ?
C21 C20 S4 118.8(7) . . ?
C19 C20 S4 118.9(7) . . ?
C20 C21 C22 122.6(10) . . ?
C20 C21 H21A 118.7 . . ?
C22 C21 H21A 118.7 . . ?
C21 C22 C23 116.1(9) . . ?
C21 C22 C54 126.2(10) . . ?
C23 C22 C54 117.1(10) . . ?
C24 C23 C22 121.6(9) . . ?
C24 C23 H23A 119.2 . . ?
C22 C23 H23A 119.2 . . ?
C23 C24 C19 122.4(8) . . ?
C23 C24 S3 117.6(7) . . ?
C19 C24 S3 119.9(7) . . ?
N2 C25 H25A 109.5 . . ?
N2 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
N2 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N2 C26 H26A 109.5 . . ?
N2 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
N2 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N1 C27 H27A 109.5 . . ?
N1 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N1 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N1 C28 H28A 109.5 . . ?
N1 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
N1 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O9 C29 N1 120.9(9) . . ?
O11 C31 O12 127.6(8) . . ?
O11 C31 C32 117.6(8) . . ?
O12 C31 C32 114.8(8) . . ?
C33 C32 C37 118.8(8) . . ?
C33 C32 C31 117.9(8) . . ?
C37 C32 C31 123.3(8) . . ?
C32 C33 C34 121.8(8) . . ?
C32 C33 H33A 119.1 . . ?
C34 C33 H33A 119.1 . . ?
C35 C34 C33 117.8(8) . . ?
C35 C34 C38 122.3(8) . . ?
C33 C34 C38 119.9(8) . . ?
C36 C35 C34 121.4(8) . . ?
C36 C35 H35A 119.3 . . ?
C34 C35 H35A 119.3 . . ?
C35 C36 C37 119.0(8) . . ?
C35 C36 C58 119.6(8) . . ?
C37 C36 C58 121.3(8) . . ?
C32 C37 C36 120.9(8) . . ?
C32 C37 H37A 119.5 . . ?
C36 C37 H37A 119.5 . . ?
C39 C38 C41 115.7(8) . . ?
C39 C38 C34 120.7(8) . . ?
C41 C38 C34 123.6(8) . . ?
N3 C39 C38 123.7(8) . . ?
N3 C39 H39A 118.1 . . ?
C38 C39 H39A 118.1 . . ?
N4 C40 N3 127.1(8) . . ?
N4 C40 H40A 116.5 . . ?
N3 C40 H40A 116.5 . . ?
N4 C41 C38 122.7(9) . . ?
N4 C41 H41A 118.7 . . ?
C38 C41 H41A 118.7 . . ?
C44 C42 C43 111.0(9) . . ?
C44 C42 C45 107.5(10) . . ?
C43 C42 C45 107.6(9) . . ?
C44 C42 C4 108.9(8) . . ?
C43 C42 C4 111.4(8) . . ?
C45 C42 C4 110.3(8) . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C42 C45 H45A 109.5 . . ?
C42 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C42 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C49 C46 C47 110.2(7) . . ?
C49 C46 C48 109.3(7) . . ?
C47 C46 C48 108.5(7) . . ?
C49 C46 C10 111.5(8) . . ?
C47 C46 C10 109.2(8) . . ?
C48 C46 C10 108.0(8) . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C46 C48 H48A 109.5 . . ?
C46 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C46 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C46 C49 H49A 109.5 . . ?
C46 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C46 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C51 C50 C52 110.0(11) . . ?
C51 C50 C16 111.7(10) . . ?
C52 C50 C16 109.3(9) . . ?
C51 C50 C53 110.5(10) . . ?
C52 C50 C53 108.3(11) . . ?
C16 C50 C53 107.0(10) . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C50 C52 H52A 109.5 . . ?
C50 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C50 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C50 C53 H53A 109.5 . . ?
C50 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C50 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C55 C54 C57 110.7(8) . . ?
C55 C54 C22 111.3(9) . . ?
C57 C54 C22 108.5(9) . . ?
C55 C54 C56 107.5(8) . . ?
C57 C54 C56 107.4(8) . . ?
C22 C54 C56 111.4(10) . . ?
C54 C55 H55A 109.5 . . ?
C54 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C54 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C54 C56 H56A 109.5 . . ?
C54 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C54 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C54 C57 H57A 109.5 . . ?
C54 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C54 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
O13 C58 O14 120.9(8) . . ?
O13 C58 C36 120.4(9) . . ?
O14 C58 C36 118.7(9) . . ?
O13 C58 Ni1 60.8(4) . 2_645 ?
O14 C58 Ni1 60.1(4) . 2_645 ?
C36 C58 Ni1 178.8(8) . 2_645 ?
O10 C59 N5 124.3(17) . . ?
N5 C60 H60A 109.5 . . ?
N5 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
N5 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
N5 C61 H61A 109.5 . . ?
N5 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
N5 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?

_refine_diff_density_max         0.841
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.111




# SQUEEZE RESULTS (Version = 230917)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.092 0.408 0.000 964 199 ' '
2 0.037 0.463 0.500 964 199 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
A. L. Spek, Acta Crystallogr., 2015, C71, 9.
;
# start Validation Reply Form
_vrf_THETM01_hang66_0m_sq        
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE:  The current data are best among the data from a couple of crystals.
We believe that it is due to disorder of the solvents which could not be defined from the DF maps.
;
_vrf_REFNR01_hang66_0m_sq        
;
PROBLEM: Ratio of reflections to parameters is < 8 for a
RESPONSE: The crystal does not diffract well at the high 2-theta angle.
;
_vrf_PLAT088_hang66_0m_sq        
;
PROBLEM: Poor Data / Parameter Ratio ....................       7.87 Note  
RESPONSE: The crystal does not diffract well at the high 2-theta angle.
;
_vrf_PLAT220_hang66_0m_sq        
;
PROBLEM: Non-Solvent Resd 1   C   Ueq(max)/Ueq(min) Range        8.3 Ratio 
RESPONSE: It is due to disorder.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_hxx12_0m_sq
_database_code_depnum_ccdc_archive 'CCDC 1562141'
_audit_update_record             
;
2017-12-22 deposited with the CCDC.
2018-01-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C256 H236 Cl4 N16 Ni18.80 O54.80 S16'
_chemical_formula_weight         6171.90

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

_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_H-M_alt        'I 4/m'
_space_group_name_Hall           '-I 4'

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

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

_cell_length_a                   30.0460(12)
_cell_length_b                   30.0460(12)
_cell_length_c                   21.8685(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     19742(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9736
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      25.08

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.038
_exptl_crystal_F_000             6346
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    1.037
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.813
_exptl_absorpt_correction_T_max  0.856
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            111403
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_av_R_equivalents  0.1053
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.779
_diffrn_reflns_theta_max         25.119
_diffrn_reflns_theta_full        25.119
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             9043
_reflns_number_gt                5729
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0854P)²+75.2376P] 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         9043
_refine_ls_number_parameters     482
_refine_ls_number_restraints     737
_refine_ls_R_factor_all          0.1028
_refine_ls_R_factor_gt           0.0546
_refine_ls_wR_factor_ref         0.1825
_refine_ls_wR_factor_gt          0.1485
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2252(4) 0.3160(5) 0.0884(6) 0.0416(17) Uani 1 1 d . . . . .
C2 C 0.2246(5) 0.2905(4) 0.1420(8) 0.0466(12) Uani 1 1 d . U . . .
C3 C 0.1846(5) 0.2805(5) 0.1735(7) 0.068(4) Uani 1 1 d . . . . .
H3 H 0.185399 0.264206 0.209616 0.081 Uiso 1 1 calc R U . . .
C4 C 0.1436(4) 0.2953(6) 0.1497(9) 0.121(5) Uani 1 1 d D . . . .
C5 C 0.1457(5) 0.3222(6) 0.0970(8) 0.066(4) Uani 1 1 d . . . . .
H5 H 0.119488 0.334972 0.082841 0.079 Uiso 1 1 calc R U . . .
C6 C 0.1841(5) 0.3304(5) 0.0655(8) 0.051(3) Uani 1 1 d . . . . .
C7 C 0.3180(5) 0.2241(4) 0.0904(7) 0.0413(13) Uani 1 1 d . U . . .
C8 C 0.2913(4) 0.2233(5) 0.1429(8) 0.0457(12) Uani 1 1 d . U . . .
C9 C 0.2801(6) 0.1831(5) 0.1683(7) 0.076(5) Uani 1 1 d . . . . .
H9 H 0.260115 0.183031 0.200752 0.091 Uiso 1 1 calc R U . . .
C10 C 0.2965(5) 0.1429(4) 0.1486(6) 0.070(3) Uani 1 1 d D . . . .
C11 C 0.3189(6) 0.1428(5) 0.0931(8) 0.069(4) Uani 1 1 d . . . . .
H11 H 0.325578 0.115878 0.074094 0.082 Uiso 1 1 calc R U . . .
C12 C 0.3316(5) 0.1829(5) 0.0656(7) 0.049(3) Uani 1 1 d . . . . .
C13 C 0.4170(5) 0.2989(4) 0.1139(7) 0.041(3) Uani 1 1 d D . . . .
C14 C 0.4605(6) 0.3128(16) 0.1438(14) 0.045(4) Uani 0.5 1 d DG U P A 1
C19 C 0.4608(8) 0.3306(16) 0.2025(14) 0.066(5) Uani 0.5 1 d DG U P A 1
H19 H 0.434077 0.337595 0.221769 0.079 Uiso 0.5 1 calc R U P A 1
C18 C 0.5009(11) 0.3381(10) 0.2323(12) 0.046(5) Uani 0.5 1 d DG . P A 1
C17 C 0.5408(8) 0.3276(13) 0.2035(16) 0.040(6) Uani 0.5 1 d DG . P A 1
H17 H 0.567718 0.332618 0.223410 0.048 Uiso 0.5 1 calc R U P A 1
C16 C 0.5406(6) 0.3098(16) 0.1448(16) 0.041(9) Uani 0.5 1 d DG U P A 1
C15 C 0.5004(7) 0.3024(13) 0.1150(12) 0.041(3) Uani 0.5 1 d DG U P A 1
H15 H 0.500189 0.290409 0.075786 0.049 Uiso 0.5 1 calc R U P A 1
C20 C 0.5834(5) 0.3016(4) 0.1135(7) 0.045(3) Uani 1 1 d . . . . .
C21B C 0.5048(5) 0.3539(4) 0.2980(4) 0.049(3) Uani 0.5 1 d G U P A 1
C24B C 0.4685(4) 0.3763(4) 0.3226(6) 0.063(7) Uani 0.5 1 d G U P A 1
H24B H 0.442955 0.380512 0.299303 0.075 Uiso 0.5 1 calc R U P A 1
N2B N 0.4704(4) 0.3925(4) 0.3821(6) 0.086(5) Uani 0.5 1 d G U P A 1
C23B C 0.5086(5) 0.3863(5) 0.4169(4) 0.108(7) Uani 0.5 1 d G U P A 1
H23B H 0.509877 0.397124 0.456749 0.129 Uiso 0.5 1 calc R U P A 1
N1B N 0.5449(4) 0.3639(5) 0.3923(6) 0.115(6) Uani 0.5 1 d G U P A 1
C22B C 0.5430(4) 0.3477(4) 0.3328(6) 0.102(7) Uani 0.5 1 d G U P A 1
H22B H 0.567246 0.332710 0.316325 0.123 Uiso 0.5 1 calc R U P A 1
C26 C 0.2841(4) 0.0975(4) 0.1790(6) 0.096(3) Uani 1 1 d D U . . .
C27 C 0.2604(5) 0.1026(4) 0.2372(6) 0.143(5) Uani 1 1 d D U . . .
H27A H 0.238493 0.125715 0.233341 0.215 Uiso 1 1 calc R U . . .
H27B H 0.246022 0.075142 0.247619 0.215 Uiso 1 1 calc R U . . .
H27C H 0.281239 0.110452 0.268696 0.215 Uiso 1 1 calc R U . . .
C28 C 0.2459(6) 0.0774(5) 0.1417(9) 0.189(6) Uani 1 1 d D U . . .
H28A H 0.255943 0.071638 0.100762 0.284 Uiso 1 1 calc R U . . .
H28B H 0.236505 0.049998 0.160274 0.284 Uiso 1 1 calc R U . . .
H28C H 0.221440 0.097871 0.140670 0.284 Uiso 1 1 calc R U . . .
C29 C 0.3210(5) 0.0647(4) 0.1661(9) 0.175(6) Uani 1 1 d D U . . .
H29A H 0.330826 0.068022 0.124566 0.263 Uiso 1 1 calc R U . . .
H29B H 0.345481 0.070221 0.193300 0.263 Uiso 1 1 calc R U . . .
H29C H 0.310264 0.034911 0.172223 0.263 Uiso 1 1 calc R U . . .
C30 C 0.1009(3) 0.2890(4) 0.1863(5) 0.145(3) Uani 1 1 d D U . . .
C31 C 0.0759(4) 0.3320(4) 0.1999(7) 0.145(3) Uani 1 1 d D U . . .
H31A H 0.093531 0.350457 0.226355 0.218 Uiso 1 1 calc R U . . .
H31B H 0.048167 0.325150 0.219637 0.218 Uiso 1 1 calc R U . . .
H31C H 0.070154 0.347573 0.162390 0.218 Uiso 1 1 calc R U . . .
C32 C 0.0678(4) 0.2664(5) 0.1436(6) 0.145(3) Uani 1 1 d D U . . .
H32A H 0.078006 0.236953 0.134251 0.218 Uiso 1 1 calc R U . . .
H32B H 0.065240 0.283355 0.106562 0.218 Uiso 1 1 calc R U . . .
H32C H 0.039245 0.264786 0.163241 0.218 Uiso 1 1 calc R U . . .
C33 C 0.1093(4) 0.2785(6) 0.2535(6) 0.145(3) Uani 1 1 d D U . . .
H33A H 0.121480 0.249021 0.257043 0.218 Uiso 1 1 calc R U . . .
H33B H 0.081815 0.280090 0.275665 0.218 Uiso 1 1 calc R U . . .
H33C H 0.130030 0.299611 0.270070 0.218 Uiso 1 1 calc R U . . .
O1 O 0.2605(3) 0.3277(3) 0.0632(4) 0.0402(14) Uani 1 1 d . . . . .
O2 O 0.3276(3) 0.2636(3) 0.0632(4) 0.0411(14) Uani 1 1 d . . . . .
O3 O 0.3820(3) 0.3163(3) 0.1376(5) 0.0488(19) Uani 1 1 d . . . . .
O4 O 0.4196(3) 0.2777(3) 0.0637(4) 0.0434(18) Uani 1 1 d . . . . .
O5 O 0.5801(3) 0.2792(3) 0.0658(4) 0.051(2) Uani 1 1 d . . . . .
O6 O 0.6176(3) 0.3156(3) 0.1382(5) 0.047(2) Uani 1 1 d . . . . .
S1 S 0.27601(12) 0.27593(12) 0.17622(6) 0.0456(3) Uani 1 1 d . . . . .
S2 S 0.3673(2) 0.18419(19) 0.000000 0.0489(11) Uani 1 2 d S T P . .
S3 S 0.18428(19) 0.3668(2) 0.000000 0.0489(11) Uani 1 2 d S T P . .
Cl1 Cl 0.35009(18) 0.35097(18) 0.000000 0.0417(4) Uani 1 2 d S T P . .
O7 O 0.6333(4) 0.3657(4) 0.3707(2) 0.0248(12) Uani 0.5 1 d . U P . .
H7A H 0.666068 0.350561 0.385009 0.037 Uiso 0.5 1 d R U P . .
H7B H 0.628683 0.351511 0.322964 0.037 Uiso 0.5 1 d R U P . .
O8 O 0.5422(8) 0.4584(8) 0.500000 0.0051(14) Uani 0.35 2 d S TU P . .
O9 O 0.6440(4) 0.4296(4) 0.500000 0.0051(14) Uani 0.35 2 d S TU P . .
Ni1 Ni 0.32065(6) 0.32059(6) 0.10317(3) 0.03755(19) Uani 1 1 d . . . . .
Ni2 Ni 0.37401(8) 0.26746(9) 0.000000 0.0378(6) Uani 1 2 d S T P . .
Ni3 Ni 0.26762(9) 0.37395(8) 0.000000 0.0385(6) Uani 1 2 d S T P . .
Ni4 Ni 0.58654(19) 0.41341(19) 0.42715(8) 0.0506(5) Uani 0.35 1 d . . P . .
C14A C 0.4603(6) 0.3087(16) 0.1465(15) 0.045(4) Uani 0.5 1 d DG U P A 2
C19A C 0.4599(9) 0.3355(16) 0.1983(16) 0.066(5) Uani 0.5 1 d DG U P A 2
H19A H 0.432944 0.343803 0.215809 0.079 Uiso 0.5 1 calc R U P A 2
C18A C 0.4997(12) 0.3500(10) 0.2238(14) 0.069(10) Uani 0.5 1 d DG . P A 2
C17A C 0.5400(9) 0.3376(14) 0.1975(19) 0.061(12) Uani 0.5 1 d DG . P A 2
H17A H 0.566636 0.347284 0.214631 0.073 Uiso 0.5 1 calc R U P A 2
C16A C 0.5404(6) 0.3108(16) 0.1458(18) 0.047(10) Uani 0.5 1 d DG U P A 2
C15A C 0.5006(7) 0.2963(13) 0.1202(13) 0.041(3) Uani 0.5 1 d DG U P A 2
H15A H 0.500934 0.278382 0.085582 0.049 Uiso 0.5 1 calc R U P A 2
C21A C 0.4999(6) 0.3802(4) 0.2765(6) 0.081(4) Uani 0.5 1 d G U P A 2
C24A C 0.4678(5) 0.4135(5) 0.2785(7) 0.126(8) Uani 0.5 1 d G U P A 2
H24A H 0.446047 0.414950 0.248342 0.151 Uiso 0.5 1 calc R U P A 2
N2A N 0.4683(6) 0.4446(5) 0.3255(8) 0.162(9) Uani 0.5 1 d G U P A 2
C23A C 0.5009(7) 0.4424(5) 0.3706(7) 0.131(7) Uani 0.5 1 d G U P A 2
H23A H 0.501227 0.463213 0.402027 0.157 Uiso 0.5 1 calc R U P A 2
N1A N 0.5330(6) 0.4091(5) 0.3686(7) 0.114(7) Uani 0.5 1 d G U P A 2
C22A C 0.5325(5) 0.3780(5) 0.3215(7) 0.091(9) Uani 0.5 1 d G U P A 2
H22A H 0.553926 0.355682 0.320207 0.110 Uiso 0.5 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.244(14) . ?
C1 C2 1.400(19) . ?
C1 C6 1.401(17) . ?
C2 C3 1.417(19) . ?
C2 S1 1.773(15) . ?
C3 C4 1.408(19) . ?
C3 H3 0.9300 . ?
C4 C5 1.41(2) . ?
C4 C30 1.524(5) . ?
C5 C6 1.366(19) . ?
C5 H5 0.9300 . ?
C6 S3 1.802(16) . ?
C7 O2 1.358(14) . ?
C7 C8 1.401(19) . ?
C7 C12 1.413(18) . ?
C8 C9 1.372(19) . ?
C8 S1 1.800(15) . ?
C9 C10 1.375(17) . ?
C9 H9 0.9300 . ?
C10 C11 1.387(19) . ?
C10 C26 1.564(11) . ?
C11 C12 1.400(19) . ?
C11 H11 0.9300 . ?
C12 S2 1.792(15) . ?
C13 O4 1.271(15) . ?
C13 O3 1.284(15) . ?
C13 C14A 1.513(18) . ?
C13 C14 1.519(18) . ?
C14 C19 1.3900 . ?
C14 C15 1.3900 . ?
C19 C18 1.3900 . ?
C19 H19 0.9300 . ?
C18 C17 1.3900 . ?
C18 C21B 1.52(2) . ?
C17 C16 1.3900 . ?
C17 H17 0.9300 . ?
C16 C15 1.3900 . ?
C16 C20 1.48(3) . ?
C15 H15 0.9300 . ?
C20 O6 1.236(16) . ?
C20 O5 1.246(15) . ?
C20 C16A 1.50(3) . ?
C21B C24B 1.3900 . ?
C21B C22B 1.3900 . ?
C24B N2B 1.3900 . ?
C24B H24B 0.9300 . ?
N2B C23B 1.3900 . ?
N2B Ni4 2.074(11) 4_565 ?
C23B N1B 1.3900 . ?
C23B H23B 0.9300 . ?
N1B C22B 1.3900 . ?
C22B H22B 0.9300 . ?
C26 C27 1.466(12) . ?
C26 C29 1.511(12) . ?
C26 C28 1.530(14) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 C33 1.524(5) . ?
C30 C32 1.524(5) . ?
C30 C31 1.524(5) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
O1 Ni3 1.972(9) . ?
O1 Ni1 2.019(8) . ?
O2 Ni1 1.933(8) . ?
O2 Ni2 1.967(9) . ?
O3 Ni1 1.996(8) . ?
O4 Ni2 1.978(9) . ?
O5 Ni3 2.024(9) 3_655 ?
O6 Ni1 2.014(9) 3_655 ?
S1 Ni1 2.4801(14) . ?
S2 Ni2 2.510(6) . ?
S3 Ni3 2.513(6) . ?
Cl1 Ni3 2.572(7) . ?
Cl1 Ni1 2.5897(11) 10 ?
Cl1 Ni1 2.5897(11) . ?
Cl1 Ni2 2.610(7) . ?
O7 Ni4 2.356(6) . ?
O7 H7A 1.1287 . ?
O7 H7B 1.1371 . ?
O8 Ni4 2.479(7) . ?
O9 Ni4 2.399(10) . ?
O9 Ni4 2.399(10) 10_556 ?
Ni4 N1A 2.061(13) . ?
C14A C19A 1.3900 . ?
C14A C15A 1.3900 . ?
C19A C18A 1.3900 . ?
C19A H19A 0.9300 . ?
C18A C17A 1.3900 . ?
C18A C21A 1.47(3) . ?
C17A C16A 1.3900 . ?
C17A H17A 0.9300 . ?
C16A C15A 1.3900 . ?
C15A H15A 0.9300 . ?
C21A C24A 1.3900 . ?
C21A C22A 1.3900 . ?
C24A N2A 1.3900 . ?
C24A H24A 0.9300 . ?
N2A C23A 1.3900 . ?
C23A N1A 1.3900 . ?
C23A H23A 0.9300 . ?
N1A C22A 1.3900 . ?
C22A H22A 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 122.4(13) . . ?
O1 C1 C6 120.4(14) . . ?
C2 C1 C6 117.0(13) . . ?
C1 C2 C3 122.4(14) . . ?
C1 C2 S1 118.5(11) . . ?
C3 C2 S1 118.8(12) . . ?
C4 C3 C2 119.6(14) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C5 C4 C3 116.4(12) . . ?
C5 C4 C30 122.5(13) . . ?
C3 C4 C30 120.2(14) . . ?
C6 C5 C4 123.6(14) . . ?
C6 C5 H5 118.2 . . ?
C4 C5 H5 118.2 . . ?
C5 C6 C1 120.6(15) . . ?
C5 C6 S3 120.9(12) . . ?
C1 C6 S3 117.9(12) . . ?
O2 C7 C8 119.7(12) . . ?
O2 C7 C12 122.5(13) . . ?
C8 C7 C12 117.7(13) . . ?
C9 C8 C7 119.1(14) . . ?
C9 C8 S1 123.2(12) . . ?
C7 C8 S1 117.6(11) . . ?
C8 C9 C10 124.0(14) . . ?
C8 C9 H9 118.0 . . ?
C10 C9 H9 118.0 . . ?
C9 C10 C11 116.8(12) . . ?
C9 C10 C26 123.2(12) . . ?
C11 C10 C26 119.1(12) . . ?
C10 C11 C12 120.4(14) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C11 C12 C7 120.8(14) . . ?
C11 C12 S2 121.7(12) . . ?
C7 C12 S2 117.5(11) . . ?
O4 C13 O3 127.0(14) . . ?
O4 C13 C14A 116.8(15) . . ?
O3 C13 C14A 115.8(15) . . ?
O4 C13 C14 117.2(15) . . ?
O3 C13 C14 114.8(15) . . ?
C19 C14 C15 120.0 . . ?
C19 C14 C13 120.6(15) . . ?
C15 C14 C13 118.9(14) . . ?
C14 C19 C18 120.0 . . ?
C14 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C19 C18 C17 120.0 . . ?
C19 C18 C21B 124(2) . . ?
C17 C18 C21B 116(2) . . ?
C16 C17 C18 120.0 . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C15 C16 C17 120.0 . . ?
C15 C16 C20 120.8(19) . . ?
C17 C16 C20 119(2) . . ?
C16 C15 C14 120.0 . . ?
C16 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
O6 C20 O5 128.3(16) . . ?
O6 C20 C16 117.6(17) . . ?
O5 C20 C16 114.0(17) . . ?
O6 C20 C16A 116.6(18) . . ?
O5 C20 C16A 115.1(18) . . ?
C24B C21B C22B 120.0 . . ?
C24B C21B C18 117.4(15) . . ?
C22B C21B C18 122.6(16) . . ?
C21B C24B N2B 120.0 . . ?
C21B C24B H24B 120.0 . . ?
N2B C24B H24B 120.0 . . ?
C23B N2B C24B 120.0 . . ?
C23B N2B Ni4 117.5(8) . 4_565 ?
C24B N2B Ni4 121.1(8) . 4_565 ?
N1B C23B N2B 120.0 . . ?
N1B C23B H23B 120.0 . . ?
N2B C23B H23B 120.0 . . ?
C22B N1B C23B 120.0 . . ?
N1B C22B C21B 120.0 . . ?
N1B C22B H22B 120.0 . . ?
C21B C22B H22B 120.0 . . ?
C27 C26 C29 126.0(12) . . ?
C27 C26 C28 98.2(12) . . ?
C29 C26 C28 101.2(12) . . ?
C27 C26 C10 113.1(10) . . ?
C29 C26 C10 108.3(10) . . ?
C28 C26 C10 107.3(11) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C33 C30 C32 127.3(11) . . ?
C33 C30 C31 94.0(10) . . ?
C32 C30 C31 100.1(10) . . ?
C33 C30 C4 113.1(11) . . ?
C32 C30 C4 106.4(10) . . ?
C31 C30 C4 114.5(11) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C1 O1 Ni3 126.9(9) . . ?
C1 O1 Ni1 122.8(9) . . ?
Ni3 O1 Ni1 106.3(4) . . ?
C7 O2 Ni1 123.6(8) . . ?
C7 O2 Ni2 120.6(8) . . ?
Ni1 O2 Ni2 110.0(4) . . ?
C13 O3 Ni1 129.1(10) . . ?
C13 O4 Ni2 130.1(10) . . ?
C20 O5 Ni3 129.2(10) . 3_655 ?
C20 O6 Ni1 128.7(11) . 3_655 ?
C2 S1 C8 105.7(3) . . ?
C2 S1 Ni1 93.8(5) . . ?
C8 S1 Ni1 94.4(5) . . ?
C12 S2 C12 106.2(10) . 10 ?
C12 S2 Ni2 94.0(5) . . ?
C12 S2 Ni2 94.0(5) 10 . ?
C6 S3 C6 105.4(10) 10 . ?
C6 S3 Ni3 93.2(5) 10 . ?
C6 S3 Ni3 93.2(5) . . ?
Ni3 Cl1 Ni1 76.44(12) . 10 ?
Ni3 Cl1 Ni1 76.44(12) . . ?
Ni1 Cl1 Ni1 121.20(7) 10 . ?
Ni3 Cl1 Ni2 121.55(7) . . ?
Ni1 Cl1 Ni2 75.83(12) 10 . ?
Ni1 Cl1 Ni2 75.83(12) . . ?
Ni4 O7 H7A 128.4 . . ?
Ni4 O7 H7B 129.5 . . ?
H7A O7 H7B 102.1 . . ?
Ni4 O9 Ni4 83.2(4) . 10_556 ?
O2 Ni1 O3 90.8(4) . . ?
O2 Ni1 O6 175.0(4) . 4_565 ?
O3 Ni1 O6 89.15(15) . 4_565 ?
O2 Ni1 O1 89.68(14) . . ?
O3 Ni1 O1 175.7(4) . . ?
O6 Ni1 O1 90.0(4) 4_565 . ?
O2 Ni1 S1 82.6(3) . . ?
O3 Ni1 S1 102.8(3) . . ?
O6 Ni1 S1 102.3(3) 4_565 . ?
O1 Ni1 S1 81.5(3) . . ?
O2 Ni1 Cl1 83.2(3) . . ?
O3 Ni1 Cl1 92.1(3) . . ?
O6 Ni1 Cl1 91.8(3) 4_565 . ?
O1 Ni1 Cl1 83.8(3) . . ?
S1 Ni1 Cl1 159.49(5) . . ?
O2 Ni2 O2 89.3(5) 10 . ?
O2 Ni2 O4 90.3(4) 10 10 ?
O2 Ni2 O4 174.4(4) . 10 ?
O2 Ni2 O4 174.4(4) 10 . ?
O2 Ni2 O4 90.3(4) . . ?
O4 Ni2 O4 89.6(5) 10 . ?
O2 Ni2 S2 83.4(3) 10 . ?
O2 Ni2 S2 83.4(3) . . ?
O4 Ni2 S2 102.1(3) 10 . ?
O4 Ni2 S2 102.1(3) . . ?
O2 Ni2 Cl1 82.0(3) 10 . ?
O2 Ni2 Cl1 82.0(3) . . ?
O4 Ni2 Cl1 92.4(3) 10 . ?
O4 Ni2 Cl1 92.4(3) . . ?
S2 Ni2 Cl1 159.4(2) . . ?
O1 Ni3 O1 89.0(5) . 10 ?
O1 Ni3 O5 90.1(4) . 4_565 ?
O1 Ni3 O5 176.1(4) 10 4_565 ?
O1 Ni3 O5 176.1(4) . 11_565 ?
O1 Ni3 O5 90.1(4) 10 11_565 ?
O5 Ni3 O5 90.6(5) 4_565 11_565 ?
O1 Ni3 S3 80.3(3) . . ?
O1 Ni3 S3 80.3(3) 10 . ?
O5 Ni3 S3 103.3(3) 4_565 . ?
O5 Ni3 S3 103.3(3) 11_565 . ?
O1 Ni3 Cl1 85.2(3) . . ?
O1 Ni3 Cl1 85.2(3) 10 . ?
O5 Ni3 Cl1 91.0(3) 4_565 . ?
O5 Ni3 Cl1 91.0(3) 11_565 . ?
S3 Ni3 Cl1 159.5(2) . . ?
N1A Ni4 O7 95.9(6) . . ?
N2B Ni4 O7 94.2(6) 3_655 . ?
N1A Ni4 O9 170.9(6) . . ?
N2B Ni4 O9 86.0(10) 3_655 . ?
O7 Ni4 O9 92.4(4) . . ?
N1A Ni4 O8 90.8(7) . . ?
N2B Ni4 O8 91.0(8) 3_655 . ?
O7 Ni4 O8 171.6(2) . . ?
O9 Ni4 O8 81.4(6) . . ?
C19A C14A C15A 120.0 . . ?
C19A C14A C13 119.2(15) . . ?
C15A C14A C13 120.2(15) . . ?
C14A C19A C18A 120.0 . . ?
C14A C19A H19A 120.0 . . ?
C18A C19A H19A 120.0 . . ?
C19A C18A C17A 120.0 . . ?
C19A C18A C21A 121(2) . . ?
C17A C18A C21A 119(2) . . ?
C16A C17A C18A 120.0 . . ?
C16A C17A H17A 120.0 . . ?
C18A C17A H17A 120.0 . . ?
C15A C16A C17A 120.0 . . ?
C15A C16A C20 120(2) . . ?
C17A C16A C20 120(2) . . ?
C16A C15A C14A 120.0 . . ?
C16A C15A H15A 120.0 . . ?
C14A C15A H15A 120.0 . . ?
C24A C21A C22A 120.0 . . ?
C24A C21A C18A 117.9(17) . . ?
C22A C21A C18A 122.0(17) . . ?
N2A C24A C21A 120.0 . . ?
N2A C24A H24A 120.0 . . ?
C21A C24A H24A 120.0 . . ?
C24A N2A C23A 120.0 . . ?
N1A C23A N2A 120.0 . . ?
N1A C23A H23A 120.0 . . ?
N2A C23A H23A 120.0 . . ?
C23A N1A C22A 120.0 . . ?
C23A N1A Ni4 118.5(10) . . ?
C22A N1A Ni4 120.7(10) . . ?
N1A C22A C21A 120.0 . . ?
N1A C22A H22A 120.0 . . ?
C21A C22A H22A 120.0 . . ?

_refine_diff_density_max         1.437
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.083



# start Validation Reply Form
_vrf_PLAT430_hxx12_0m_sq         
;
PROBLEM: Short Inter D...A Contact O8       ..O8        .       2.52 Ang.  
RESPONSE: It is due to "H8A-O8-H8B" is a coordinated water molecule.
;
_vrf_PLAT341_hxx12_0m_sq         
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01855 Ang.  
RESPONSE: It is due to the disorder of the tert-butyl groups.
;
_vrf_PLAT420_hxx12_0m_sq         
;
PROBLEM: D-H Without Acceptor      O7       --H7A       .     Please Check 
RESPONSE: The molecule "H7A-O7-H7B" is a coordinated water molecule.
;
# end Validation Reply Form
