# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
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# 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 
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data_nin4tf
_database_code_depnum_ccdc_archive 'CCDC 1868871'
_audit_update_record             
;
2018-12-20 deposited with the CCDC.
2019-01-04 downloaded from the CCDC.
;

_vrf_PLAT058_nin4tf              
;
PROBLEM: Maximum Transmission Factor Missing ............          ?      
RESPONSE: The "SADABS-2004/1 - Bruker Nonius area detector scaling 
and absorption correction" was applied to 3, giving 0.809880 as the 
ratio of minimum to maximum apparent transmission.  
;
_vrf_PLAT059_nin4tf              
;
PROBLEM: Minimum Transmission Factor Missing ............          ?      
RESPONSE: The "SADABS-2004/1 - Bruker Nonius area detector scaling 
and absorption correction" was applied to 3, giving 0.809880 as the 
ratio of minimum to maximum apparent transmission.  
;
_vrf_PLAT260_nin4tf              
; 
PROBLEM: Large Average Ueq of Residue Including       O4W      0.268 Check 
RESPONSE: We are confident about the counterion and lattice water 
content, and the proposed model is kept simple, with no particular disorder
treatment. However, as always in this type of structures, counterions
and lattice solvent molecules fill relatively large voids. This type of alert 
message may be generated by the overestimation of the occupancy of some 
somewhat "disordered" site, that we decided to treat as fully occupied to
avoid overparametrization in the presence of such a particularly and not 
commonly neat structure of this type (for comparison check, for instance, 
CCDC ref. numbers 1868872-1868874).
;
_vrf_PLAT306_nin4tf              
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O1W Check 
RESPONSE: The hydrogen atoms of the coordinated water (2 H2O) and hydroxo 
groups (2 OH-) as well as those of all the crystallization solvent molecules 
(found: 4 H2O in the asymmetric unit) were neither found nor calculated. 
Note that they were obviously included in the UNIT instruction, so there 
would be a discrepancy between the calculated and the reported MW. 
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C56 H46 N16 Ni4 O4, 6(C F3 S O3), 4(H2 O)'
_chemical_formula_sum            'C62 H54 F18 N16 Ni4 O26 S6'
_chemical_formula_weight         2208.41

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   12.4520(5)
_cell_length_b                   13.7523(6)
_cell_length_c                   25.1444(9)
_cell_angle_alpha                91.5590(10)
_cell_angle_beta                 95.7310(10)
_cell_angle_gamma                102.1260(10)
_cell_volume                     4183.6(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    8742
_cell_measurement_theta_min      2.94
_cell_measurement_theta_max      33.47

_exptl_crystal_description       IRREGULAR
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.753
_exptl_crystal_F_000             2232
_exptl_transmission_factor_min   
'Ratio of minimum to maximum apparent transmission:  0.809880'
_exptl_transmission_factor_max   
'Ratio of minimum to maximum apparent transmission:  0.809880'
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.162
_shelx_estimated_absorpt_T_min   0.680
_shelx_estimated_absorpt_T_max   0.801
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   
'SADABS-2004/1 - Bruker Nonius area detector scaling and absorption correction'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker X8 Apex-II CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            78753
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_av_R_equivalents  0.0161
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         2.171
_diffrn_reflns_theta_max         33.496
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             32317
_reflns_number_gt                25333
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013, version 2013-4 (Sheldrick 2013)'
_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)+(0.0838P)²+2.5728P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     Patt
_atom_sites_solution_secondary   Difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         32317
_refine_ls_number_parameters     1189
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0470
_refine_ls_wR_factor_ref         0.1528
_refine_ls_wR_factor_gt          0.1400
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_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 0.16315(2) 0.14461(2) 0.15566(2) 0.02669(5) Uani 1 1 d . . . . .
Ni2 Ni 0.14331(2) 0.31196(2) 0.25822(2) 0.02962(5) Uani 1 1 d . . . . .
Ni3 Ni 0.18360(2) 0.13533(2) 0.35019(2) 0.02946(5) Uani 1 1 d . . . . .
Ni4 Ni 0.22348(2) -0.02155(2) 0.24837(2) 0.02704(5) Uani 1 1 d . . . . .
O4 O 0.10605(10) 0.05254(10) 0.21516(5) 0.0275(2) Uani 1 1 d . . . . .
O3 O 0.28068(10) 0.11457(10) 0.29060(5) 0.0289(2) Uani 1 1 d . . . . .
O2 O 0.08133(10) 0.17191(10) 0.28659(5) 0.0297(2) Uani 1 1 d . . . . .
O1 O 0.24640(10) 0.23516(10) 0.22222(5) 0.0287(2) Uani 1 1 d . . . . .
N1 N 0.05112(13) 0.05316(13) 0.09915(6) 0.0320(3) Uani 1 1 d . . . . .
N2 N 0.02581(12) 0.20485(12) 0.15740(6) 0.0293(3) Uani 1 1 d . . . . .
N3 N 0.02108(13) 0.27443(12) 0.19451(6) 0.0307(3) Uani 1 1 d . . . . .
N4 N 0.02015(15) 0.37964(14) 0.28245(8) 0.0381(4) Uani 1 1 d . . . . .
C1 C 0.06659(19) -0.02977(17) 0.07510(9) 0.0398(4) Uani 1 1 d . . . . .
H1 H 0.1384 -0.0438 0.0788 0.048 Uiso 1 1 calc R U . . .
C2 C -0.0181(2) -0.09635(19) 0.04484(10) 0.0479(5) Uani 1 1 d . . . . .
H2 H -0.0051 -0.1561 0.0294 0.057 Uiso 1 1 calc R U . . .
C3 C -0.1209(2) -0.0744(2) 0.03768(10) 0.0498(5) Uani 1 1 d . . . . .
H3 H -0.1798 -0.1183 0.0166 0.060 Uiso 1 1 calc R U . . .
C4 C -0.13813(18) 0.01301(19) 0.06163(9) 0.0425(5) Uani 1 1 d . . . . .
H4 H -0.2084 0.0301 0.0567 0.051 Uiso 1 1 calc R U . . .
C5 C -0.05077(15) 0.07402(15) 0.09267(7) 0.0331(3) Uani 1 1 d . . . . .
C6 C -0.06434(15) 0.16054(15) 0.12544(8) 0.0335(4) Uani 1 1 d . . . . .
C7 C -0.16451(18) 0.1903(2) 0.12761(10) 0.0468(5) Uani 1 1 d . . . . .
H7 H -0.2272 0.1622 0.1031 0.056 Uiso 1 1 calc R U . . .
C8 C -0.16989(18) 0.2609(2) 0.16585(11) 0.0499(6) Uani 1 1 d . . . . .
H8 H -0.2365 0.2829 0.1689 0.060 Uiso 1 1 calc R U . . .
C9 C -0.07468(16) 0.30007(16) 0.20048(9) 0.0358(4) Uani 1 1 d . . . . .
C10 C -0.07204(17) 0.36758(15) 0.24773(9) 0.0371(4) Uani 1 1 d . . . . .
C11 C -0.1586(2) 0.4131(2) 0.25605(12) 0.0504(6) Uani 1 1 d . . . . .
H11 H -0.2223 0.4036 0.2308 0.061 Uiso 1 1 calc R U . . .
C12 C -0.1497(2) 0.4731(2) 0.30244(13) 0.0595(7) Uani 1 1 d . . . . .
H12 H -0.2082 0.5043 0.3098 0.071 Uiso 1 1 calc R U . . .
C13 C -0.0561(3) 0.4865(2) 0.33715(13) 0.0612(7) Uani 1 1 d . . . . .
H13 H -0.0479 0.5279 0.3688 0.073 Uiso 1 1 calc R U . . .
C14 C 0.0264(2) 0.4392(2) 0.32579(11) 0.0529(6) Uani 1 1 d . . . . .
H14 H 0.0915 0.4496 0.3502 0.064 Uiso 1 1 calc R U . . .
N5 N 0.23676(15) 0.44812(13) 0.23992(8) 0.0391(4) Uani 1 1 d . . . . .
N6 N 0.25898(13) 0.34633(13) 0.32458(7) 0.0336(3) Uani 1 1 d . . . . .
N7 N 0.27028(13) 0.28022(13) 0.36116(6) 0.0327(3) Uani 1 1 d . . . . .
N8 N 0.30085(14) 0.12485(15) 0.41330(7) 0.0376(3) Uani 1 1 d . . . . .
C15 C 0.2257(2) 0.49317(19) 0.19388(12) 0.0509(5) Uani 1 1 d . . . . .
H15 H 0.1687 0.4628 0.1669 0.061 Uiso 1 1 calc R U . . .
C16 C 0.2943(3) 0.5825(2) 0.18420(15) 0.0665(8) Uani 1 1 d . . . . .
H16 H 0.2860 0.6120 0.1507 0.080 Uiso 1 1 calc R U . . .
C17 C 0.3745(3) 0.6278(2) 0.22374(17) 0.0729(9) Uani 1 1 d . . . . .
H17 H 0.4215 0.6897 0.2180 0.087 Uiso 1 1 calc R U . . .
C18 C 0.3869(3) 0.5831(2) 0.27207(14) 0.0633(8) Uani 1 1 d . . . . .
H18 H 0.4413 0.6140 0.3001 0.076 Uiso 1 1 calc R U . . .
C19 C 0.31754(19) 0.49163(16) 0.27836(10) 0.0426(4) Uani 1 1 d . . . . .
C20 C 0.33167(17) 0.43302(16) 0.32558(9) 0.0394(4) Uani 1 1 d . . . . .
C21 C 0.4165(2) 0.4586(2) 0.36787(12) 0.0546(6) Uani 1 1 d . . . . .
H21 H 0.4652 0.5222 0.3704 0.065 Uiso 1 1 calc R U . . .
C22 C 0.4279(2) 0.3909(2) 0.40513(11) 0.0516(6) Uani 1 1 d . . . . .
H22 H 0.4846 0.4061 0.4342 0.062 Uiso 1 1 calc R U . . .
C23 C 0.35441(16) 0.29846(17) 0.39980(8) 0.0373(4) Uani 1 1 d . . . . .
C24 C 0.36427(17) 0.21315(18) 0.43302(8) 0.0392(4) Uani 1 1 d . . . . .
C25 C 0.4342(2) 0.2205(2) 0.48002(10) 0.0531(6) Uani 1 1 d . . . . .
H25 H 0.4778 0.2831 0.4935 0.064 Uiso 1 1 calc R U . . .
C26 C 0.4393(3) 0.1355(3) 0.50688(12) 0.0654(8) Uani 1 1 d . . . . .
H26 H 0.4865 0.1392 0.5393 0.079 Uiso 1 1 calc R U . . .
C27 C 0.3764(3) 0.0455(3) 0.48692(12) 0.0596(7) Uani 1 1 d . . . . .
H27 H 0.3794 -0.0136 0.5051 0.072 Uiso 1 1 calc R U . . .
C28 C 0.3081(2) 0.0429(2) 0.43944(10) 0.0470(5) Uani 1 1 d . . . . .
H28 H 0.2651 -0.0194 0.4251 0.056 Uiso 1 1 calc R U . . .
N9 N 0.06794(14) 0.13269(15) 0.40499(7) 0.0382(4) Uani 1 1 d . . . . .
N10 N 0.09944(12) -0.01006(13) 0.34218(6) 0.0312(3) Uani 1 1 d . . . . .
N11 N 0.11688(12) -0.07177(12) 0.30392(6) 0.0307(3) Uani 1 1 d . . . . .
N12 N 0.14056(13) -0.16035(12) 0.21440(7) 0.0338(3) Uani 1 1 d . . . . .
C29 C 0.0591(2) 0.2080(2) 0.43710(10) 0.0510(6) Uani 1 1 d . . . . .
H29 H 0.1078 0.2707 0.4348 0.061 Uiso 1 1 calc R U . . .
C30 C -0.0179(2) 0.1995(3) 0.47389(12) 0.0588(7) Uani 1 1 d . . . . .
H30 H -0.0216 0.2548 0.4966 0.071 Uiso 1 1 calc R U . . .
C31 C -0.0885(2) 0.1091(3) 0.47664(11) 0.0579(7) Uani 1 1 d . . . . .
H31 H -0.1433 0.1015 0.5008 0.069 Uiso 1 1 calc R U . . .
C32 C -0.0798(2) 0.0288(2) 0.44401(10) 0.0482(5) Uani 1 1 d . . . . .
H32 H -0.1272 -0.0346 0.4459 0.058 Uiso 1 1 calc R U . . .
C33 C 0.00003(16) 0.04347(18) 0.40859(8) 0.0365(4) Uani 1 1 d . . . . .
C34 C 0.01557(15) -0.03709(16) 0.37157(8) 0.0343(4) Uani 1 1 d . . . . .
C35 C -0.05116(19) -0.13270(18) 0.36532(10) 0.0443(5) Uani 1 1 d . . . . .
H35 H -0.1072 -0.1535 0.3881 0.053 Uiso 1 1 calc R U . . .
C36 C -0.03400(18) -0.19552(17) 0.32567(10) 0.0434(5) Uani 1 1 d . . . . .
H36 H -0.0783 -0.2609 0.3198 0.052 Uiso 1 1 calc R U . . .
C37 C 0.05044(15) -0.16115(15) 0.29385(8) 0.0340(3) Uani 1 1 d . . . . .
C38 C 0.06811(17) -0.21417(15) 0.24446(9) 0.0364(4) Uani 1 1 d . . . . .
C39 C 0.0088(2) -0.30869(18) 0.22777(12) 0.0535(6) Uani 1 1 d . . . . .
H39 H -0.0392 -0.3465 0.2503 0.064 Uiso 1 1 calc R U . . .
C40 C 0.0206(3) -0.3474(2) 0.17769(15) 0.0638(8) Uani 1 1 d . . . . .
H40 H -0.0207 -0.4114 0.1650 0.077 Uiso 1 1 calc R U . . .
C41 C 0.0924(3) -0.2921(2) 0.14690(13) 0.0569(6) Uani 1 1 d . . . . .
H41 H 0.1013 -0.3170 0.1124 0.068 Uiso 1 1 calc R U . . .
C42 C 0.1523(2) -0.19928(17) 0.16654(10) 0.0431(4) Uani 1 1 d . . . . .
H42 H 0.2035 -0.1620 0.1452 0.052 Uiso 1 1 calc R U . . .
N13 N 0.36142(13) -0.07557(13) 0.27470(7) 0.0329(3) Uani 1 1 d . . . . .
N14 N 0.32900(12) 0.02847(11) 0.19226(6) 0.0274(3) Uani 1 1 d . . . . .
N15 N 0.30330(12) 0.08841(11) 0.15471(6) 0.0272(3) Uani 1 1 d . . . . .
N16 N 0.24386(14) 0.22735(13) 0.09806(7) 0.0339(3) Uani 1 1 d . . . . .
C43 C 0.37173(19) -0.13071(18) 0.31684(9) 0.0421(4) Uani 1 1 d . . . . .
H43A H 0.3106 -0.1491 0.3369 0.051 Uiso 1 1 calc R U . . .
C44 C 0.4681(2) -0.1623(2) 0.33252(11) 0.0496(5) Uani 1 1 d . . . . .
H44A H 0.4726 -0.2025 0.3625 0.060 Uiso 1 1 calc R U . . .
C45 C 0.5572(2) -0.1344(2) 0.30386(12) 0.0551(6) Uani 1 1 d . . . . .
H45A H 0.6244 -0.1547 0.3139 0.066 Uiso 1 1 calc R U . . .
C46 C 0.54786(18) -0.0764(2) 0.26021(11) 0.0474(5) Uani 1 1 d . . . . .
H46A H 0.6087 -0.0557 0.2402 0.057 Uiso 1 1 calc R U . . .
C47 C 0.44870(15) -0.04922(15) 0.24629(8) 0.0330(3) Uani 1 1 d . . . . .
C48 C 0.43116(14) 0.01277(14) 0.20069(8) 0.0302(3) Uani 1 1 d . . . . .
C49 C 0.51263(16) 0.05431(17) 0.16805(9) 0.0387(4) Uani 1 1 d . . . . .
H49A H 0.5846 0.0409 0.1731 0.046 Uiso 1 1 calc R U . . .
C50 C 0.48551(16) 0.11447(17) 0.12886(9) 0.0377(4) Uani 1 1 d . . . . .
H50A H 0.5377 0.1432 0.1056 0.045 Uiso 1 1 calc R U . . .
C51 C 0.37840(14) 0.13254(14) 0.12401(7) 0.0294(3) Uani 1 1 d . . . . .
C52 C 0.33982(16) 0.20309(15) 0.08768(7) 0.0330(3) Uani 1 1 d . . . . .
C53 C 0.3983(2) 0.2431(2) 0.04667(10) 0.0491(5) Uani 1 1 d . . . . .
H53A H 0.4648 0.2241 0.0398 0.059 Uiso 1 1 calc R U . . .
C54 C 0.3572(3) 0.3120(3) 0.01567(12) 0.0644(8) Uani 1 1 d . . . . .
H54A H 0.3962 0.3418 -0.0124 0.077 Uiso 1 1 calc R U . . .
C55 C 0.2593(3) 0.3365(2) 0.02597(12) 0.0609(7) Uani 1 1 d . . . . .
H55A H 0.2293 0.3825 0.0048 0.073 Uiso 1 1 calc R U . . .
C56 C 0.2052(2) 0.29314(19) 0.06763(10) 0.0459(5) Uani 1 1 d . . . . .
H56A H 0.1382 0.3108 0.0749 0.055 Uiso 1 1 calc R U . . .
O1W O 0.4532(2) 0.3344(2) 0.21538(13) 0.0899(9) Uani 1 1 d . . . . .
O2W O -0.13437(17) 0.1151(2) 0.29588(13) 0.0860(9) Uani 1 1 d . . . . .
S1 S -0.18844(4) -0.08571(5) 0.19762(3) 0.04685(13) Uani 1 1 d . . . . .
O5 O -0.08101(13) -0.08337(15) 0.18069(9) 0.0562(5) Uani 1 1 d . . . . .
O6 O -0.24820(18) -0.01891(18) 0.17195(10) 0.0650(5) Uani 1 1 d . . . . .
O7 O -0.1917(2) -0.0861(2) 0.25451(10) 0.0707(6) Uani 1 1 d . . . . .
C57 C -0.2656(3) -0.2074(3) 0.17232(18) 0.0723(9) Uani 1 1 d . . . . .
F1 F -0.36991(16) -0.22190(19) 0.18164(13) 0.1006(9) Uani 1 1 d . . . . .
F2 F -0.2641(3) -0.2173(3) 0.11981(14) 0.1343(13) Uani 1 1 d . . . . .
F3 F -0.2235(2) -0.27822(19) 0.19498(19) 0.1382(15) Uani 1 1 d . . . . .
S2 S 0.59915(6) 0.21193(7) 0.31789(4) 0.0644(2) Uani 1 1 d . . . . .
O8 O 0.6631(2) 0.1812(3) 0.28009(11) 0.0873(8) Uani 1 1 d . . . . .
O9 O 0.49969(18) 0.1427(3) 0.32516(14) 0.0958(10) Uani 1 1 d . . . . .
O10 O 0.5864(3) 0.3134(3) 0.31286(19) 0.1248(14) Uani 1 1 d . . . . .
C58 C 0.6815(3) 0.2182(5) 0.37993(17) 0.0938(15) Uani 1 1 d . . . . .
F4 F 0.7807(2) 0.2712(3) 0.37987(13) 0.1314(13) Uani 1 1 d . . . . .
F5 F 0.6949(3) 0.1275(4) 0.39163(17) 0.1609(18) Uani 1 1 d . . . . .
F6 F 0.6347(3) 0.2537(5) 0.41866(14) 0.187(2) Uani 1 1 d . . . . .
S3 S 0.65409(9) 0.43362(9) 0.10961(5) 0.0861(3) Uani 1 1 d . . . . .
O11 O 0.7626(4) 0.4796(4) 0.1280(2) 0.162(2) Uani 1 1 d . . . . .
O12 O 0.6334(4) 0.4235(4) 0.05090(16) 0.1270(14) Uani 1 1 d . . . . .
O13 O 0.6097(2) 0.3456(2) 0.13477(16) 0.0962(10) Uani 1 1 d . . . . .
C59 C 0.5679(6) 0.5189(4) 0.1251(2) 0.1102(18) Uani 1 1 d . . . . .
F7 F 0.4604(4) 0.4731(3) 0.11392(19) 0.1495(15) Uani 1 1 d . . . . .
F8 F 0.5911(5) 0.6002(2) 0.10256(16) 0.184(2) Uani 1 1 d . . . . .
F9 F 0.5850(5) 0.5426(3) 0.17768(16) 0.1627(18) Uani 1 1 d . . . . .
S4 S 0.69490(5) 0.68901(5) 0.40124(3) 0.05071(14) Uani 1 1 d . . . . .
O14 O 0.57681(18) 0.66752(17) 0.39896(13) 0.0750(7) Uani 1 1 d . . . . .
O15 O 0.7415(3) 0.6725(2) 0.35297(11) 0.0896(9) Uani 1 1 d . . . . .
O16 O 0.7472(2) 0.77985(16) 0.43097(12) 0.0752(7) Uani 1 1 d . . . . .
C60 C 0.7323(3) 0.5941(3) 0.44261(15) 0.0643(7) Uani 1 1 d . . . . .
F10 F 0.6930(2) 0.50425(16) 0.42025(12) 0.0948(8) Uani 1 1 d . . . . .
F11 F 0.8386(2) 0.6018(3) 0.45147(16) 0.1235(11) Uani 1 1 d . . . . .
F12 F 0.6948(4) 0.5959(3) 0.48989(12) 0.1349(14) Uani 1 1 d . . . . .
S5 S 0.18504(10) 0.70524(6) 0.40732(3) 0.0757(3) Uani 1 1 d . . . . .
O17 O 0.0692(3) 0.6830(3) 0.41851(17) 0.1202(13) Uani 1 1 d . . . . .
O18 O 0.1948(4) 0.6740(3) 0.35478(13) 0.1344(17) Uani 1 1 d . . . . .
O19 O 0.2377(5) 0.8016(2) 0.42569(16) 0.1405(19) Uani 1 1 d . . . . .
C61 C 0.2352(5) 0.6217(4) 0.4494(2) 0.116(2) Uani 1 1 d . . . . .
F13 F 0.3443(4) 0.6351(5) 0.4468(4) 0.304(5) Uani 1 1 d . . . . .
F14 F 0.2193(5) 0.6367(3) 0.50004(14) 0.191(2) Uani 1 1 d . . . . .
F15 F 0.1943(4) 0.5276(2) 0.43520(13) 0.1383(15) Uani 1 1 d . . . . .
S6 S 0.67894(5) 0.14145(6) -0.02942(3) 0.05341(15) Uani 1 1 d . . . . .
O20 O 0.64681(19) 0.1463(2) 0.02340(8) 0.0672(6) Uani 1 1 d . . . . .
O21 O 0.7760(2) 0.2131(3) -0.03848(14) 0.0960(9) Uani 1 1 d . . . . .
O22 O 0.6781(2) 0.0451(2) -0.05152(12) 0.0871(9) Uani 1 1 d . . . . .
C62 C 0.5694(3) 0.1815(3) -0.07094(13) 0.0757(11) Uani 1 1 d . . . . .
F16 F 0.5581(3) 0.2692(3) -0.05650(12) 0.1224(12) Uani 1 1 d . . . . .
F17 F 0.5874(3) 0.1795(3) -0.12224(9) 0.1099(10) Uani 1 1 d . . . . .
F18 F 0.4731(2) 0.1206(3) -0.06733(12) 0.1155(11) Uani 1 1 d . . . . .
O3W O 0.9573(5) 0.5425(5) -0.0809(2) 0.182(3) Uani 1 1 d . . . . .
O4W O 0.8273(6) 0.4141(5) -0.0006(5) 0.268(5) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N15 2.0537(14) . ?
Ni1 N2 2.0545(15) . ?
Ni1 O4 2.0701(13) . ?
Ni1 N16 2.0741(17) . ?
Ni1 N1 2.0775(16) . ?
Ni1 O1 2.1035(13) . ?
Ni1 Ni4 3.4471(3) . ?
Ni1 Ni2 3.4714(3) . ?
Ni2 N6 2.0673(16) . ?
Ni2 N3 2.0704(16) . ?
Ni2 N5 2.0761(18) . ?
Ni2 O1 2.0813(13) . ?
Ni2 N4 2.0845(17) . ?
Ni2 O2 2.0914(14) . ?
Ni2 Ni3 3.4765(4) . ?
Ni3 N10 2.0476(17) . ?
Ni3 N7 2.0538(16) . ?
Ni3 O3 2.0668(13) . ?
Ni3 N8 2.0756(17) . ?
Ni3 O2 2.0830(13) . ?
Ni3 N9 2.0860(17) . ?
Ni3 Ni4 3.4437(3) . ?
Ni4 N11 2.0559(15) . ?
Ni4 N14 2.0577(15) . ?
Ni4 N13 2.0679(16) . ?
Ni4 O4 2.0741(12) . ?
Ni4 O3 2.0784(13) . ?
Ni4 N12 2.0848(17) . ?
O4 O2 2.4855(18) . ?
O4 O5 2.711(2) . ?
O3 O1 2.4888(19) . ?
O3 O9 2.722(3) . ?
O2 O2W 2.671(2) . ?
O1 O1W 2.673(3) . ?
N1 C1 1.335(3) . ?
N1 C5 1.354(2) . ?
N2 N3 1.333(2) . ?
N2 C6 1.335(2) . ?
N3 C9 1.333(2) . ?
N4 C14 1.331(3) . ?
N4 C10 1.349(3) . ?
C1 C2 1.387(3) . ?
C2 C3 1.372(4) . ?
C3 C4 1.396(3) . ?
C4 C5 1.381(3) . ?
C5 C6 1.477(3) . ?
C6 C7 1.398(3) . ?
C7 C8 1.364(3) . ?
C8 C9 1.398(3) . ?
C9 C10 1.481(3) . ?
C10 C11 1.385(3) . ?
C11 C12 1.392(4) . ?
C12 C13 1.361(5) . ?
C13 C14 1.375(4) . ?
N5 C15 1.336(3) . ?
N5 C19 1.351(3) . ?
N6 N7 1.329(3) . ?
N6 C20 1.335(3) . ?
N7 C23 1.333(2) . ?
N8 C28 1.335(3) . ?
N8 C24 1.353(3) . ?
C15 C16 1.384(4) . ?
C16 C17 1.371(5) . ?
C17 C18 1.386(5) . ?
C18 C19 1.391(3) . ?
C19 C20 1.470(3) . ?
C20 C21 1.404(3) . ?
C21 C22 1.357(4) . ?
C22 C23 1.396(3) . ?
C23 C24 1.477(3) . ?
C24 C25 1.384(3) . ?
C25 C26 1.376(5) . ?
C26 C27 1.370(5) . ?
C27 C28 1.390(4) . ?
N9 C29 1.325(3) . ?
N9 C33 1.347(3) . ?
N10 N11 1.330(2) . ?
N10 C34 1.335(2) . ?
N11 C37 1.332(2) . ?
N12 C42 1.337(3) . ?
N12 C38 1.349(3) . ?
C29 C30 1.387(3) . ?
C30 C31 1.372(5) . ?
C31 C32 1.387(4) . ?
C32 C33 1.387(3) . ?
C33 C34 1.484(3) . ?
C34 C35 1.396(3) . ?
C35 C36 1.364(3) . ?
C36 C37 1.396(3) . ?
C37 C38 1.481(3) . ?
C38 C39 1.384(3) . ?
C39 C40 1.387(4) . ?
C40 C41 1.365(5) . ?
C41 C42 1.387(4) . ?
N13 C43 1.331(3) . ?
N13 C47 1.352(2) . ?
N14 N15 1.329(2) . ?
N14 C48 1.332(2) . ?
N15 C51 1.330(2) . ?
N16 C56 1.335(3) . ?
N16 C52 1.354(3) . ?
C43 C44 1.385(3) . ?
C44 C45 1.376(4) . ?
C45 C46 1.384(3) . ?
C46 C47 1.379(3) . ?
C47 C48 1.473(3) . ?
C48 C49 1.406(3) . ?
C49 C50 1.366(3) . ?
C50 C51 1.401(3) . ?
C51 C52 1.471(3) . ?
C52 C53 1.381(3) . ?
C53 C54 1.389(4) . ?
C54 C55 1.377(4) . ?
C55 C56 1.383(4) . ?
O1W O10 2.876(5) . ?
O2W O7 2.848(4) . ?
S1 O6 1.428(2) . ?
S1 O7 1.435(3) . ?
S1 O5 1.4380(18) . ?
S1 C57 1.809(3) . ?
C57 F3 1.317(5) . ?
C57 F1 1.318(4) . ?
C57 F2 1.326(5) . ?
S2 O8 1.409(3) . ?
S2 O9 1.426(3) . ?
S2 O10 1.444(4) . ?
S2 C58 1.769(4) . ?
C58 F4 1.296(5) . ?
C58 F6 1.316(5) . ?
C58 F5 1.330(7) . ?
S3 O11 1.393(4) . ?
S3 O13 1.415(3) . ?
S3 O12 1.471(4) . ?
S3 C59 1.808(6) . ?
C59 F8 1.259(6) . ?
C59 F9 1.339(7) . ?
C59 F7 1.353(7) . ?
S4 O15 1.429(3) . ?
S4 O14 1.433(2) . ?
S4 O16 1.433(2) . ?
S4 C60 1.799(4) . ?
C60 F11 1.302(4) . ?
C60 F10 1.317(4) . ?
C60 F12 1.321(4) . ?
S5 O19 1.393(3) . ?
S5 O18 1.403(3) . ?
S5 O17 1.468(4) . ?
S5 C61 1.751(6) . ?
C61 F15 1.312(5) . ?
C61 F14 1.325(8) . ?
C61 F13 1.339(8) . ?
S6 O22 1.421(3) . ?
S6 O20 1.429(2) . ?
S6 O21 1.432(3) . ?
S6 C62 1.821(3) . ?
C62 F16 1.290(5) . ?
C62 F18 1.323(5) . ?
C62 F17 1.332(4) . ?

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
N15 Ni1 N2 178.31(6) . . ?
N15 Ni1 O4 92.44(5) . . ?
N2 Ni1 O4 88.28(6) . . ?
N15 Ni1 N16 78.08(6) . . ?
N2 Ni1 N16 101.18(7) . . ?
O4 Ni1 N16 170.47(6) . . ?
N15 Ni1 N1 103.28(6) . . ?
N2 Ni1 N1 78.25(6) . . ?
O4 Ni1 N1 89.87(6) . . ?
N16 Ni1 N1 93.21(7) . . ?
N15 Ni1 O1 86.48(5) . . ?
N2 Ni1 O1 92.11(5) . . ?
O4 Ni1 O1 81.77(5) . . ?
N16 Ni1 O1 96.54(6) . . ?
N1 Ni1 O1 167.46(6) . . ?
N15 Ni1 Ni4 59.20(4) . . ?
N2 Ni1 Ni4 121.33(5) . . ?
O4 Ni1 Ni4 33.75(3) . . ?
N16 Ni1 Ni4 136.73(5) . . ?
N1 Ni1 Ni4 102.37(5) . . ?
O1 Ni1 Ni4 75.67(4) . . ?
N15 Ni1 Ni2 119.86(4) . . ?
N2 Ni1 Ni2 58.82(4) . . ?
O4 Ni1 Ni2 77.03(4) . . ?
N16 Ni1 Ni2 106.75(5) . . ?
N1 Ni1 Ni2 135.04(4) . . ?
O1 Ni1 Ni2 33.74(3) . . ?
Ni4 Ni1 Ni2 90.172(8) . . ?
N6 Ni2 N3 176.87(7) . . ?
N6 Ni2 N5 77.83(7) . . ?
N3 Ni2 N5 104.61(7) . . ?
N6 Ni2 O1 89.90(6) . . ?
N3 Ni2 O1 91.98(5) . . ?
N5 Ni2 O1 91.56(6) . . ?
N6 Ni2 N4 100.20(7) . . ?
N3 Ni2 N4 77.89(6) . . ?
N5 Ni2 N4 91.42(7) . . ?
O1 Ni2 N4 169.86(6) . . ?
N6 Ni2 O2 90.90(6) . . ?
N3 Ni2 O2 86.86(6) . . ?
N5 Ni2 O2 167.37(6) . . ?
O1 Ni2 O2 82.64(5) . . ?
N4 Ni2 O2 96.24(6) . . ?
N6 Ni2 Ni1 122.88(5) . . ?
N3 Ni2 Ni1 58.60(4) . . ?
N5 Ni2 Ni1 105.75(5) . . ?
O1 Ni2 Ni1 34.15(3) . . ?
N4 Ni2 Ni1 135.81(5) . . ?
O2 Ni2 Ni1 75.47(4) . . ?
N6 Ni2 Ni3 58.24(5) . . ?
N3 Ni2 Ni3 119.81(5) . . ?
N5 Ni2 Ni3 134.13(5) . . ?
O1 Ni2 Ni3 76.91(4) . . ?
N4 Ni2 Ni3 107.64(6) . . ?
O2 Ni2 Ni3 33.53(3) . . ?
Ni1 Ni2 Ni3 89.216(8) . . ?
N10 Ni3 N7 177.80(7) . . ?
N10 Ni3 O3 92.23(6) . . ?
N7 Ni3 O3 88.75(6) . . ?
N10 Ni3 N8 99.47(7) . . ?
N7 Ni3 N8 78.47(7) . . ?
O3 Ni3 N8 95.54(6) . . ?
N10 Ni3 O2 90.68(6) . . ?
N7 Ni3 O2 91.39(6) . . ?
O3 Ni3 O2 83.07(5) . . ?
N8 Ni3 O2 169.81(7) . . ?
N10 Ni3 N9 78.09(7) . . ?
N7 Ni3 N9 101.02(7) . . ?
O3 Ni3 N9 169.95(6) . . ?
N8 Ni3 N9 88.80(7) . . ?
O2 Ni3 N9 94.23(6) . . ?
N10 Ni3 Ni4 58.98(4) . . ?
N7 Ni3 Ni4 122.22(5) . . ?
O3 Ni3 Ni4 33.93(4) . . ?
N8 Ni3 Ni4 106.02(5) . . ?
O2 Ni3 Ni4 78.41(4) . . ?
N9 Ni3 Ni4 136.05(5) . . ?
N10 Ni3 Ni2 123.28(5) . . ?
N7 Ni3 Ni2 58.89(5) . . ?
O3 Ni3 Ni2 75.46(4) . . ?
N8 Ni3 Ni2 136.22(5) . . ?
O2 Ni3 Ni2 33.69(4) . . ?
N9 Ni3 Ni2 107.48(6) . . ?
Ni4 Ni3 Ni2 90.144(8) . . ?
N11 Ni4 N14 179.49(6) . . ?
N11 Ni4 N13 102.38(6) . . ?
N14 Ni4 N13 78.02(6) . . ?
N11 Ni4 O4 87.55(6) . . ?
N14 Ni4 O4 92.07(5) . . ?
N13 Ni4 O4 169.16(6) . . ?
N11 Ni4 O3 91.87(6) . . ?
N14 Ni4 O3 88.41(6) . . ?
N13 Ni4 O3 93.60(6) . . ?
O4 Ni4 O3 81.60(5) . . ?
N11 Ni4 N12 77.87(7) . . ?
N14 Ni4 N12 101.82(6) . . ?
N13 Ni4 N12 92.15(7) . . ?
O4 Ni4 N12 94.21(6) . . ?
O3 Ni4 N12 169.12(6) . . ?
N11 Ni4 Ni3 58.98(5) . . ?
N14 Ni4 Ni3 121.24(4) . . ?
N13 Ni4 Ni3 106.39(5) . . ?
O4 Ni4 Ni3 74.85(3) . . ?
O3 Ni4 Ni3 33.71(3) . . ?
N12 Ni4 Ni3 135.48(5) . . ?
N11 Ni4 Ni1 120.94(5) . . ?
N14 Ni4 Ni1 58.71(4) . . ?
N13 Ni4 Ni1 135.82(5) . . ?
O4 Ni4 Ni1 33.68(3) . . ?
O3 Ni4 Ni1 77.76(4) . . ?
N12 Ni4 Ni1 104.28(5) . . ?
Ni3 Ni4 Ni1 90.155(8) . . ?
Ni1 O4 Ni4 112.57(5) . . ?
Ni1 O4 O2 103.02(6) . . ?
Ni4 O4 O2 105.96(6) . . ?
Ni1 O4 O5 112.63(7) . . ?
Ni4 O4 O5 108.78(7) . . ?
O2 O4 O5 113.66(7) . . ?
Ni3 O3 Ni4 112.36(6) . . ?
Ni3 O3 O1 105.07(6) . . ?
Ni4 O3 O1 102.30(6) . . ?
Ni3 O3 O9 113.86(9) . . ?
Ni4 O3 O9 111.27(9) . . ?
O1 O3 O9 111.19(9) . . ?
Ni3 O2 Ni2 112.78(6) . . ?
Ni3 O2 O4 100.64(6) . . ?
Ni2 O2 O4 104.24(6) . . ?
Ni3 O2 O2W 114.34(9) . . ?
Ni2 O2 O2W 119.70(9) . . ?
O4 O2 O2W 101.79(8) . . ?
Ni2 O1 Ni1 112.10(6) . . ?
Ni2 O1 O3 102.40(6) . . ?
Ni1 O1 O3 104.07(6) . . ?
Ni2 O1 O1W 116.76(9) . . ?
Ni1 O1 O1W 118.01(9) . . ?
O3 O1 O1W 100.33(9) . . ?
C1 N1 C5 118.50(17) . . ?
C1 N1 Ni1 125.75(14) . . ?
C5 N1 Ni1 115.08(12) . . ?
N3 N2 C6 120.85(15) . . ?
N3 N2 Ni1 121.38(11) . . ?
C6 N2 Ni1 116.93(12) . . ?
N2 N3 C9 120.09(16) . . ?
N2 N3 Ni2 120.78(11) . . ?
C9 N3 Ni2 116.35(13) . . ?
C14 N4 C10 117.19(19) . . ?
C14 N4 Ni2 127.18(17) . . ?
C10 N4 Ni2 115.39(13) . . ?
N1 C1 C2 122.6(2) . . ?
C3 C2 C1 118.8(2) . . ?
C2 C3 C4 119.4(2) . . ?
C5 C4 C3 118.5(2) . . ?
N1 C5 C4 122.12(18) . . ?
N1 C5 C6 115.12(16) . . ?
C4 C5 C6 122.47(18) . . ?
N2 C6 C7 120.94(18) . . ?
N2 C6 C5 114.57(16) . . ?
C7 C6 C5 124.24(18) . . ?
C8 C7 C6 118.23(19) . . ?
C7 C8 C9 118.19(19) . . ?
N3 C9 C8 121.40(18) . . ?
N3 C9 C10 114.60(17) . . ?
C8 C9 C10 123.92(18) . . ?
N4 C10 C11 122.7(2) . . ?
N4 C10 C9 114.79(17) . . ?
C11 C10 C9 122.5(2) . . ?
C10 C11 C12 118.3(3) . . ?
C13 C12 C11 119.1(2) . . ?
C12 C13 C14 119.1(2) . . ?
N4 C14 C13 123.7(3) . . ?
C15 N5 C19 118.7(2) . . ?
C15 N5 Ni2 125.97(17) . . ?
C19 N5 Ni2 115.26(16) . . ?
N7 N6 C20 120.81(17) . . ?
N7 N6 Ni2 121.68(12) . . ?
C20 N6 Ni2 116.93(15) . . ?
N6 N7 C23 121.04(17) . . ?
N6 N7 Ni3 120.98(12) . . ?
C23 N7 Ni3 116.34(15) . . ?
C28 N8 C24 118.81(19) . . ?
C28 N8 Ni3 125.95(16) . . ?
C24 N8 Ni3 114.59(15) . . ?
N5 C15 C16 122.3(3) . . ?
C17 C16 C15 118.9(3) . . ?
C16 C17 C18 119.9(3) . . ?
C17 C18 C19 118.1(3) . . ?
N5 C19 C18 122.0(3) . . ?
N5 C19 C20 115.53(18) . . ?
C18 C19 C20 122.3(2) . . ?
N6 C20 C21 120.1(2) . . ?
N6 C20 C19 114.33(18) . . ?
C21 C20 C19 125.5(2) . . ?
C22 C21 C20 118.8(2) . . ?
C21 C22 C23 118.5(2) . . ?
N7 C23 C22 120.4(2) . . ?
N7 C23 C24 114.72(18) . . ?
C22 C23 C24 124.8(2) . . ?
N8 C24 C25 121.6(2) . . ?
N8 C24 C23 114.66(17) . . ?
C25 C24 C23 123.7(2) . . ?
C26 C25 C24 118.8(3) . . ?
C27 C26 C25 120.0(2) . . ?
C26 C27 C28 118.4(3) . . ?
N8 C28 C27 122.3(3) . . ?
C29 N9 C33 118.65(19) . . ?
C29 N9 Ni3 126.34(16) . . ?
C33 N9 Ni3 114.94(14) . . ?
N11 N10 C34 120.51(17) . . ?
N11 N10 Ni3 121.29(11) . . ?
C34 N10 Ni3 117.53(14) . . ?
N10 N11 C37 120.68(16) . . ?
N10 N11 Ni4 120.68(12) . . ?
C37 N11 Ni4 117.27(13) . . ?
C42 N12 C38 118.35(19) . . ?
C42 N12 Ni4 126.41(15) . . ?
C38 N12 Ni4 115.24(14) . . ?
N9 C29 C30 123.0(3) . . ?
C31 C30 C29 118.2(3) . . ?
C30 C31 C32 119.8(2) . . ?
C31 C32 C33 118.2(2) . . ?
N9 C33 C32 122.1(2) . . ?
N9 C33 C34 115.37(16) . . ?
C32 C33 C34 122.6(2) . . ?
N10 C34 C35 120.9(2) . . ?
N10 C34 C33 113.97(18) . . ?
C35 C34 C33 125.08(18) . . ?
C36 C35 C34 118.37(19) . . ?
C35 C36 C37 118.2(2) . . ?
N11 C37 C36 121.0(2) . . ?
N11 C37 C38 114.40(16) . . ?
C36 C37 C38 124.37(19) . . ?
N12 C38 C39 121.9(2) . . ?
N12 C38 C37 114.86(17) . . ?
C39 C38 C37 123.1(2) . . ?
C38 C39 C40 119.1(2) . . ?
C41 C40 C39 119.0(2) . . ?
C40 C41 C42 119.3(3) . . ?
N12 C42 C41 122.4(2) . . ?
C43 N13 C47 118.55(17) . . ?
C43 N13 Ni4 126.15(14) . . ?
C47 N13 Ni4 115.28(13) . . ?
N15 N14 C48 120.70(15) . . ?
N15 N14 Ni4 121.42(10) . . ?
C48 N14 Ni4 116.88(12) . . ?
N14 N15 C51 120.79(14) . . ?
N14 N15 Ni1 120.45(11) . . ?
C51 N15 Ni1 116.79(12) . . ?
C56 N16 C52 118.40(18) . . ?
C56 N16 Ni1 126.44(15) . . ?
C52 N16 Ni1 114.81(13) . . ?
N13 C43 C44 122.6(2) . . ?
C45 C44 C43 118.7(2) . . ?
C44 C45 C46 119.3(2) . . ?
C47 C46 C45 118.9(2) . . ?
N13 C47 C46 121.98(19) . . ?
N13 C47 C48 115.25(15) . . ?
C46 C47 C48 122.75(18) . . ?
N14 C48 C49 120.89(17) . . ?
N14 C48 C47 114.19(15) . . ?
C49 C48 C47 124.92(16) . . ?
C50 C49 C48 118.24(17) . . ?
C49 C50 C51 118.04(17) . . ?
N15 C51 C50 121.18(17) . . ?
N15 C51 C52 114.11(15) . . ?
C50 C51 C52 124.66(17) . . ?
N16 C52 C53 122.5(2) . . ?
N16 C52 C51 115.00(16) . . ?
C53 C52 C51 122.50(19) . . ?
C52 C53 C54 118.3(2) . . ?
C55 C54 C53 119.4(2) . . ?
C54 C55 C56 119.1(2) . . ?
N16 C56 C55 122.4(2) . . ?
O1 O1W O10 108.51(14) . . ?
O2 O2W O7 104.38(10) . . ?
O6 S1 O7 113.69(15) . . ?
O6 S1 O5 115.33(14) . . ?
O7 S1 O5 114.49(14) . . ?
O6 S1 C57 103.67(17) . . ?
O7 S1 C57 105.14(18) . . ?
O5 S1 C57 102.58(14) . . ?
S1 O5 O4 125.62(12) . . ?
S1 O7 O2W 108.01(15) . . ?
F3 C57 F1 107.6(3) . . ?
F3 C57 F2 108.6(4) . . ?
F1 C57 F2 107.3(3) . . ?
F3 C57 S1 110.9(3) . . ?
F1 C57 S1 111.8(3) . . ?
F2 C57 S1 110.5(3) . . ?
O8 S2 O9 115.4(2) . . ?
O8 S2 O10 113.5(3) . . ?
O9 S2 O10 114.3(2) . . ?
O8 S2 C58 104.73(19) . . ?
O9 S2 C58 104.4(2) . . ?
O10 S2 C58 102.6(3) . . ?
S2 O9 O3 137.5(2) . . ?
S2 O10 O1W 111.3(2) . . ?
F4 C58 F6 108.5(4) . . ?
F4 C58 F5 105.0(4) . . ?
F6 C58 F5 108.7(5) . . ?
F4 C58 S2 113.8(4) . . ?
F6 C58 S2 111.1(3) . . ?
F5 C58 S2 109.5(4) . . ?
O11 S3 O13 115.8(3) . . ?
O11 S3 O12 113.2(3) . . ?
O13 S3 O12 113.1(3) . . ?
O11 S3 C59 107.1(4) . . ?
O13 S3 C59 104.4(2) . . ?
O12 S3 C59 101.5(3) . . ?
F8 C59 F9 105.6(5) . . ?
F8 C59 F7 112.4(6) . . ?
F9 C59 F7 107.1(6) . . ?
F8 C59 S3 113.2(6) . . ?
F9 C59 S3 108.7(4) . . ?
F7 C59 S3 109.4(4) . . ?
O15 S4 O14 117.20(19) . . ?
O15 S4 O16 114.58(15) . . ?
O14 S4 O16 113.61(15) . . ?
O15 S4 C60 102.49(18) . . ?
O14 S4 C60 102.79(15) . . ?
O16 S4 C60 103.58(18) . . ?
F11 C60 F10 105.4(3) . . ?
F11 C60 F12 106.8(4) . . ?
F10 C60 F12 107.3(4) . . ?
F11 C60 S4 113.1(3) . . ?
F10 C60 S4 111.8(3) . . ?
F12 C60 S4 112.0(2) . . ?
O19 S5 O18 118.7(2) . . ?
O19 S5 O17 111.1(3) . . ?
O18 S5 O17 111.1(3) . . ?
O19 S5 C61 108.2(3) . . ?
O18 S5 C61 106.6(3) . . ?
O17 S5 C61 99.2(3) . . ?
F15 C61 F14 108.4(6) . . ?
F15 C61 F13 105.6(5) . . ?
F14 C61 F13 107.9(5) . . ?
F15 C61 S5 114.1(3) . . ?
F14 C61 S5 112.4(4) . . ?
F13 C61 S5 108.0(6) . . ?
O22 S6 O20 116.5(2) . . ?
O22 S6 O21 112.56(19) . . ?
O20 S6 O21 114.83(18) . . ?
O22 S6 C62 103.85(17) . . ?
O20 S6 C62 103.74(14) . . ?
O21 S6 C62 103.3(2) . . ?
F16 C62 F18 106.3(3) . . ?
F16 C62 F17 109.5(4) . . ?
F18 C62 F17 107.1(3) . . ?
F16 C62 S6 112.6(3) . . ?
F18 C62 S6 110.4(3) . . ?
F17 C62 S6 110.7(2) . . ?

_refine_diff_density_max         1.166
_refine_diff_density_min         -1.003
_refine_diff_density_rms         0.084

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_RB39nm
_database_code_depnum_ccdc_archive 'CCDC 1868872'
_audit_update_record             
;
2018-12-20 deposited with the CCDC.
2019-01-04 downloaded from the CCDC.
;

_vrf_THETM01_RB39nm              
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: Crystals of 1 diffracted poorly. One reason could be partial 
solvent loss, but also the intrinsic nature of the crystal.

;
_vrf_PLAT430_RB39nm              
;
PROBLEM: Short Inter D...A Contact  O6A      ..O17W     .       1.93 Ang.  
RESPONSE: All such alerts generally involve disordered atoms and/or 
partially occupied sites. 
;
_vrf_PLAT213_RB39nm              
;
PROBLEM: Atom C78             has ADP max/min Ratio .....        4.1 oblate
RESPONSE: The present data are the best available but as said above the
crystals diffracted poorly so the collected data are not ideal.
;
_vrf_PLAT214_RB39nm              
;
PROBLEM: Atom O4P       (Anion/Solvent) ADP max/min Ratio        5.1 prolat
RESPONSE: Atom O4P belongs to the perchlorate anion [Cl1], hydrogen bonded 
to the core of the tetramer [Ni1-Ni4]. It was a choice not to model the 
perchlorate anions hydrogen-bonded to the tetramers cores over multiple 
positions, but in some cases there are indeed signs of unresolved 
disorder.  
;
_vrf_PLAT260_RB39nm              
;
PROBLEM: Large Average Ueq of Residue Including      O18W      0.156 Check 
RESPONSE: After some free refinement cycles, the occupancies of disordered 
atoms - both oxygen atoms of perchlorate anions and oxygen atoms of lattice 
water molecules (including O18w) - were fixed to values very close to the 
respective refined free variable values, to avoid the appearance of fractional 
occupancies of O and H atoms at the end of the refinement. In some of such 
cases, the fixed site occupancy could, after more refinement cycles, result 
a bit higher or a bit lower than the "real" one.
;
_vrf_PLAT306_RB39nm              
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O1W Check 
RESPONSE: The hydrogen atoms of the coordinated water (2 H2O) and hydroxo 
groups (2 OH-) as well as those of all the crystallization solvent molecules 
(found: 13 H2O in the asymmetric unit = formally 6.5 H2O per tetramer) were 
neither found nor calculated. Note that they were obviously included in the  
UNIT instruction, so there would be a discrepancy between the calculated and 
the reported MW. 
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C56 H46 N16 Ni4 O4), 12(Cl O4), 13(H2 O)'
_chemical_formula_sum            'C112 H118 Cl12 N32 Ni8 O69'
_chemical_formula_weight         3911.46

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'
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      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                   12.3939(6)
_cell_length_b                   26.0105(12)
_cell_length_c                   26.2478(13)
_cell_angle_alpha                112.7939(15)
_cell_angle_beta                 95.4248(17)
_cell_angle_gamma                97.6923(18)
_cell_volume                     7630.6(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5497
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      18.76

_exptl_crystal_description       LAMINAR
_exptl_crystal_colour            AMBER-YELLOW
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_F_000             3988
_exptl_transmission_factor_min   0.6694
_exptl_transmission_factor_max   0.7450
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    1.282
_shelx_estimated_absorpt_T_min   0.715
_shelx_estimated_absorpt_T_max   0.975
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   
'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker X8 Apex-II CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            88475
_diffrn_reflns_av_unetI/netI     0.0942
_diffrn_reflns_av_R_equivalents  0.1001
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.439
_diffrn_reflns_theta_max         24.011
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.803
_diffrn_measured_fraction_theta_full 0.698
_diffrn_reflns_Laue_measured_fraction_max 0.803
_diffrn_reflns_Laue_measured_fraction_full 0.698
_diffrn_reflns_point_group_measured_fraction_max 0.803
_diffrn_reflns_point_group_measured_fraction_full 0.698
_reflns_number_total             19267
_reflns_number_gt                12555
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013, version 2013-4 (Sheldrick 2013)'
_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)+(0.0766P)²+30.6742P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     Patt
_atom_sites_solution_secondary   Difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         19267
_refine_ls_number_parameters     2202
_refine_ls_number_restraints     482
_refine_ls_R_factor_all          0.1088
_refine_ls_R_factor_gt           0.0603
_refine_ls_wR_factor_ref         0.1685
_refine_ls_wR_factor_gt          0.1418
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.118
_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 0.78889(8) 0.81931(4) 0.44004(4) 0.0173(3) Uani 1 1 d . . . . .
Ni2 Ni 0.74652(8) 0.82382(4) 0.57131(4) 0.0164(3) Uani 1 1 d . . . . .
Ni3 Ni 0.75419(8) 0.67879(4) 0.52222(4) 0.0147(3) Uani 1 1 d . . . . .
Ni4 Ni 0.82283(8) 0.68132(4) 0.39890(4) 0.0146(3) Uani 1 1 d . . . . .
O1 O 0.8573(4) 0.8151(2) 0.5148(2) 0.0200(13) Uani 1 1 d . . . . .
O2 O 0.6703(4) 0.7409(2) 0.5144(2) 0.0165(13) Uani 1 1 d . . . . .
O3 O 0.8721(4) 0.7120(2) 0.4853(2) 0.0195(13) Uani 1 1 d . . . . .
O4 O 0.7158(4) 0.7375(2) 0.4224(2) 0.0133(12) Uani 1 1 d . . . . .
N1 N 0.6932(6) 0.8215(3) 0.3719(3) 0.0205(17) Uani 1 1 d . . . . .
C1 C 0.7198(7) 0.8110(4) 0.3215(3) 0.024(2) Uani 1 1 d . . . . .
H1A H 0.7876 0.7987 0.3141 0.029 Uiso 1 1 calc R U . . .
C2 C 0.6550(8) 0.8168(4) 0.2792(4) 0.035(2) Uani 1 1 d . . . . .
H2A H 0.6770 0.8079 0.2435 0.042 Uiso 1 1 calc R U . . .
C3 C 0.5588(8) 0.8355(4) 0.2896(4) 0.039(3) Uani 1 1 d . . . . .
H3A H 0.5128 0.8403 0.2613 0.046 Uiso 1 1 calc R U . . .
C4 C 0.5284(8) 0.8476(4) 0.3425(4) 0.031(2) Uani 1 1 d . . . . .
H4A H 0.4618 0.8609 0.3509 0.038 Uiso 1 1 calc R U . . .
C5 C 0.5970(7) 0.8396(3) 0.3822(3) 0.023(2) Uani 1 1 d . . . . .
N2 N 0.6543(6) 0.8464(3) 0.4734(3) 0.0181(16) Uani 1 1 d . . . . .
C6 C 0.5715(7) 0.8497(3) 0.4386(3) 0.022(2) Uani 1 1 d . . . . .
C7 C 0.4719(8) 0.8603(4) 0.4562(4) 0.039(3) Uani 1 1 d . . . . .
H7A H 0.4135 0.8632 0.4319 0.047 Uiso 1 1 calc R U . . .
C8 C 0.4591(8) 0.8664(4) 0.5086(4) 0.042(3) Uani 1 1 d . . . . .
H8A H 0.3919 0.8742 0.5219 0.051 Uiso 1 1 calc R U . . .
C9 C 0.5458(7) 0.8610(4) 0.5428(3) 0.025(2) Uani 1 1 d . . . . .
N3 N 0.6406(5) 0.8514(3) 0.5248(3) 0.0196(17) Uani 1 1 d . . . . .
C10 C 0.5423(7) 0.8638(4) 0.6000(3) 0.024(2) Uani 1 1 d . . . . .
C11 C 0.4659(7) 0.8901(4) 0.6331(4) 0.038(3) Uani 1 1 d . . . . .
H11D H 0.4091 0.9041 0.6185 0.046 Uiso 1 1 calc R U . . .
C12 C 0.4768(8) 0.8946(4) 0.6881(4) 0.036(3) Uani 1 1 d . . . . .
H12A H 0.4296 0.9139 0.7125 0.043 Uiso 1 1 calc R U . . .
C13 C 0.5556(8) 0.8713(4) 0.7067(4) 0.036(2) Uani 1 1 d . . . . .
H13A H 0.5613 0.8729 0.7437 0.043 Uiso 1 1 calc R U . . .
C14 C 0.6271(7) 0.8455(4) 0.6722(3) 0.025(2) Uani 1 1 d . . . . .
H14A H 0.6819 0.8298 0.6860 0.029 Uiso 1 1 calc R U . . .
N4 N 0.6212(5) 0.8418(3) 0.6192(3) 0.0187(16) Uani 1 1 d . . . . .
N5 N 0.8413(5) 0.8970(3) 0.6346(3) 0.0203(17) Uani 1 1 d . . . . .
C15 C 0.8310(7) 0.9504(3) 0.6444(3) 0.023(2) Uani 1 1 d . . . . .
H15A H 0.7839 0.9571 0.6178 0.027 Uiso 1 1 calc R U . . .
C16 C 0.8863(7) 0.9961(4) 0.6918(4) 0.033(2) Uani 1 1 d . . . . .
H16A H 0.8775 1.0335 0.6973 0.039 Uiso 1 1 calc R U . . .
C17 C 0.9538(8) 0.9873(4) 0.7307(4) 0.040(3) Uani 1 1 d . . . . .
H17A H 0.9928 1.0184 0.7634 0.048 Uiso 1 1 calc R U . . .
C18 C 0.9639(7) 0.9328(4) 0.7216(4) 0.032(2) Uani 1 1 d . . . . .
H18A H 1.0091 0.9258 0.7486 0.038 Uiso 1 1 calc R U . . .
C19 C 0.9087(7) 0.8879(3) 0.6732(3) 0.022(2) Uani 1 1 d . . . . .
N6 N 0.8425(5) 0.7910(3) 0.6161(3) 0.0150(16) Uani 1 1 d . . . . .
C20 C 0.9154(6) 0.8279(4) 0.6594(3) 0.019(2) Uani 1 1 d . . . . .
C21 C 0.9928(7) 0.8100(4) 0.6882(3) 0.023(2) Uani 1 1 d . . . . .
H21A H 1.0420 0.8365 0.7206 0.027 Uiso 1 1 calc R U . . .
C22 C 0.9955(7) 0.7528(4) 0.6684(3) 0.022(2) Uani 1 1 d . . . . .
H22A H 1.0479 0.7389 0.6861 0.027 Uiso 1 1 calc R U . . .
C23 C 0.9189(6) 0.7156(3) 0.6213(3) 0.018(2) Uani 1 1 d . . . . .
N7 N 0.8439(5) 0.7352(3) 0.5974(2) 0.0147(16) Uani 1 1 d . . . . .
C24 C 0.9183(7) 0.6545(3) 0.5917(3) 0.019(2) Uani 1 1 d . . . . .
C25 C 0.9826(7) 0.6250(4) 0.6122(4) 0.028(2) Uani 1 1 d . . . . .
H25A H 1.0304 0.6440 0.6471 0.034 Uiso 1 1 calc R U . . .
C26 C 0.9763(7) 0.5681(4) 0.5815(4) 0.031(2) Uani 1 1 d . . . . .
H26A H 1.0195 0.5471 0.5950 0.037 Uiso 1 1 calc R U . . .
C27 C 0.9067(7) 0.5417(4) 0.5310(4) 0.029(2) Uani 1 1 d . . . . .
H27A H 0.9013 0.5023 0.5091 0.034 Uiso 1 1 calc R U . . .
C28 C 0.8452(7) 0.5730(4) 0.5127(3) 0.022(2) Uani 1 1 d . . . . .
H28A H 0.7968 0.5546 0.4779 0.026 Uiso 1 1 calc R U . . .
N8 N 0.8510(5) 0.6290(3) 0.5422(3) 0.0166(16) Uani 1 1 d . . . . .
N9 N 0.6226(5) 0.6396(3) 0.5453(3) 0.0163(16) Uani 1 1 d . . . . .
C29 C 0.6036(7) 0.6499(3) 0.5974(3) 0.024(2) Uani 1 1 d . . . . .
H29A H 0.6525 0.6795 0.6278 0.029 Uiso 1 1 calc R U . . .
C30 C 0.5162(7) 0.6197(4) 0.6090(3) 0.028(2) Uani 1 1 d . . . . .
H30A H 0.5055 0.6283 0.6466 0.033 Uiso 1 1 calc R U . . .
C31 C 0.4443(8) 0.5765(4) 0.5651(4) 0.034(3) Uani 1 1 d . . . . .
H31A H 0.3828 0.5555 0.5720 0.041 Uiso 1 1 calc R U . . .
C32 C 0.4639(7) 0.5649(4) 0.5121(3) 0.026(2) Uani 1 1 d . . . . .
H32A H 0.4162 0.5352 0.4813 0.032 Uiso 1 1 calc R U . . .
C33 C 0.5526(6) 0.5962(3) 0.5026(3) 0.019(2) Uani 1 1 d . . . . .
N10 N 0.6704(5) 0.6204(3) 0.4463(2) 0.0155(16) Uani 1 1 d . . . . .
C34 C 0.5782(6) 0.5878(3) 0.4469(3) 0.019(2) Uani 1 1 d . . . . .
C35 C 0.5129(7) 0.5494(4) 0.3963(3) 0.026(2) Uani 1 1 d . . . . .
H35A H 0.4512 0.5233 0.3960 0.032 Uiso 1 1 calc R U . . .
C36 C 0.5396(7) 0.5503(4) 0.3478(3) 0.028(2) Uani 1 1 d . . . . .
H36A H 0.4957 0.5256 0.3129 0.033 Uiso 1 1 calc R U . . .
C37 C 0.6337(7) 0.5884(3) 0.3498(3) 0.020(2) Uani 1 1 d . . . . .
N11 N 0.6986(5) 0.6207(3) 0.3986(3) 0.0158(16) Uani 1 1 d . . . . .
C38 C 0.6641(6) 0.6001(3) 0.3022(3) 0.017(2) Uani 1 1 d . . . . .
C39 C 0.6069(7) 0.5725(4) 0.2486(3) 0.026(2) Uani 1 1 d . . . . .
H39A H 0.5481 0.5415 0.2399 0.032 Uiso 1 1 calc R U . . .
C40 C 0.6348(7) 0.5899(4) 0.2073(4) 0.025(2) Uani 1 1 d . . . . .
H40A H 0.5952 0.5715 0.1702 0.030 Uiso 1 1 calc R U . . .
C41 C 0.7221(7) 0.6348(3) 0.2211(3) 0.022(2) Uani 1 1 d . . . . .
H41A H 0.7435 0.6477 0.1936 0.027 Uiso 1 1 calc R U . . .
C42 C 0.7775(7) 0.6605(4) 0.2759(3) 0.021(2) Uani 1 1 d . . . . .
H42A H 0.8377 0.6910 0.2853 0.025 Uiso 1 1 calc R U . . .
N12 N 0.7498(5) 0.6441(3) 0.3158(3) 0.0189(16) Uani 1 1 d . . . . .
C43 C 0.9578(7) 0.5868(3) 0.3776(3) 0.020(2) Uani 1 1 d . . . . .
H43A H 0.8946 0.5656 0.3830 0.024 Uiso 1 1 calc R U . . .
N13 N 0.9548(5) 0.6392(3) 0.3822(3) 0.0169(16) Uani 1 1 d . . . . .
C44 C 1.0484(8) 0.5618(4) 0.3655(4) 0.033(2) Uani 1 1 d . . . . .
H44A H 1.0487 0.5248 0.3642 0.039 Uiso 1 1 calc R U . . .
C45 C 1.1376(8) 0.5909(4) 0.3555(4) 0.038(3) Uani 1 1 d . . . . .
H45A H 1.2003 0.5740 0.3461 0.046 Uiso 1 1 calc R U . . .
C46 C 1.1366(7) 0.6453(4) 0.3591(4) 0.029(2) Uani 1 1 d . . . . .
H46A H 1.1975 0.6660 0.3515 0.035 Uiso 1 1 calc R U . . .
C47 C 1.0452(7) 0.6686(3) 0.3739(3) 0.021(2) Uani 1 1 d . . . . .
N14 N 0.9415(5) 0.7419(3) 0.3942(2) 0.0153(16) Uani 1 1 d . . . . .
C48 C 1.0371(7) 0.7279(3) 0.3821(3) 0.019(2) Uani 1 1 d . . . . .
C49 C 1.1237(7) 0.7683(4) 0.3800(4) 0.030(2) Uani 1 1 d . . . . .
H49A H 1.1922 0.7582 0.3704 0.035 Uiso 1 1 calc R U . . .
C50 C 1.1054(7) 0.8217(3) 0.3921(4) 0.028(2) Uani 1 1 d . . . . .
H50A H 1.1607 0.8501 0.3907 0.033 Uiso 1 1 calc R U . . .
C51 C 1.0045(7) 0.8341(3) 0.4063(3) 0.021(2) Uani 1 1 d . . . . .
N15 N 0.9244(5) 0.7942(3) 0.4065(3) 0.0174(16) Uani 1 1 d . . . . .
C52 C 0.9716(7) 0.8903(3) 0.4210(4) 0.025(2) Uani 1 1 d . . . . .
C53 C 1.0254(8) 0.9331(4) 0.4085(4) 0.034(2) Uani 1 1 d . . . . .
H53A H 1.0897 0.9286 0.3914 0.041 Uiso 1 1 calc R U . . .
C54 C 0.9837(9) 0.9818(4) 0.4213(5) 0.048(3) Uani 1 1 d . . . . .
H54A H 1.0176 1.0114 0.4121 0.057 Uiso 1 1 calc R U . . .
C55 C 0.8916(9) 0.9878(4) 0.4476(4) 0.046(3) Uani 1 1 d . . . . .
H55A H 0.8627 1.0218 0.4574 0.055 Uiso 1 1 calc R U . . .
C56 C 0.8429(8) 0.9442(4) 0.4595(4) 0.031(2) Uani 1 1 d . . . . .
H56A H 0.7796 0.9485 0.4775 0.037 Uiso 1 1 calc R U . . .
N16 N 0.8812(6) 0.8955(3) 0.4468(3) 0.0266(18) Uani 1 1 d . . . . .
Ni5 Ni 0.77290(8) 0.31371(4) -0.04065(4) 0.0134(3) Uani 1 1 d . . . . .
Ni6 Ni 0.73293(8) 0.33883(4) 0.09556(4) 0.0132(3) Uani 1 1 d . . . . .
Ni7 Ni 0.77291(8) 0.20249(4) 0.07302(4) 0.0117(2) Uani 1 1 d . . . . .
Ni8 Ni 0.81887(8) 0.17986(4) -0.06189(4) 0.0129(3) Uani 1 1 d . . . . .
O5 O 0.8422(4) 0.3234(2) 0.0385(2) 0.0139(12) Uani 1 1 d . . . . .
O6 O 0.6706(4) 0.2508(2) 0.0494(2) 0.0142(12) Uani 1 1 d . . . . .
O7 O 0.8772(4) 0.2271(2) 0.0245(2) 0.0149(12) Uani 1 1 d . . . . .
O8 O 0.7073(4) 0.2337(2) -0.0476(2) 0.0132(12) Uani 1 1 d . . . . .
N17 N 0.6763(5) 0.3043(3) -0.1137(3) 0.0167(16) Uani 1 1 d . . . . .
C57 C 0.7059(7) 0.2886(3) -0.1643(3) 0.023(2) Uani 1 1 d . . . . .
H57A H 0.7739 0.2758 -0.1694 0.027 Uiso 1 1 calc R U . . .
C58 C 0.6425(8) 0.2901(4) -0.2092(4) 0.032(2) Uani 1 1 d . . . . .
H58A H 0.6661 0.2784 -0.2447 0.038 Uiso 1 1 calc R U . . .
C59 C 0.5441(8) 0.3090(4) -0.2021(4) 0.036(3) Uani 1 1 d . . . . .
H59A H 0.4989 0.3104 -0.2326 0.043 Uiso 1 1 calc R U . . .
C60 C 0.5116(7) 0.3258(4) -0.1499(3) 0.026(2) Uani 1 1 d . . . . .
H60A H 0.4443 0.3392 -0.1438 0.031 Uiso 1 1 calc R U . . .
C61 C 0.5799(7) 0.3225(3) -0.1068(3) 0.018(2) Uani 1 1 d . . . . .
N18 N 0.6347(5) 0.3419(2) -0.0114(3) 0.0146(16) Uani 1 1 d . . . . .
C62 C 0.5512(6) 0.3378(3) -0.0495(3) 0.0139(19) Uani 1 1 d . . . . .
C63 C 0.4472(7) 0.3448(3) -0.0355(3) 0.021(2) Uani 1 1 d . . . . .
H63A H 0.3886 0.3428 -0.0627 0.026 Uiso 1 1 calc R U . . .
C64 C 0.4305(7) 0.3545(4) 0.0173(3) 0.024(2) Uani 1 1 d . . . . .
H64A H 0.3606 0.3600 0.0282 0.029 Uiso 1 1 calc R U . . .
C65 C 0.5191(7) 0.3562(3) 0.0555(3) 0.018(2) Uani 1 1 d . . . . .
N19 N 0.6189(5) 0.3512(3) 0.0409(3) 0.0147(16) Uani 1 1 d . . . . .
C66 C 0.5115(7) 0.3597(3) 0.1126(3) 0.016(2) Uani 1 1 d . . . . .
C67 C 0.4165(7) 0.3693(4) 0.1362(3) 0.030(2) Uani 1 1 d . . . . .
H67A H 0.3550 0.3763 0.1171 0.036 Uiso 1 1 calc R U . . .
C68 C 0.4142(7) 0.3683(4) 0.1885(4) 0.030(2) Uani 1 1 d . . . . .
H68A H 0.3510 0.3754 0.2062 0.036 Uiso 1 1 calc R U . . .
C69 C 0.5039(7) 0.3571(4) 0.2149(4) 0.025(2) Uani 1 1 d . . . . .
H69A H 0.5030 0.3555 0.2503 0.030 Uiso 1 1 calc R U . . .
C70 C 0.5947(7) 0.3485(3) 0.1886(3) 0.022(2) Uani 1 1 d . . . . .
H70A H 0.6571 0.3416 0.2072 0.026 Uiso 1 1 calc R U . . .
N20 N 0.5994(5) 0.3492(3) 0.1382(3) 0.0156(16) Uani 1 1 d . . . . .
N21 N 0.8158(5) 0.4202(3) 0.1467(3) 0.0136(15) Uani 1 1 d . . . . .
C71 C 0.7987(7) 0.4680(3) 0.1424(3) 0.020(2) Uani 1 1 d . . . . .
H71A H 0.7413 0.4660 0.1147 0.024 Uiso 1 1 calc R U . . .
C72 C 0.8627(8) 0.5211(4) 0.1775(4) 0.030(2) Uani 1 1 d . . . . .
H72A H 0.8496 0.5544 0.1732 0.036 Uiso 1 1 calc R U . . .
C73 C 0.9439(7) 0.5242(4) 0.2180(3) 0.026(2) Uani 1 1 d . . . . .
H73A H 0.9881 0.5598 0.2423 0.032 Uiso 1 1 calc R U . . .
C74 C 0.9615(7) 0.4750(3) 0.2235(3) 0.019(2) Uani 1 1 d . . . . .
H74A H 1.0174 0.4762 0.2516 0.022 Uiso 1 1 calc R U . . .
C75 C 0.8966(6) 0.4244(3) 0.1876(3) 0.0148(19) Uani 1 1 d . . . . .
N22 N 0.8427(5) 0.3238(3) 0.1497(2) 0.0116(15) Uani 1 1 d . . . . .
C76 C 0.9133(6) 0.3686(3) 0.1880(3) 0.0130(19) Uani 1 1 d . . . . .
C77 C 0.9993(6) 0.3626(3) 0.2229(3) 0.017(2) Uani 1 1 d . . . . .
H77A H 1.0457 0.3948 0.2517 0.020 Uiso 1 1 calc R U . . .
C78 C 1.0136(6) 0.3095(3) 0.2141(3) 0.0151(19) Uani 1 1 d . . . . .
H78A H 1.0707 0.3035 0.2368 0.018 Uiso 1 1 calc R U . . .
C79 C 0.9423(6) 0.2630(3) 0.1706(3) 0.0132(19) Uani 1 1 d . . . . .
N23 N 0.8574(5) 0.2720(3) 0.1415(3) 0.0134(15) Uani 1 1 d . . . . .
C80 C 0.9547(6) 0.2033(3) 0.1511(3) 0.0126(19) Uani 1 1 d . . . . .
C81 C 1.0357(6) 0.1851(3) 0.1773(3) 0.0174(19) Uani 1 1 d . . . . .
H81A H 1.0813 0.2108 0.2112 0.021 Uiso 1 1 calc R U . . .
C82 C 1.0484(7) 0.1295(3) 0.1533(4) 0.024(2) Uani 1 1 d . . . . .
H82A H 1.1036 0.1163 0.1701 0.029 Uiso 1 1 calc R U . . .
C83 C 0.9795(7) 0.0930(4) 0.1044(4) 0.025(2) Uani 1 1 d . . . . .
H83A H 0.9879 0.0546 0.0867 0.030 Uiso 1 1 calc R U . . .
C84 C 0.8994(6) 0.1127(3) 0.0816(3) 0.017(2) Uani 1 1 d . . . . .
H84A H 0.8504 0.0869 0.0488 0.021 Uiso 1 1 calc R U . . .
N24 N 0.8875(5) 0.1673(3) 0.1038(3) 0.0143(15) Uani 1 1 d . . . . .
N25 N 0.6521(5) 0.1731(3) 0.1086(3) 0.0153(16) Uani 1 1 d . . . . .
C85 C 0.6411(6) 0.1945(3) 0.1625(3) 0.017(2) Uani 1 1 d . . . . .
H85A H 0.6908 0.2277 0.1879 0.021 Uiso 1 1 calc R U . . .
C86 C 0.5593(7) 0.1696(4) 0.1825(3) 0.026(2) Uani 1 1 d . . . . .
H86A H 0.5504 0.1868 0.2206 0.031 Uiso 1 1 calc R U . . .
C87 C 0.4916(7) 0.1203(3) 0.1471(3) 0.023(2) Uani 1 1 d . . . . .
H87A H 0.4363 0.1024 0.1607 0.028 Uiso 1 1 calc R U . . .
C88 C 0.5036(6) 0.0964(3) 0.0915(3) 0.018(2) Uani 1 1 d . . . . .
H88A H 0.4592 0.0611 0.0665 0.022 Uiso 1 1 calc R U . . .
C89 C 0.5811(6) 0.1247(3) 0.0733(3) 0.0143(19) Uani 1 1 d . . . . .
N26 N 0.6858(5) 0.1331(3) 0.0047(3) 0.0158(16) Uani 1 1 d . . . . .
C90 C 0.5945(6) 0.1065(3) 0.0134(3) 0.0097(18) Uani 1 1 d . . . . .
C91 C 0.5166(6) 0.0670(3) -0.0314(3) 0.0150(19) Uani 1 1 d . . . . .
H91A H 0.4533 0.0470 -0.0249 0.018 Uiso 1 1 calc R U . . .
C92 C 0.5331(6) 0.0580(3) -0.0841(3) 0.018(2) Uani 1 1 d . . . . .
H92A H 0.4811 0.0319 -0.1154 0.021 Uiso 1 1 calc R U . . .
C93 C 0.6293(6) 0.0882(3) -0.0913(3) 0.017(2) Uani 1 1 d . . . . .
N27 N 0.7029(5) 0.1241(2) -0.0478(3) 0.0125(15) Uani 1 1 d . . . . .
C94 C 0.6529(7) 0.0875(3) -0.1464(3) 0.017(2) Uani 1 1 d . . . . .
C95 C 0.5921(7) 0.0502(4) -0.1967(3) 0.026(2) Uani 1 1 d . . . . .
H95A H 0.5336 0.0218 -0.1981 0.031 Uiso 1 1 calc R U . . .
C96 C 0.6170(8) 0.0544(4) -0.2450(3) 0.032(2) Uani 1 1 d . . . . .
H96A H 0.5758 0.0290 -0.2803 0.038 Uiso 1 1 calc R U . . .
C97 C 0.7026(7) 0.0961(4) -0.2414(4) 0.028(2) Uani 1 1 d . . . . .
H97A H 0.7210 0.1000 -0.2742 0.033 Uiso 1 1 calc R U . . .
C98 C 0.7606(7) 0.1316(4) -0.1901(4) 0.024(2) Uani 1 1 d . . . . .
H98A H 0.8197 0.1600 -0.1880 0.029 Uiso 1 1 calc R U . . .
N28 N 0.7378(5) 0.1282(3) -0.1421(3) 0.0176(16) Uani 1 1 d . . . . .
N29 N 0.9549(5) 0.1409(3) -0.0714(3) 0.0152(16) Uani 1 1 d . . . . .
C99 C 0.9632(7) 0.0929(4) -0.0662(4) 0.024(2) Uani 1 1 d . . . . .
H99A H 0.9016 0.0734 -0.0577 0.029 Uiso 1 1 calc R U . . .
C100 C 1.0586(8) 0.0699(4) -0.0725(4) 0.041(3) Uani 1 1 d . . . . .
H10A H 1.0637 0.0366 -0.0663 0.050 Uiso 1 1 calc R U . . .
C101 C 1.1453(8) 0.0962(4) -0.0878(5) 0.046(3) Uani 1 1 d . . . . .
H10B H 1.2102 0.0805 -0.0938 0.056 Uiso 1 1 calc R U . . .
C102 C 1.1371(7) 0.1459(4) -0.0943(4) 0.030(2) Uani 1 1 d . . . . .
H10C H 1.1957 0.1646 -0.1053 0.036 Uiso 1 1 calc R U . . .
C103 C 1.0432(6) 0.1675(3) -0.0847(3) 0.019(2) Uani 1 1 d . . . . .
N30 N 0.9312(5) 0.2359(3) -0.0769(2) 0.0128(15) Uani 1 1 d . . . . .
C104 C 1.0301(7) 0.2233(3) -0.0846(3) 0.017(2) Uani 1 1 d . . . . .
C105 C 1.1146(7) 0.2624(4) -0.0894(3) 0.022(2) Uani 1 1 d . . . . .
H10D H 1.1848 0.2529 -0.0961 0.026 Uiso 1 1 calc R U . . .
C106 C 1.0934(7) 0.3140(3) -0.0841(3) 0.022(2) Uani 1 1 d . . . . .
H10E H 1.1484 0.3414 -0.0871 0.026 Uiso 1 1 calc R U . . .
C107 C 0.9887(6) 0.3255(3) -0.0743(3) 0.0163(19) Uani 1 1 d . . . . .
N31 N 0.9105(5) 0.2871(3) -0.0713(3) 0.0140(15) Uani 1 1 d . . . . .
C108 C 0.9521(7) 0.3806(3) -0.0656(3) 0.020(2) Uani 1 1 d . . . . .
C109 C 1.0074(7) 0.4193(3) -0.0824(3) 0.023(2) Uani 1 1 d . . . . .
H10F H 1.0729 0.4130 -0.0981 0.028 Uiso 1 1 calc R U . . .
C110 C 0.9644(8) 0.4677(4) -0.0757(4) 0.033(2) Uani 1 1 d . . . . .
H11A H 0.9993 0.4953 -0.0872 0.039 Uiso 1 1 calc R U . . .
C111 C 0.8706(7) 0.4749(3) -0.0521(4) 0.027(2) Uani 1 1 d . . . . .
H11B H 0.8397 0.5077 -0.0470 0.032 Uiso 1 1 calc R U . . .
C112 C 0.8214(7) 0.4345(4) -0.0358(3) 0.023(2) Uani 1 1 d . . . . .
H11C H 0.7571 0.4404 -0.0189 0.028 Uiso 1 1 calc R U . . .
N32 N 0.8609(5) 0.3868(3) -0.0429(3) 0.0178(16) Uani 1 1 d . . . . .
Cl1 Cl 0.43555(18) 0.69203(11) 0.35354(10) 0.0381(6) Uani 1 1 d . . . . .
O1P O 0.3657(5) 0.7298(3) 0.3503(3) 0.0497(19) Uani 1 1 d . . . . .
O2P O 0.3795(6) 0.6359(3) 0.3187(5) 0.104(4) Uani 1 1 d . . . . .
O3P O 0.5366(4) 0.7033(2) 0.3335(2) 0.0258(14) Uani 1 1 d . . . . .
O4P O 0.4615(6) 0.6981(7) 0.4087(4) 0.149(6) Uani 1 1 d . . . . .
Cl2 Cl 1.1765(4) 0.7536(2) 0.5298(3) 0.0875(15) Uani 0.600(4) 1 d D U P A 1
O5P O 1.0904(12) 0.7107(6) 0.5264(7) 0.105(4) Uani 0.600(4) 1 d D U P A 1
O6P O 1.2425(10) 0.7310(7) 0.4858(5) 0.128(4) Uani 0.600(4) 1 d D U P A 1
O7P O 1.2527(11) 0.7798(8) 0.5800(5) 0.150(5) Uani 0.600(4) 1 d D U P A 1
O8P O 1.1344(14) 0.7954(6) 0.5125(7) 0.140(4) Uani 0.600(4) 1 d D U P A 1
O2W O 1.0532(11) 0.8879(7) 0.5619(8) 0.054(3) Uani 0.600(4) 1 d . U P A 1
Cl2A Cl 1.1444(6) 0.8663(4) 0.5823(4) 0.0875(15) Uani 0.400(4) 1 d D U P A 2
O5A O 1.0519(19) 0.8879(13) 0.5674(13) 0.105(4) Uani 0.400(4) 1 d D U P A 2
O6A O 1.1829(16) 0.8951(10) 0.6420(6) 0.128(4) Uani 0.400(4) 1 d D U P A 2
O7A O 1.2285(15) 0.8699(11) 0.5501(8) 0.150(5) Uani 0.400(4) 1 d D U P A 2
O8A O 1.109(2) 0.8079(6) 0.5754(11) 0.140(4) Uani 0.400(4) 1 d D U P A 2
O2WA O 1.0792(14) 0.6882(8) 0.5076(10) 0.054(3) Uani 0.400(4) 1 d . . P A 2
Cl3 Cl 1.13012(18) 0.39460(10) 0.09233(11) 0.0359(6) Uani 1 1 d . . . . .
O9P O 1.1727(8) 0.3606(6) 0.0466(4) 0.144(6) Uani 1 1 d . . . . .
O10P O 1.0299(5) 0.4089(3) 0.0740(3) 0.054(2) Uani 1 1 d . . . . .
O11P O 1.1110(6) 0.3657(3) 0.1264(3) 0.057(2) Uani 1 1 d . . . . .
O12P O 1.2064(7) 0.4449(4) 0.1234(5) 0.129(5) Uani 1 1 d . . . . .
Cl4 Cl 0.42382(16) 0.17700(9) -0.12832(9) 0.0246(5) Uani 1 1 d . . . . .
O13P O 0.3701(6) 0.1204(3) -0.1539(4) 0.089(3) Uani 1 1 d . . . . .
O14P O 0.5229(5) 0.1859(3) -0.1502(3) 0.0354(16) Uani 1 1 d . . . . .
O15P O 0.4553(7) 0.1921(5) -0.0704(3) 0.104(4) Uani 1 1 d . . . . .
O16P O 0.3507(5) 0.2126(3) -0.1354(3) 0.0402(17) Uani 1 1 d . . . . .
Cl5 Cl 0.31630(16) 0.23816(9) 0.24751(8) 0.0224(5) Uani 1 1 d . . . . .
O17P O 0.4268(4) 0.2651(2) 0.2774(2) 0.0295(15) Uani 1 1 d . . . . .
O18P O 0.2408(4) 0.2450(2) 0.2873(2) 0.0261(14) Uani 1 1 d . . . . .
O19P O 0.3115(5) 0.1785(2) 0.2151(2) 0.0310(15) Uani 1 1 d . . . . .
O20P O 0.2844(5) 0.2648(2) 0.2106(2) 0.0287(15) Uani 1 1 d . . . . .
Cl6 Cl 0.25922(17) 0.43476(9) 0.33502(9) 0.0267(5) Uani 1 1 d . . . . .
O21P O 0.2886(5) 0.4616(3) 0.3949(2) 0.049(2) Uani 1 1 d . . . . .
O22P O 0.3575(5) 0.4388(3) 0.3111(2) 0.0381(17) Uani 1 1 d . . . . .
O23P O 0.2093(5) 0.3764(2) 0.3177(3) 0.0379(17) Uani 1 1 d . . . . .
O24P O 0.1824(6) 0.4629(3) 0.3173(3) 0.058(2) Uani 1 1 d . . . . .
Cl7 Cl 0.75750(18) 0.44654(9) 0.32949(9) 0.0353(6) Uani 1 1 d . . . . .
O25P O 0.6855(5) 0.3943(3) 0.3216(2) 0.0405(18) Uani 1 1 d . . . . .
O26P O 0.7706(7) 0.4860(3) 0.3862(3) 0.075(3) Uani 1 1 d . . . . .
O27P O 0.8610(5) 0.4336(3) 0.3145(2) 0.0360(16) Uani 1 1 d . . . . .
O28P O 0.7122(6) 0.4717(3) 0.2930(3) 0.057(2) Uani 1 1 d . . . . .
Cl8 Cl 0.22495(17) 0.03030(8) 0.04401(9) 0.0249(5) Uani 1 1 d . . . . .
O29P O 0.2543(5) 0.0811(3) 0.0361(3) 0.056(2) Uani 1 1 d . . . . .
O30P O 0.2406(6) 0.0427(4) 0.1026(3) 0.076(3) Uani 1 1 d . . . . .
O31P O 0.2957(5) -0.0076(3) 0.0187(3) 0.055(2) Uani 1 1 d . . . . .
O32P O 0.1116(4) 0.0047(2) 0.0193(2) 0.0285(15) Uani 1 1 d . . . . .
Cl9 Cl 0.64518(18) 0.54080(10) 0.05034(9) 0.0293(6) Uani 1 1 d . . . . .
O33P O 0.7284(5) 0.5812(3) 0.0951(3) 0.058(2) Uani 1 1 d . . . . .
O34P O 0.5397(5) 0.5546(2) 0.0608(3) 0.0335(16) Uani 1 1 d . . . . .
O35P O 0.6680(5) 0.5433(3) -0.0013(2) 0.0329(16) Uani 1 1 d . . . . .
O36P O 0.6457(6) 0.4843(3) 0.0483(3) 0.0449(18) Uani 1 1 d . . . . .
Cl10 Cl 0.2600(2) 0.94675(12) 0.81916(13) 0.0541(8) Uani 1 1 d . . . . .
O37P O 0.1845(6) 0.9796(3) 0.8120(3) 0.065(2) Uani 1 1 d . . . . .
O38P O 0.3616(5) 0.9563(3) 0.8009(3) 0.0480(19) Uani 1 1 d . . . . .
O39P O 0.2128(6) 0.8893(3) 0.7975(4) 0.075(3) Uani 1 1 d . . . . .
O40P O 0.2904(7) 0.9661(4) 0.8815(3) 0.083(3) Uani 1 1 d . . . . .
Cl11 Cl 0.3626(7) 0.9745(3) 0.4141(3) 0.0396(18) Uani 0.520(11) 1 d D U P B 1
O41P O 0.3946(11) 0.9993(5) 0.3755(5) 0.064(4) Uani 0.520(11) 1 d D U P B 1
Cl12 Cl 0.3486(8) 0.9668(4) 0.4268(4) 0.056(2) Uani 0.480(11) 1 d D U P B 2
O41A O 0.3027(10) 0.9426(5) 0.4631(5) 0.065(4) Uani 0.480(11) 1 d D U P B 2
O42P O 0.3294(7) 1.0192(3) 0.4511(3) 0.078(2) Uani 1 1 d D U . . .
O43P O 0.2930(7) 0.9278(4) 0.3787(3) 0.126(4) Uani 1 1 d D U . . .
O44P O 0.4606(6) 0.9647(4) 0.4328(4) 0.095(3) Uani 1 1 d D U . . .
Cl13 Cl 1.0040(2) 0.80145(11) 0.24353(11) 0.0323(7) Uani 0.8 1 d D U P C 1
O45P O 1.0824(6) 0.8496(3) 0.2843(3) 0.057(2) Uani 0.8 1 d D U P C 1
O46P O 0.9305(8) 0.8221(4) 0.2131(3) 0.089(4) Uani 0.8 1 d D U P C 1
Cl14 Cl 1.0156(9) 0.7293(5) 0.2320(5) 0.042(2) Uani 0.2 1 d D U P C 2
O45A O 0.9353(17) 0.6802(6) 0.1956(7) 0.058(7) Uani 0.2 1 d D U P C 2
O46A O 1.0962(16) 0.7160(10) 0.2655(9) 0.061(6) Uani 0.2 1 d D U P C 2
O47P O 1.0617(5) 0.7623(2) 0.2043(2) 0.0342(14) Uani 1 1 d D U . . .
O48P O 0.9488(5) 0.7707(3) 0.2725(3) 0.0536(18) Uani 1 1 d D U . . .
O1W O 0.4610(5) 0.7247(3) 0.5249(3) 0.065(2) Uani 1 1 d . . . . .
O3W O 1.0935(5) 0.2385(3) 0.0549(3) 0.0402(17) Uani 1 1 d . . . . .
O4W O 0.4536(5) 0.2192(3) 0.0418(2) 0.0334(16) Uani 1 1 d . . . . .
O5W O 0.2731(4) 0.1985(2) 0.0925(2) 0.0246(14) Uani 1 1 d . . . . .
O6W O 0.7972(5) 0.2940(3) 0.2770(2) 0.0406(17) Uani 1 1 d . . . . .
O7W O 0.7345(6) 0.1960(4) 0.3061(4) 0.085(3) Uani 1 1 d . . . . .
O8W O 0.5874(8) 0.2611(4) 0.3629(4) 0.095(3) Uani 1 1 d . . . . .
O9W O 1.0411(8) 0.6564(4) 0.2350(4) 0.064(3) Uani 0.8 1 d . . P . .
O10W O 1.2124(9) 0.5923(4) 0.2121(5) 0.067(3) Uani 0.7 1 d . . P . .
O11W O 0.1823(10) 1.0800(5) 0.7512(6) 0.085(4) Uani 0.7 1 d . . P . .
O12W O 0.4401(13) 0.4852(6) 0.1191(5) 0.053(4) Uani 0.5 1 d . . P . .
O13W O 1.3444(12) 0.9753(7) 0.5891(7) 0.066(5) Uani 0.5 1 d . . P . .
O14W O 1.3739(17) 0.5335(10) 0.1296(7) 0.076(7) Uani 0.4 1 d . . P . .
O15W O 0.320(2) 0.5051(10) 0.2355(10) 0.068(6) Uani 0.3 1 d . . P . .
O16W O 0.296(2) 1.0068(10) 0.7064(10) 0.068(6) Uani 0.3 1 d . . P . .
O17W O 1.183(2) 0.9743(12) 0.6601(11) 0.106(8) Uani 0.4 1 d . . P . .
O18W O 1.229(2) 0.6452(10) 0.5729(16) 0.156(15) Uani 0.4 1 d . . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N15 2.037(6) . ?
Ni1 N2 2.039(6) . ?
Ni1 O4 2.050(5) . ?
Ni1 N1 2.074(7) . ?
Ni1 N16 2.085(7) . ?
Ni1 O1 2.112(5) . ?
Ni2 N6 2.076(7) . ?
Ni2 N4 2.078(6) . ?
Ni2 O1 2.084(5) . ?
Ni2 N5 2.085(7) . ?
Ni2 N3 2.089(7) . ?
Ni2 O2 2.113(5) . ?
Ni3 N7 2.047(6) . ?
Ni3 N10 2.049(6) . ?
Ni3 N8 2.053(7) . ?
Ni3 N9 2.071(6) . ?
Ni3 O3 2.096(5) . ?
Ni3 O2 2.097(5) . ?
Ni4 N11 2.049(6) . ?
Ni4 N14 2.057(6) . ?
Ni4 O4 2.062(5) . ?
Ni4 N12 2.067(6) . ?
Ni4 N13 2.076(6) . ?
Ni4 O3 2.088(5) . ?
N1 C1 1.328(10) . ?
N1 C5 1.353(11) . ?
C1 C2 1.377(12) . ?
C2 C3 1.359(13) . ?
C3 C4 1.402(12) . ?
C4 C5 1.377(12) . ?
C5 C6 1.473(12) . ?
N2 N3 1.334(9) . ?
N2 C6 1.342(10) . ?
C6 C7 1.384(12) . ?
C7 C8 1.348(13) . ?
C8 C9 1.391(12) . ?
C9 N3 1.327(10) . ?
C9 C10 1.478(12) . ?
C10 N4 1.347(11) . ?
C10 C11 1.410(12) . ?
C11 C12 1.394(13) . ?
C12 C13 1.364(13) . ?
C13 C14 1.377(12) . ?
C14 N4 1.353(10) . ?
N5 C15 1.336(10) . ?
N5 C19 1.364(11) . ?
C15 C16 1.380(12) . ?
C16 C17 1.365(13) . ?
C17 C18 1.369(13) . ?
C18 C19 1.385(11) . ?
C19 C20 1.473(12) . ?
N6 C20 1.327(10) . ?
N6 N7 1.343(9) . ?
C20 C21 1.403(12) . ?
C21 C22 1.380(12) . ?
C22 C23 1.403(11) . ?
C23 N7 1.334(10) . ?
C23 C24 1.474(11) . ?
C24 N8 1.342(10) . ?
C24 C25 1.383(12) . ?
C25 C26 1.373(12) . ?
C26 C27 1.376(12) . ?
C27 C28 1.370(12) . ?
C28 N8 1.347(10) . ?
N9 C29 1.338(10) . ?
N9 C33 1.363(10) . ?
C29 C30 1.380(11) . ?
C30 C31 1.384(12) . ?
C31 C32 1.360(12) . ?
C32 C33 1.378(11) . ?
C33 C34 1.465(11) . ?
N10 N11 1.333(9) . ?
N10 C34 1.335(10) . ?
C34 C35 1.403(11) . ?
C35 C36 1.353(11) . ?
C36 C37 1.408(11) . ?
C37 N11 1.335(10) . ?
C37 C38 1.467(11) . ?
C38 N12 1.361(10) . ?
C38 C39 1.374(11) . ?
C39 C40 1.381(12) . ?
C40 C41 1.387(12) . ?
C41 C42 1.392(11) . ?
C42 N12 1.330(10) . ?
C43 N13 1.328(10) . ?
C43 C44 1.373(12) . ?
N13 C47 1.353(10) . ?
C44 C45 1.361(13) . ?
C45 C46 1.384(13) . ?
C46 C47 1.372(12) . ?
C47 C48 1.493(12) . ?
N14 C48 1.317(10) . ?
N14 N15 1.321(9) . ?
C48 C49 1.418(11) . ?
C49 C50 1.357(12) . ?
C50 C51 1.382(12) . ?
C51 N15 1.339(10) . ?
C51 C52 1.483(12) . ?
C52 N16 1.357(11) . ?
C52 C53 1.386(12) . ?
C53 C54 1.365(13) . ?
C54 C55 1.385(13) . ?
C55 C56 1.370(13) . ?
C56 N16 1.343(11) . ?
Ni5 N31 2.044(6) . ?
Ni5 N18 2.052(6) . ?
Ni5 O8 2.061(5) . ?
Ni5 N17 2.073(6) . ?
Ni5 O5 2.077(5) . ?
Ni5 N32 2.085(7) . ?
Ni6 N22 2.058(6) . ?
Ni6 N19 2.063(6) . ?
Ni6 N21 2.071(6) . ?
Ni6 N20 2.073(6) . ?
Ni6 O5 2.074(5) . ?
Ni6 O6 2.123(5) . ?
Ni7 N24 2.051(6) . ?
Ni7 N25 2.052(6) . ?
Ni7 N23 2.052(6) . ?
Ni7 N26 2.061(6) . ?
Ni7 O7 2.103(5) . ?
Ni7 O6 2.110(5) . ?
Ni8 O8 2.055(5) . ?
Ni8 N30 2.057(6) . ?
Ni8 N27 2.066(6) . ?
Ni8 N29 2.068(6) . ?
Ni8 N28 2.073(6) . ?
Ni8 O7 2.113(5) . ?
N17 C57 1.331(10) . ?
N17 C61 1.347(10) . ?
C57 C58 1.371(12) . ?
C58 C59 1.377(12) . ?
C59 C60 1.385(12) . ?
C60 C61 1.382(11) . ?
C61 C62 1.490(11) . ?
N18 C62 1.331(10) . ?
N18 N19 1.339(8) . ?
C62 C63 1.389(11) . ?
C63 C64 1.351(11) . ?
C64 C65 1.399(11) . ?
C65 N19 1.336(10) . ?
C65 C66 1.480(11) . ?
C66 N20 1.338(10) . ?
C66 C67 1.389(11) . ?
C67 C68 1.385(12) . ?
C68 C69 1.377(12) . ?
C69 C70 1.373(11) . ?
C70 N20 1.340(10) . ?
N21 C71 1.333(10) . ?
N21 C75 1.358(10) . ?
C71 C72 1.403(11) . ?
C72 C73 1.364(12) . ?
C73 C74 1.385(12) . ?
C74 C75 1.370(10) . ?
C75 C76 1.496(11) . ?
N22 N23 1.321(8) . ?
N22 C76 1.337(9) . ?
C76 C77 1.404(11) . ?
C77 C78 1.348(11) . ?
C78 C79 1.415(10) . ?
C79 N23 1.341(10) . ?
C79 C80 1.468(11) . ?
C80 N24 1.344(9) . ?
C80 C81 1.397(11) . ?
C81 C82 1.374(11) . ?
C82 C83 1.382(11) . ?
C83 C84 1.367(12) . ?
C84 N24 1.346(10) . ?
N25 C85 1.333(10) . ?
N25 C89 1.365(9) . ?
C85 C86 1.381(11) . ?
C86 C87 1.362(11) . ?
C87 C88 1.378(11) . ?
C88 C89 1.366(11) . ?
C89 C90 1.489(11) . ?
N26 C90 1.331(9) . ?
N26 N27 1.347(8) . ?
C90 C91 1.397(10) . ?
C91 C92 1.351(11) . ?
C92 C93 1.409(11) . ?
C93 N27 1.325(9) . ?
C93 C94 1.496(11) . ?
C94 N28 1.351(10) . ?
C94 C95 1.371(11) . ?
C95 C96 1.374(12) . ?
C96 C97 1.380(12) . ?
C97 C98 1.364(11) . ?
C98 N28 1.348(10) . ?
N29 C99 1.323(10) . ?
N29 C103 1.361(10) . ?
C99 C100 1.390(12) . ?
C100 C101 1.372(13) . ?
C101 C102 1.383(13) . ?
C102 C103 1.362(11) . ?
C103 C104 1.481(11) . ?
N30 C104 1.324(10) . ?
N30 N31 1.342(9) . ?
C104 C105 1.409(11) . ?
C105 C106 1.358(11) . ?
C106 C107 1.396(11) . ?
C107 N31 1.328(10) . ?
C107 C108 1.499(11) . ?
C108 N32 1.326(10) . ?
C108 C109 1.377(11) . ?
C109 C110 1.389(12) . ?
C110 C111 1.368(12) . ?
C111 C112 1.373(11) . ?
C112 N32 1.349(10) . ?
Cl1 O4P 1.394(8) . ?
Cl1 O1P 1.415(7) . ?
Cl1 O2P 1.423(8) . ?
Cl1 O3P 1.441(6) . ?
Cl2 O5P 1.407(10) . ?
Cl2 O7P 1.410(10) . ?
Cl2 O6P 1.460(10) . ?
Cl2 O8P 1.465(10) . ?
Cl2A O7A 1.417(10) . ?
Cl2A O5A 1.429(11) . ?
Cl2A O6A 1.448(10) . ?
Cl2A O8A 1.459(10) . ?
Cl3 O9P 1.388(9) . ?
Cl3 O11P 1.392(7) . ?
Cl3 O12P 1.402(9) . ?
Cl3 O10P 1.436(6) . ?
Cl4 O13P 1.397(7) . ?
Cl4 O15P 1.415(8) . ?
Cl4 O16P 1.429(6) . ?
Cl4 O14P 1.432(6) . ?
Cl5 O19P 1.441(6) . ?
Cl5 O18P 1.443(6) . ?
Cl5 O20P 1.447(6) . ?
Cl5 O17P 1.448(6) . ?
Cl6 O24P 1.424(7) . ?
Cl6 O22P 1.433(6) . ?
Cl6 O23P 1.433(6) . ?
Cl6 O21P 1.436(6) . ?
Cl7 O27P 1.422(6) . ?
Cl7 O26P 1.423(7) . ?
Cl7 O25P 1.453(6) . ?
Cl7 O28P 1.463(7) . ?
Cl8 O31P 1.420(6) . ?
Cl8 O29P 1.422(7) . ?
Cl8 O30P 1.431(7) . ?
Cl8 O32P 1.442(6) . ?
Cl9 O34P 1.425(6) . ?
Cl9 O35P 1.433(6) . ?
Cl9 O33P 1.440(6) . ?
Cl9 O36P 1.451(7) . ?
Cl10 O39P 1.394(8) . ?
Cl10 O37P 1.395(7) . ?
Cl10 O38P 1.413(7) . ?
Cl10 O40P 1.505(7) . ?
Cl11 O43P 1.333(10) . ?
Cl11 O42P 1.339(10) . ?
Cl11 O44P 1.360(10) . ?
Cl11 O41P 1.456(11) . ?
Cl12 O43P 1.326(10) . ?
Cl12 O42P 1.327(10) . ?
Cl12 O44P 1.393(11) . ?
Cl12 O41A 1.448(12) . ?
Cl13 O46P 1.443(6) . ?
Cl13 O45P 1.448(6) . ?
Cl13 O48P 1.452(5) . ?
Cl13 O47P 1.459(5) . ?
Cl14 O47P 1.422(12) . ?
Cl14 O46A 1.433(9) . ?
Cl14 O45A 1.439(9) . ?
Cl14 O48P 1.579(13) . ?
Cl14 O9W 1.993(14) . ?
O46A O9W 1.47(3) . ?
O12W O14W 1.54(3) 1_455 ?
O14W O12W 1.54(3) 1_655 ?
O16W O17W 1.65(4) 1_455 ?
O17W O16W 1.65(4) 1_655 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N15 Ni1 N2 178.5(3) . . ?
N15 Ni1 O4 92.3(2) . . ?
N2 Ni1 O4 89.1(2) . . ?
N15 Ni1 N1 101.2(3) . . ?
N2 Ni1 N1 78.2(3) . . ?
O4 Ni1 N1 92.9(2) . . ?
N15 Ni1 N16 77.6(3) . . ?
N2 Ni1 N16 101.0(3) . . ?
O4 Ni1 N16 169.3(2) . . ?
N1 Ni1 N16 85.7(3) . . ?
N15 Ni1 O1 88.9(2) . . ?
N2 Ni1 O1 91.9(2) . . ?
O4 Ni1 O1 82.2(2) . . ?
N1 Ni1 O1 169.0(2) . . ?
N16 Ni1 O1 100.9(2) . . ?
N6 Ni2 N4 100.6(3) . . ?
N6 Ni2 O1 91.3(2) . . ?
N4 Ni2 O1 168.0(2) . . ?
N6 Ni2 N5 77.7(3) . . ?
N4 Ni2 N5 85.3(2) . . ?
O1 Ni2 N5 95.4(2) . . ?
N6 Ni2 N3 175.6(3) . . ?
N4 Ni2 N3 77.7(3) . . ?
O1 Ni2 N3 90.6(2) . . ?
N5 Ni2 N3 106.0(3) . . ?
N6 Ni2 O2 90.5(2) . . ?
N4 Ni2 O2 97.8(2) . . ?
O1 Ni2 O2 83.9(2) . . ?
N5 Ni2 O2 168.2(2) . . ?
N3 Ni2 O2 85.8(2) . . ?
N7 Ni3 N10 177.3(3) . . ?
N7 Ni3 N8 78.5(3) . . ?
N10 Ni3 N8 99.2(3) . . ?
N7 Ni3 N9 103.1(2) . . ?
N10 Ni3 N9 78.0(3) . . ?
N8 Ni3 N9 88.9(2) . . ?
N7 Ni3 O3 86.2(2) . . ?
N10 Ni3 O3 92.7(2) . . ?
N8 Ni3 O3 95.1(2) . . ?
N9 Ni3 O3 170.4(2) . . ?
N7 Ni3 O2 91.7(2) . . ?
N10 Ni3 O2 90.6(2) . . ?
N8 Ni3 O2 170.2(2) . . ?
N9 Ni3 O2 93.9(2) . . ?
O3 Ni3 O2 83.7(2) . . ?
N11 Ni4 N14 176.0(3) . . ?
N11 Ni4 O4 87.0(2) . . ?
N14 Ni4 O4 91.9(2) . . ?
N11 Ni4 N12 77.8(3) . . ?
N14 Ni4 N12 98.5(3) . . ?
O4 Ni4 N12 94.2(2) . . ?
N11 Ni4 N13 103.6(3) . . ?
N14 Ni4 N13 77.8(3) . . ?
O4 Ni4 N13 168.6(2) . . ?
N12 Ni4 N13 92.3(2) . . ?
N11 Ni4 O3 92.7(2) . . ?
N14 Ni4 O3 90.9(2) . . ?
O4 Ni4 O3 82.7(2) . . ?
N12 Ni4 O3 170.2(2) . . ?
N13 Ni4 O3 92.4(2) . . ?
Ni2 O1 Ni1 112.7(2) . . ?
Ni3 O2 Ni2 112.5(2) . . ?
Ni4 O3 Ni3 110.9(2) . . ?
Ni1 O4 Ni4 112.7(2) . . ?
C1 N1 C5 117.5(7) . . ?
C1 N1 Ni1 127.2(6) . . ?
C5 N1 Ni1 115.2(5) . . ?
N1 C1 C2 124.1(8) . . ?
C3 C2 C1 118.5(8) . . ?
C2 C3 C4 119.2(9) . . ?
C5 C4 C3 118.7(9) . . ?
N1 C5 C4 122.1(8) . . ?
N1 C5 C6 114.9(7) . . ?
C4 C5 C6 123.0(8) . . ?
N3 N2 C6 120.5(7) . . ?
N3 N2 Ni1 121.3(5) . . ?
C6 N2 Ni1 117.2(5) . . ?
N2 C6 C7 120.4(8) . . ?
N2 C6 C5 114.1(7) . . ?
C7 C6 C5 125.5(8) . . ?
C8 C7 C6 118.8(9) . . ?
C7 C8 C9 119.0(9) . . ?
N3 C9 C8 120.5(8) . . ?
N3 C9 C10 114.2(7) . . ?
C8 C9 C10 125.3(8) . . ?
C9 N3 N2 120.7(7) . . ?
C9 N3 Ni2 115.8(5) . . ?
N2 N3 Ni2 121.6(5) . . ?
N4 C10 C11 122.3(8) . . ?
N4 C10 C9 115.0(7) . . ?
C11 C10 C9 122.6(8) . . ?
C12 C11 C10 117.5(9) . . ?
C13 C12 C11 119.5(9) . . ?
C12 C13 C14 120.3(9) . . ?
N4 C14 C13 121.7(8) . . ?
C10 N4 C14 118.5(7) . . ?
C10 N4 Ni2 115.1(5) . . ?
C14 N4 Ni2 124.5(6) . . ?
C15 N5 C19 118.3(7) . . ?
C15 N5 Ni2 126.1(6) . . ?
C19 N5 Ni2 114.9(5) . . ?
N5 C15 C16 122.3(9) . . ?
C17 C16 C15 119.8(9) . . ?
C16 C17 C18 118.6(9) . . ?
C17 C18 C19 120.3(9) . . ?
N5 C19 C18 120.7(8) . . ?
N5 C19 C20 115.0(7) . . ?
C18 C19 C20 124.3(8) . . ?
C20 N6 N7 120.4(7) . . ?
C20 N6 Ni2 117.0(6) . . ?
N7 N6 Ni2 121.9(5) . . ?
N6 C20 C21 121.3(8) . . ?
N6 C20 C19 114.6(7) . . ?
C21 C20 C19 124.0(7) . . ?
C22 C21 C20 118.1(7) . . ?
C21 C22 C23 118.2(8) . . ?
N7 C23 C22 120.7(8) . . ?
N7 C23 C24 114.4(7) . . ?
C22 C23 C24 124.7(8) . . ?
C23 N7 N6 121.2(6) . . ?
C23 N7 Ni3 116.4(5) . . ?
N6 N7 Ni3 121.2(5) . . ?
N8 C24 C25 121.8(7) . . ?
N8 C24 C23 114.8(7) . . ?
C25 C24 C23 123.4(7) . . ?
C26 C25 C24 119.1(8) . . ?
C25 C26 C27 119.2(8) . . ?
C28 C27 C26 119.1(8) . . ?
N8 C28 C27 122.3(8) . . ?
C24 N8 C28 118.4(7) . . ?
C24 N8 Ni3 115.6(5) . . ?
C28 N8 Ni3 125.7(5) . . ?
C29 N9 C33 117.3(7) . . ?
C29 N9 Ni3 127.0(5) . . ?
C33 N9 Ni3 115.6(5) . . ?
N9 C29 C30 122.9(7) . . ?
C29 C30 C31 119.2(8) . . ?
C32 C31 C30 118.4(8) . . ?
C31 C32 C33 120.3(8) . . ?
N9 C33 C32 121.9(7) . . ?
N9 C33 C34 114.1(7) . . ?
C32 C33 C34 124.0(7) . . ?
N11 N10 C34 121.6(6) . . ?
N11 N10 Ni3 120.9(5) . . ?
C34 N10 Ni3 116.8(5) . . ?
N10 C34 C35 119.8(7) . . ?
N10 C34 C33 115.3(7) . . ?
C35 C34 C33 124.9(7) . . ?
C36 C35 C34 118.7(8) . . ?
C35 C36 C37 118.8(8) . . ?
N11 C37 C36 120.3(7) . . ?
N11 C37 C38 114.5(7) . . ?
C36 C37 C38 125.0(7) . . ?
N10 N11 C37 120.3(6) . . ?
N10 N11 Ni4 121.1(5) . . ?
C37 N11 Ni4 117.4(5) . . ?
N12 C38 C39 121.4(7) . . ?
N12 C38 C37 114.4(7) . . ?
C39 C38 C37 123.9(7) . . ?
C38 C39 C40 120.1(8) . . ?
C39 C40 C41 118.5(8) . . ?
C40 C41 C42 118.6(8) . . ?
N12 C42 C41 122.7(8) . . ?
C42 N12 C38 118.6(7) . . ?
C42 N12 Ni4 125.7(6) . . ?
C38 N12 Ni4 115.7(5) . . ?
N13 C43 C44 122.9(8) . . ?
C43 N13 C47 117.8(7) . . ?
C43 N13 Ni4 126.7(5) . . ?
C47 N13 Ni4 115.4(5) . . ?
C45 C44 C43 118.9(9) . . ?
C44 C45 C46 119.6(9) . . ?
C47 C46 C45 118.3(8) . . ?
N13 C47 C46 122.4(8) . . ?
N13 C47 C48 114.6(7) . . ?
C46 C47 C48 123.1(7) . . ?
C48 N14 N15 121.3(6) . . ?
C48 N14 Ni4 117.8(5) . . ?
N15 N14 Ni4 120.7(5) . . ?
N14 C48 C49 120.6(8) . . ?
N14 C48 C47 114.2(7) . . ?
C49 C48 C47 125.1(8) . . ?
C50 C49 C48 117.8(8) . . ?
C49 C50 C51 118.6(8) . . ?
N15 C51 C50 121.4(8) . . ?
N15 C51 C52 113.2(7) . . ?
C50 C51 C52 125.4(8) . . ?
N14 N15 C51 120.2(7) . . ?
N14 N15 Ni1 120.7(5) . . ?
C51 N15 Ni1 118.1(5) . . ?
N16 C52 C53 122.7(8) . . ?
N16 C52 C51 113.6(7) . . ?
C53 C52 C51 123.7(8) . . ?
C54 C53 C52 118.4(9) . . ?
C53 C54 C55 119.6(9) . . ?
C56 C55 C54 119.2(9) . . ?
N16 C56 C55 122.5(9) . . ?
C56 N16 C52 117.6(7) . . ?
C56 N16 Ni1 124.5(6) . . ?
C52 N16 Ni1 115.0(5) . . ?
N31 Ni5 N18 178.2(3) . . ?
N31 Ni5 O8 91.7(2) . . ?
N18 Ni5 O8 89.6(2) . . ?
N31 Ni5 N17 100.3(2) . . ?
N18 Ni5 N17 78.4(3) . . ?
O8 Ni5 N17 93.5(2) . . ?
N31 Ni5 O5 89.9(2) . . ?
N18 Ni5 O5 91.5(2) . . ?
O8 Ni5 O5 82.89(19) . . ?
N17 Ni5 O5 169.3(2) . . ?
N31 Ni5 N32 77.4(2) . . ?
N18 Ni5 N32 101.1(2) . . ?
O8 Ni5 N32 168.9(2) . . ?
N17 Ni5 N32 86.3(2) . . ?
O5 Ni5 N32 99.2(2) . . ?
N22 Ni6 N19 177.9(2) . . ?
N22 Ni6 N21 78.2(2) . . ?
N19 Ni6 N21 103.7(2) . . ?
N22 Ni6 N20 100.9(2) . . ?
N19 Ni6 N20 78.1(2) . . ?
N21 Ni6 N20 92.0(2) . . ?
N22 Ni6 O5 89.8(2) . . ?
N19 Ni6 O5 91.1(2) . . ?
N21 Ni6 O5 95.1(2) . . ?
N20 Ni6 O5 168.2(2) . . ?
N22 Ni6 O6 92.1(2) . . ?
N19 Ni6 O6 86.0(2) . . ?
N21 Ni6 O6 170.0(2) . . ?
N20 Ni6 O6 92.1(2) . . ?
O5 Ni6 O6 82.36(19) . . ?
N24 Ni7 N25 92.0(2) . . ?
N24 Ni7 N23 78.7(2) . . ?
N25 Ni7 N23 100.4(2) . . ?
N24 Ni7 N26 101.9(2) . . ?
N25 Ni7 N26 78.9(2) . . ?
N23 Ni7 N26 179.1(3) . . ?
N24 Ni7 O7 94.3(2) . . ?
N25 Ni7 O7 170.5(2) . . ?
N23 Ni7 O7 87.7(2) . . ?
N26 Ni7 O7 92.9(2) . . ?
N24 Ni7 O6 171.1(2) . . ?
N25 Ni7 O6 91.7(2) . . ?
N23 Ni7 O6 92.7(2) . . ?
N26 Ni7 O6 86.7(2) . . ?
O7 Ni7 O6 83.0(2) . . ?
O8 Ni8 N30 91.6(2) . . ?
O8 Ni8 N27 87.2(2) . . ?
N30 Ni8 N27 178.6(3) . . ?
O8 Ni8 N29 168.2(2) . . ?
N30 Ni8 N29 77.7(2) . . ?
N27 Ni8 N29 103.5(2) . . ?
O8 Ni8 N28 93.3(2) . . ?
N30 Ni8 N28 101.6(2) . . ?
N27 Ni8 N28 77.6(2) . . ?
N29 Ni8 N28 93.8(2) . . ?
O8 Ni8 O7 83.03(19) . . ?
N30 Ni8 O7 87.8(2) . . ?
N27 Ni8 O7 93.0(2) . . ?
N29 Ni8 O7 91.4(2) . . ?
N28 Ni8 O7 170.1(2) . . ?
Ni6 O5 Ni5 113.6(2) . . ?
Ni7 O6 Ni6 110.3(2) . . ?
Ni7 O7 Ni8 110.9(2) . . ?
Ni8 O8 Ni5 113.4(2) . . ?
C57 N17 C61 118.1(7) . . ?
C57 N17 Ni5 126.5(6) . . ?
C61 N17 Ni5 114.9(5) . . ?
N17 C57 C58 122.9(8) . . ?
C57 C58 C59 118.9(8) . . ?
C58 C59 C60 119.3(8) . . ?
C61 C60 C59 118.1(8) . . ?
N17 C61 C60 122.6(7) . . ?
N17 C61 C62 114.8(7) . . ?
C60 C61 C62 122.6(7) . . ?
C62 N18 N19 120.3(6) . . ?
C62 N18 Ni5 116.8(5) . . ?
N19 N18 Ni5 121.0(5) . . ?
N18 C62 C63 121.0(7) . . ?
N18 C62 C61 113.8(7) . . ?
C63 C62 C61 125.2(7) . . ?
C64 C63 C62 119.1(8) . . ?
C63 C64 C65 118.2(8) . . ?
N19 C65 C64 120.9(7) . . ?
N19 C65 C66 114.2(7) . . ?
C64 C65 C66 124.9(7) . . ?
C65 N19 N18 120.4(6) . . ?
C65 N19 Ni6 116.4(5) . . ?
N18 N19 Ni6 121.5(5) . . ?
N20 C66 C67 122.7(7) . . ?
N20 C66 C65 115.3(7) . . ?
C67 C66 C65 121.9(7) . . ?
C68 C67 C66 118.0(8) . . ?
C69 C68 C67 119.7(8) . . ?
C70 C69 C68 118.4(8) . . ?
N20 C70 C69 123.2(8) . . ?
C66 N20 C70 118.0(7) . . ?
C66 N20 Ni6 115.4(5) . . ?
C70 N20 Ni6 126.5(5) . . ?
C71 N21 C75 117.6(7) . . ?
C71 N21 Ni6 126.3(5) . . ?
C75 N21 Ni6 116.1(5) . . ?
N21 C71 C72 122.2(8) . . ?
C73 C72 C71 119.0(8) . . ?
C72 C73 C74 119.4(8) . . ?
C75 C74 C73 118.6(8) . . ?
N21 C75 C74 123.1(7) . . ?
N21 C75 C76 114.1(6) . . ?
C74 C75 C76 122.7(7) . . ?
N23 N22 C76 119.9(6) . . ?
N23 N22 Ni6 121.9(5) . . ?
C76 N22 Ni6 117.2(5) . . ?
N22 C76 C77 121.8(7) . . ?
N22 C76 C75 114.4(7) . . ?
C77 C76 C75 123.7(7) . . ?
C78 C77 C76 117.7(7) . . ?
C77 C78 C79 119.0(7) . . ?
N23 C79 C78 119.8(7) . . ?
N23 C79 C80 114.3(6) . . ?
C78 C79 C80 125.8(7) . . ?
N22 N23 C79 121.5(6) . . ?
N22 N23 Ni7 121.3(5) . . ?
C79 N23 Ni7 116.0(5) . . ?
N24 C80 C81 121.4(7) . . ?
N24 C80 C79 115.5(7) . . ?
C81 C80 C79 122.9(7) . . ?
C82 C81 C80 119.2(7) . . ?
C81 C82 C83 118.9(8) . . ?
C84 C83 C82 119.5(8) . . ?
N24 C84 C83 122.3(7) . . ?
C80 N24 C84 118.7(7) . . ?
C80 N24 Ni7 115.1(5) . . ?
C84 N24 Ni7 126.2(5) . . ?
C85 N25 C89 118.0(7) . . ?
C85 N25 Ni7 126.5(5) . . ?
C89 N25 Ni7 115.3(5) . . ?
N25 C85 C86 121.6(7) . . ?
C87 C86 C85 119.6(8) . . ?
C86 C87 C88 119.8(8) . . ?
C89 C88 C87 118.1(7) . . ?
N25 C89 C88 122.6(7) . . ?
N25 C89 C90 114.0(7) . . ?
C88 C89 C90 123.3(7) . . ?
C90 N26 N27 120.5(6) . . ?
C90 N26 Ni7 115.9(5) . . ?
N27 N26 Ni7 121.5(5) . . ?
N26 C90 C91 121.0(7) . . ?
N26 C90 C89 114.7(6) . . ?
C91 C90 C89 124.2(7) . . ?
C92 C91 C90 118.7(7) . . ?
C91 C92 C93 118.2(7) . . ?
N27 C93 C92 121.2(7) . . ?
N27 C93 C94 114.2(7) . . ?
C92 C93 C94 124.4(7) . . ?
C93 N27 N26 120.2(6) . . ?
C93 N27 Ni8 117.3(5) . . ?
N26 N27 Ni8 120.5(4) . . ?
N28 C94 C95 122.8(7) . . ?
N28 C94 C93 114.0(6) . . ?
C95 C94 C93 123.2(7) . . ?
C94 C95 C96 119.0(8) . . ?
C95 C96 C97 119.0(8) . . ?
C98 C97 C96 119.1(8) . . ?
N28 C98 C97 122.9(8) . . ?
C98 N28 C94 117.2(7) . . ?
C98 N28 Ni8 126.5(5) . . ?
C94 N28 Ni8 116.3(5) . . ?
C99 N29 C103 117.9(7) . . ?
C99 N29 Ni8 126.1(5) . . ?
C103 N29 Ni8 116.0(5) . . ?
N29 C99 C100 122.4(8) . . ?
C101 C100 C99 118.8(9) . . ?
C100 C101 C102 119.3(9) . . ?
C103 C102 C101 118.7(8) . . ?
N29 C103 C102 122.8(8) . . ?
N29 C103 C104 114.0(7) . . ?
C102 C103 C104 123.2(7) . . ?
C104 N30 N31 120.9(6) . . ?
C104 N30 Ni8 117.6(5) . . ?
N31 N30 Ni8 120.9(5) . . ?
N30 C104 C105 120.6(7) . . ?
N30 C104 C103 114.5(7) . . ?
C105 C104 C103 124.8(7) . . ?
C106 C105 C104 118.5(8) . . ?
C105 C106 C107 118.2(7) . . ?
N31 C107 C106 121.4(7) . . ?
N31 C107 C108 113.0(7) . . ?
C106 C107 C108 125.5(7) . . ?
C107 N31 N30 120.3(6) . . ?
C107 N31 Ni5 117.7(5) . . ?
N30 N31 Ni5 120.6(5) . . ?
N32 C108 C109 124.3(7) . . ?
N32 C108 C107 114.1(7) . . ?
C109 C108 C107 121.5(7) . . ?
C108 C109 C110 117.9(8) . . ?
C111 C110 C109 118.6(8) . . ?
C110 C111 C112 119.7(8) . . ?
N32 C112 C111 122.5(8) . . ?
C108 N32 C112 117.0(7) . . ?
C108 N32 Ni5 115.7(5) . . ?
C112 N32 Ni5 125.4(5) . . ?
O4P Cl1 O1P 110.7(6) . . ?
O4P Cl1 O2P 110.7(8) . . ?
O1P Cl1 O2P 107.7(5) . . ?
O4P Cl1 O3P 108.5(4) . . ?
O1P Cl1 O3P 110.3(4) . . ?
O2P Cl1 O3P 108.9(5) . . ?
O5P Cl2 O7P 117.3(9) . . ?
O5P Cl2 O6P 110.0(8) . . ?
O7P Cl2 O6P 105.3(7) . . ?
O5P Cl2 O8P 111.3(8) . . ?
O7P Cl2 O8P 111.9(8) . . ?
O6P Cl2 O8P 99.3(8) . . ?
O7A Cl2A O5A 111.1(10) . . ?
O7A Cl2A O6A 112.8(9) . . ?
O5A Cl2A O6A 109.7(10) . . ?
O7A Cl2A O8A 111.2(9) . . ?
O5A Cl2A O8A 109.6(10) . . ?
O6A Cl2A O8A 102.1(9) . . ?
O9P Cl3 O11P 108.9(6) . . ?
O9P Cl3 O12P 110.0(8) . . ?
O11P Cl3 O12P 108.5(6) . . ?
O9P Cl3 O10P 110.2(5) . . ?
O11P Cl3 O10P 110.6(4) . . ?
O12P Cl3 O10P 108.7(5) . . ?
O13P Cl4 O15P 109.4(7) . . ?
O13P Cl4 O16P 109.5(5) . . ?
O15P Cl4 O16P 108.8(5) . . ?
O13P Cl4 O14P 111.6(4) . . ?
O15P Cl4 O14P 106.8(4) . . ?
O16P Cl4 O14P 110.7(4) . . ?
O19P Cl5 O18P 109.3(3) . . ?
O19P Cl5 O20P 109.5(3) . . ?
O18P Cl5 O20P 109.0(4) . . ?
O19P Cl5 O17P 110.4(4) . . ?
O18P Cl5 O17P 109.2(3) . . ?
O20P Cl5 O17P 109.5(4) . . ?
O24P Cl6 O22P 110.2(5) . . ?
O24P Cl6 O23P 108.8(4) . . ?
O22P Cl6 O23P 110.1(4) . . ?
O24P Cl6 O21P 109.3(4) . . ?
O22P Cl6 O21P 108.2(4) . . ?
O23P Cl6 O21P 110.3(4) . . ?
O27P Cl7 O26P 110.7(4) . . ?
O27P Cl7 O25P 108.5(4) . . ?
O26P Cl7 O25P 109.8(4) . . ?
O27P Cl7 O28P 107.7(4) . . ?
O26P Cl7 O28P 109.2(5) . . ?
O25P Cl7 O28P 110.9(4) . . ?
O31P Cl8 O29P 108.8(5) . . ?
O31P Cl8 O30P 108.0(5) . . ?
O29P Cl8 O30P 109.6(5) . . ?
O31P Cl8 O32P 110.2(3) . . ?
O29P Cl8 O32P 110.0(4) . . ?
O30P Cl8 O32P 110.2(4) . . ?
O34P Cl9 O35P 110.5(4) . . ?
O34P Cl9 O33P 109.1(4) . . ?
O35P Cl9 O33P 108.6(4) . . ?
O34P Cl9 O36P 108.4(4) . . ?
O35P Cl9 O36P 110.7(4) . . ?
O33P Cl9 O36P 109.7(5) . . ?
O39P Cl10 O37P 111.8(5) . . ?
O39P Cl10 O38P 112.3(5) . . ?
O37P Cl10 O38P 115.0(5) . . ?
O39P Cl10 O40P 107.1(6) . . ?
O37P Cl10 O40P 105.5(5) . . ?
O38P Cl10 O40P 104.2(5) . . ?
O43P Cl11 O42P 123.1(9) . . ?
O43P Cl11 O44P 114.1(8) . . ?
O42P Cl11 O44P 113.9(7) . . ?
O43P Cl11 O41P 100.0(7) . . ?
O42P Cl11 O41P 98.4(7) . . ?
O44P Cl11 O41P 101.6(8) . . ?
O43P Cl12 O42P 124.6(9) . . ?
O43P Cl12 O44P 112.4(8) . . ?
O42P Cl12 O44P 112.6(8) . . ?
O43P Cl12 O41A 97.4(8) . . ?
O42P Cl12 O41A 99.7(8) . . ?
O44P Cl12 O41A 105.8(9) . . ?
O46P Cl13 O45P 108.2(6) . . ?
O46P Cl13 O48P 114.0(5) . . ?
O45P Cl13 O48P 108.7(4) . . ?
O46P Cl13 O47P 109.1(4) . . ?
O45P Cl13 O47P 110.1(4) . . ?
O48P Cl13 O47P 106.8(4) . . ?
O47P Cl14 O46A 113.7(10) . . ?
O47P Cl14 O45A 113.6(10) . . ?
O46A Cl14 O45A 112.5(11) . . ?
O47P Cl14 O48P 102.1(7) . . ?
O46A Cl14 O48P 108.2(10) . . ?
O45A Cl14 O48P 105.7(10) . . ?
O47P Cl14 O9W 133.2(8) . . ?
O46A Cl14 O9W 47.4(11) . . ?
O45A Cl14 O9W 65.1(11) . . ?
O48P Cl14 O9W 123.8(7) . . ?
Cl14 O46A O9W 86.7(12) . . ?
O46A O9W Cl14 45.9(5) . . ?

_refine_diff_density_max         1.560
_refine_diff_density_min         -1.341
_refine_diff_density_rms         0.120

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_NINO3DPnew
_database_code_depnum_ccdc_archive 'CCDC 1874222'
_audit_update_record             
;
2018-12-20 deposited with the CCDC.
2019-01-04 downloaded from the CCDC.
;

_vrf_THETM01_NINO3DPnew          
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Crystals of compound 2 were difficult to handle out of the 
mother solution because of the rapid loss of lattice solvent molecules. 
To slow down the degradation process, the crystals were collected at 
low T in Paratone oil. However, a partial solvent loss (and crystal 
degradation) occurred anyway, so the collected crystal(s) diffracted 
poorly. 
;
_vrf_PLAT214_NINO3DPnew          
;
PROBLEM: Atom O8        (Anion/Solvent) ADP max/min Ratio        7.9 oblate
RESPONSE: Atom O8 belongs to a disordered nitrate counterion. The nitrate 
anions and the lattice solvent (water) molecules in this crystal structure
are severely disordered. Although the one provided here is our best model, 
we acknowledge it has some problems, probably due to the poor quality 
of the collected data.
;
_vrf_PLAT216_NINO3DPnew          
;
PROBLEM: Disordered O11W      (An/Solv) ADP max/min Ratio       14.0 Note  
RESPONSE: Atoms O11w and O12w identify possible sites with half occupancy 
each for a disordered lattice water molecule.
;
_vrf_PLAT430_NINO3DPnew          
;
PROBLEM: Short Inter D...A Contact  O1W      ..O16      .       2.18 Ang.  
RESPONSE: All such alert messages involve disordered anions/solvent atoms, 
for which we attempted to identify/model their positions/occupancies.
;
_vrf_PLAT043_NINO3DPnew          
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      34.35 Check 
RESPONSE: The hydrogen atoms of the coordinated water (2 H2O) and hydroxo 
groups (2 OH-) as well as those of the crystallization solvent molecules 
(declared 14 H2O per tetramer) were neither found nor calculated, but they 
were obviously included in the UNIT instruction.
;
_vrf_PLAT097_NINO3DPnew          
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       3.00 eA-3  
RESPONSE: The two largest residual density peaks (Q1= 3.00 eA-3; 
Q2= 2.64 eA-3) could not be modelled because they are pretty close to one 
coordinated dppn ligand. 
;
_vrf_PLAT250_NINO3DPnew          
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        4.7 Note  
RESPONSE: We are aware the proposed model is not very satisfying, probably 
due to the poor quality of the collected data. 
;
_vrf_PLAT260_NINO3DPnew          
;
PROBLEM: Large Average Ueq of Residue Including      O16A      0.155 Check 
RESPONSE:  The nitrate anions and the lattice solvent (water) molecules in 
this crystal structure are severely disordered.
;
_vrf_PLAT306_NINO3DPnew          
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O1W Check 
RESPONSE: The hydrogen atoms of the coordinated water (2 H2O) and hydroxo 
groups (2 OH-) as well as those of the crystallization solvent molecules 
(declared 14 H2O per tetramer) were neither found nor calculated.
;
_vrf_PLAT341_NINO3DPnew          
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01671 Ang.  
RESPONSE: The collected data were of poor quality.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C56 H46 N16 Ni4 O4, 6(N O3), 14(H2 O)'
_chemical_formula_sum            'C56 H74 N22 Ni4 O36'
_chemical_formula_weight         1866.21

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                   14.5870(10)
_cell_length_b                   14.7541(9)
_cell_length_c                   18.4452(12)
_cell_angle_alpha                95.571(3)
_cell_angle_beta                 97.055(3)
_cell_angle_gamma                90.120(3)
_cell_volume                     3920.7(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9928
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      22.41

_exptl_crystal_description       LAMINAR
_exptl_crystal_colour            AMBER-YELLOW
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_F_000             1928
_exptl_transmission_factor_min   0.6627
_exptl_transmission_factor_max   0.7448
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    1.049
_shelx_estimated_absorpt_T_min   0.758
_shelx_estimated_absorpt_T_max   0.969
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   
'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker X8 Apex-II CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            59861
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.118
_diffrn_reflns_theta_max         22.459
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.711
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.711
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.711
_reflns_number_total             10097
_reflns_number_gt                8593
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013, version 2013-4 (Sheldrick 2013)'
_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)+(0.1671P)²+68.7639P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     Patt
_atom_sites_solution_secondary   Difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10097
_refine_ls_number_parameters     1162
_refine_ls_number_restraints     1515
_refine_ls_R_factor_all          0.1257
_refine_ls_R_factor_gt           0.1095
_refine_ls_wR_factor_ref         0.3103
_refine_ls_wR_factor_gt          0.2901
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.049
_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 0.82834(9) 0.90802(8) 0.21198(6) 0.0234(4) Uani 1 1 d . . . . .
Ni2 Ni 0.65707(9) 0.74724(9) 0.21421(7) 0.0288(4) Uani 1 1 d . . . . .
Ni3 Ni 0.82352(10) 0.58805(8) 0.25497(7) 0.0308(4) Uani 1 1 d . . . . .
Ni4 Ni 0.99422(9) 0.74764(8) 0.24826(6) 0.0233(4) Uani 1 1 d . . . . .
O4 O 0.8875(5) 0.7869(4) 0.1744(3) 0.0246(15) Uani 1 1 d . . . . .
O3 O 0.8864(5) 0.7099(4) 0.3031(3) 0.0282(16) Uani 1 1 d . . . . .
O2 O 0.7656(5) 0.6707(4) 0.1776(3) 0.0282(16) Uani 1 1 d . . . . .
O1 O 0.7654(5) 0.8228(4) 0.2752(4) 0.0285(16) Uani 1 1 d . . . . .
N1 N 0.8742(6) 0.9831(5) 0.1332(4) 0.0251(16) Uani 1 1 d . U . . .
N2 N 0.7241(6) 0.8862(6) 0.1261(4) 0.0268(17) Uani 1 1 d . U . . .
N3 N 0.6585(6) 0.8218(6) 0.1267(4) 0.0262(17) Uani 1 1 d . U . . .
N4 N 0.5585(6) 0.6787(6) 0.1383(5) 0.0301(18) Uani 1 1 d . U . . .
C1 C 0.9501(8) 1.0341(7) 0.1421(6) 0.035(2) Uani 1 1 d . U . . .
H1A H 0.9908 1.0337 0.1864 0.042 Uiso 1 1 calc R U . . .
C2 C 0.9728(9) 1.0891(8) 0.0883(6) 0.047(3) Uani 1 1 d . U . . .
H2A H 1.0280 1.1248 0.0957 0.056 Uiso 1 1 calc R U . . .
C3 C 0.9120(8) 1.0895(8) 0.0243(6) 0.042(3) Uani 1 1 d . U . . .
H3A H 0.9249 1.1260 -0.0130 0.050 Uiso 1 1 calc R U . . .
C4 C 0.8323(8) 1.0363(7) 0.0151(6) 0.034(2) Uani 1 1 d . U . . .
H4A H 0.7901 1.0357 -0.0285 0.041 Uiso 1 1 calc R U . . .
C5 C 0.8150(8) 0.9834(7) 0.0709(5) 0.028(2) Uani 1 1 d . U . . .
C6 C 0.7369(7) 0.9197(7) 0.0634(5) 0.029(2) Uani 1 1 d . U . . .
C7 C 0.6806(8) 0.8926(8) -0.0022(6) 0.033(2) Uani 1 1 d . U . . .
H7A H 0.6870 0.9204 -0.0457 0.040 Uiso 1 1 calc R U . . .
C8 C 0.6166(8) 0.8259(8) -0.0022(6) 0.034(2) Uani 1 1 d . U . . .
H8A H 0.5793 0.8037 -0.0462 0.041 Uiso 1 1 calc R U . . .
C9 C 0.6066(7) 0.7905(7) 0.0641(5) 0.029(2) Uani 1 1 d . U . . .
C10 C 0.5446(7) 0.7125(7) 0.0713(5) 0.030(2) Uani 1 1 d . U . . .
C11 C 0.4812(7) 0.6753(8) 0.0148(6) 0.034(2) Uani 1 1 d . U . . .
H11A H 0.4719 0.7010 -0.0308 0.041 Uiso 1 1 calc R U . . .
C12 C 0.4312(8) 0.5988(8) 0.0266(7) 0.041(2) Uani 1 1 d . U . . .
H12A H 0.3876 0.5705 -0.0114 0.049 Uiso 1 1 calc R U . . .
C13 C 0.4455(8) 0.5648(8) 0.0934(6) 0.039(2) Uani 1 1 d . U . . .
H13A H 0.4117 0.5128 0.1025 0.047 Uiso 1 1 calc R U . . .
C14 C 0.5095(8) 0.6067(8) 0.1474(6) 0.037(2) Uani 1 1 d . U . . .
H14A H 0.5188 0.5823 0.1935 0.044 Uiso 1 1 calc R U . . .
N5 N 0.5562(6) 0.8132(7) 0.2665(5) 0.0373(19) Uani 1 1 d . U . . .
N6 N 0.6527(6) 0.6738(6) 0.3024(5) 0.0336(17) Uani 1 1 d . U . . .
N7 N 0.7182(7) 0.6104(6) 0.3174(5) 0.0360(18) Uani 1 1 d . U . . .
N8 N 0.8656(8) 0.5153(6) 0.3439(5) 0.0394(19) Uani 1 1 d . U . . .
C15 C 0.5070(8) 0.8850(9) 0.2451(6) 0.043(2) Uani 1 1 d . U . . .
H15A H 0.5200 0.9094 0.2016 0.051 Uiso 1 1 calc R U . . .
C16 C 0.4405(9) 0.9249(11) 0.2815(7) 0.056(3) Uani 1 1 d . U . . .
H16A H 0.4077 0.9762 0.2652 0.067 Uiso 1 1 calc R U . . .
C17 C 0.4224(9) 0.8855(12) 0.3456(8) 0.061(3) Uani 1 1 d . U . . .
H17A H 0.3756 0.9104 0.3728 0.073 Uiso 1 1 calc R U . . .
C18 C 0.4703(9) 0.8133(11) 0.3688(7) 0.059(3) Uani 1 1 d . U . . .
H18A H 0.4579 0.7879 0.4120 0.071 Uiso 1 1 calc R U . . .
C19 C 0.5367(8) 0.7776(9) 0.3289(6) 0.042(2) Uani 1 1 d . U . . .
C20 C 0.5963(9) 0.7023(8) 0.3498(6) 0.039(2) Uani 1 1 d . U . . .
C21 C 0.5992(9) 0.6618(9) 0.4171(6) 0.047(2) Uani 1 1 d . U . . .
H21A H 0.5560 0.6789 0.4504 0.056 Uiso 1 1 calc R U . . .
C22 C 0.6647(9) 0.5981(8) 0.4334(6) 0.046(2) Uani 1 1 d . U . . .
H22A H 0.6685 0.5710 0.4783 0.056 Uiso 1 1 calc R U . . .
C23 C 0.7260(9) 0.5739(7) 0.3823(6) 0.0399(19) Uani 1 1 d . U . . .
C24 C 0.8055(10) 0.5145(8) 0.3938(6) 0.043(2) Uani 1 1 d . U . . .
C25 C 0.8204(12) 0.4624(9) 0.4532(7) 0.058(3) Uani 1 1 d . U . . .
H25A H 0.7766 0.4615 0.4872 0.069 Uiso 1 1 calc R U . . .
C26 C 0.8991(12) 0.4127(10) 0.4615(7) 0.068(3) Uani 1 1 d . U . . .
H26A H 0.9102 0.3767 0.5016 0.082 Uiso 1 1 calc R U . . .
C27 C 0.9631(13) 0.4141(10) 0.4120(8) 0.067(3) Uani 1 1 d . U . . .
H27A H 1.0189 0.3810 0.4178 0.081 Uiso 1 1 calc R U . . .
C28 C 0.9416(11) 0.4672(8) 0.3523(6) 0.050(2) Uani 1 1 d . U . . .
H28A H 0.9836 0.4682 0.3169 0.060 Uiso 1 1 calc R U . . .
N9 N 0.7805(7) 0.4657(6) 0.1936(5) 0.0393(19) Uani 1 1 d . U . . .
N10 N 0.9296(7) 0.5602(5) 0.1936(4) 0.0321(17) Uani 1 1 d . U . . .
N11 N 0.9956(6) 0.6214(5) 0.1920(4) 0.0299(17) Uani 1 1 d . U . . .
N12 N 1.0992(6) 0.7638(6) 0.1831(4) 0.0284(16) Uani 1 1 d . U . . .
C29 C 0.7012(10) 0.4207(8) 0.1985(6) 0.048(2) Uani 1 1 d . U . . .
H29 H 0.6578 0.4485 0.2278 0.058 Uiso 1 1 calc R U . . .
C30 C 0.6813(11) 0.3343(8) 0.1616(8) 0.059(3) Uani 1 1 d . U . . .
H30 H 0.6258 0.3028 0.1663 0.071 Uiso 1 1 calc R U . . .
C31 C 0.7434(11) 0.2965(9) 0.1190(8) 0.065(3) Uani 1 1 d . U . . .
H31 H 0.7311 0.2381 0.0931 0.078 Uiso 1 1 calc R U . . .
C32 C 0.8256(11) 0.3429(8) 0.1130(8) 0.058(3) Uani 1 1 d . U . . .
H32 H 0.8697 0.3168 0.0836 0.070 Uiso 1 1 calc R U . . .
C33 C 0.8400(10) 0.4268(7) 0.1508(6) 0.043(2) Uani 1 1 d . U . . .
C34 C 0.9243(9) 0.4843(7) 0.1487(6) 0.038(2) Uani 1 1 d . U . . .
C35 C 0.9892(9) 0.4642(8) 0.1006(6) 0.042(2) Uani 1 1 d . U . . .
H35 H 0.9855 0.4090 0.0692 0.050 Uiso 1 1 calc R U . . .
C36 C 1.0596(9) 0.5274(7) 0.0998(6) 0.041(2) Uani 1 1 d . U . . .
H36 H 1.1071 0.5159 0.0693 0.049 Uiso 1 1 calc R U . . .
C37 C 1.0582(8) 0.6079(7) 0.1450(5) 0.0332(19) Uani 1 1 d . U . . .
C38 C 1.1224(8) 0.6869(7) 0.1447(5) 0.0333(19) Uani 1 1 d . U . . .
C39 C 1.1991(8) 0.6802(8) 0.1071(6) 0.040(2) Uani 1 1 d . U . . .
H39 H 1.2140 0.6243 0.0814 0.048 Uiso 1 1 calc R U . . .
C40 C 1.2536(9) 0.7579(9) 0.1083(6) 0.046(2) Uani 1 1 d . U . . .
H40 H 1.3070 0.7562 0.0835 0.055 Uiso 1 1 calc R U . . .
C41 C 1.2284(8) 0.8386(8) 0.1467(6) 0.037(2) Uani 1 1 d . U . . .
H41 H 1.2635 0.8930 0.1474 0.044 Uiso 1 1 calc R U . . .
C42 C 1.1514(8) 0.8376(7) 0.1837(5) 0.032(2) Uani 1 1 d . U . . .
H42 H 1.1353 0.8922 0.2106 0.039 Uiso 1 1 calc R U . . .
N13 N 1.1003(6) 0.7299(5) 0.3329(4) 0.0272(17) Uani 1 1 d . U . . .
N14 N 1.0011(6) 0.8726(5) 0.3062(4) 0.0236(15) Uani 1 1 d . U . . .
N15 N 0.9349(6) 0.9336(5) 0.2944(4) 0.0237(15) Uani 1 1 d . U . . .
N16 N 0.7863(6) 1.0264(6) 0.2690(4) 0.0293(17) Uani 1 1 d . U . . .
C43 C 1.1499(8) 0.6556(7) 0.3398(6) 0.035(2) Uani 1 1 d . U . . .
H43 H 1.1309 0.6016 0.3094 0.042 Uiso 1 1 calc R U . . .
C44 C 1.2284(9) 0.6539(8) 0.3898(6) 0.040(2) Uani 1 1 d . U . . .
H44 H 1.2624 0.5994 0.3942 0.048 Uiso 1 1 calc R U . . .
C45 C 1.2568(8) 0.7339(8) 0.4339(6) 0.038(2) Uani 1 1 d . U . . .
H45 H 1.3111 0.7351 0.4682 0.046 Uiso 1 1 calc R U . . .
C46 C 1.2045(8) 0.8114(8) 0.4266(5) 0.033(2) Uani 1 1 d . U . . .
H46 H 1.2222 0.8667 0.4558 0.040 Uiso 1 1 calc R U . . .
C47 C 1.1266(7) 0.8068(7) 0.3764(5) 0.0272(18) Uani 1 1 d . U . . .
C48 C 1.0656(7) 0.8864(7) 0.3657(5) 0.0275(18) Uani 1 1 d . U . . .
C49 C 1.0668(8) 0.9668(7) 0.4130(5) 0.0294(19) Uani 1 1 d . U . . .
H49 H 1.1141 0.9782 0.4531 0.035 Uiso 1 1 calc R U . . .
C50 C 1.0001(7) 1.0270(7) 0.4007(5) 0.0288(19) Uani 1 1 d . U . . .
H50 H 0.9989 1.0819 0.4321 0.035 Uiso 1 1 calc R U . . .
C51 C 0.9315(7) 1.0082(7) 0.3405(5) 0.0265(17) Uani 1 1 d . U . . .
C52 C 0.8470(7) 1.0642(7) 0.3248(5) 0.0279(17) Uani 1 1 d . U . . .
C53 C 0.8309(9) 1.1442(8) 0.3663(6) 0.041(2) Uani 1 1 d . U . . .
H53 H 0.8758 1.1691 0.4048 0.049 Uiso 1 1 calc R U . . .
C54 C 0.7476(9) 1.1871(8) 0.3501(7) 0.047(3) Uani 1 1 d . U . . .
H54 H 0.7337 1.2415 0.3784 0.057 Uiso 1 1 calc R U . . .
C55 C 0.6850(9) 1.1501(8) 0.2925(7) 0.048(3) Uani 1 1 d . U . . .
H55 H 0.6279 1.1792 0.2802 0.057 Uiso 1 1 calc R U . . .
C56 C 0.7068(9) 1.0697(8) 0.2529(7) 0.042(2) Uani 1 1 d . U . . .
H56 H 0.6639 1.0445 0.2131 0.051 Uiso 1 1 calc R U . . .
N17 N 0.75324(7) 0.57159(6) 0.00051(17) 0.063(3) Uani 1 1 d D U . . .
O1N O 0.8386(8) 0.5810(2) 0.0308(5) 0.091(3) Uani 0.716(12) 1 d D U P A 1
O2N O 0.7014(8) 0.58733(18) 0.0471(4) 0.074(3) Uani 0.716(12) 1 d D U P A 1
O3N O 0.7378(9) 0.55004(17) -0.0650(4) 0.082(3) Uani 0.716(12) 1 d D U P A 1
O1A O 0.7794(2) 0.5137(5) 0.0410(9) 0.091(3) Uani 0.284(12) 1 d D U P A 2
O2A O 0.72613(19) 0.6501(4) 0.0163(11) 0.074(3) Uani 0.284(12) 1 d D U P A 2
O3A O 0.7556(2) 0.5438(6) -0.0661(7) 0.082(3) Uani 0.284(12) 1 d D U P A 2
N18 N 0.92448(10) 0.74662(9) -0.01288(14) 0.040(2) Uani 1 1 d D U . . .
O4N O 0.9877(3) 0.7030(3) 0.0137(4) 0.151(8) Uani 1 1 d D U . . .
O5N O 0.8906(3) 0.8051(2) 0.0273(3) 0.053(2) Uani 1 1 d D U . . .
O6N O 0.8972(3) 0.7299(3) -0.0792(3) 0.0439(19) Uani 1 1 d D U . . .
N19 N 0.74948(19) 0.93450(5) 0.43920(7) 0.061(3) Uani 1 1 d D U . . .
O7 O 0.6892(4) 0.91155(15) 0.3890(2) 0.067(3) Uani 1 1 d D U . . .
O8 O 0.8298(5) 0.9052(2) 0.4416(2) 0.036(4) Uani 0.53(2) 1 d D U P B 1
O9 O 0.7255(6) 0.9908(2) 0.4897(3) 0.047(4) Uani 0.53(2) 1 d D U P B 1
O8A O 0.8295(8) 0.9302(2) 0.4210(5) 0.056(6) Uani 0.47(2) 1 d D U P B 2
O9A O 0.7345(14) 0.96011(18) 0.5031(4) 0.106(9) Uani 0.47(2) 1 d D U P B 2
N20 N 0.92843(9) 0.74834(5) 0.49691(12) 0.0339(19) Uani 1 1 d D U . . .
O10 O 0.9990(3) 0.7890(2) 0.4887(3) 0.037(2) Uani 0.801(12) 1 d D U P C 1
O11 O 0.8943(3) 0.7666(2) 0.5578(3) 0.036(2) Uani 0.801(12) 1 d D U P C 1
O12 O 0.8923(3) 0.6919(2) 0.4476(3) 0.060(3) Uani 0.801(12) 1 d D U P C 1
O10A O 0.9834(4) 0.7829(2) 0.4594(10) 0.037(2) Uani 0.199(12) 1 d D U P C 2
O11A O 0.9409(3) 0.7510(2) 0.5640(7) 0.036(2) Uani 0.199(12) 1 d D U P C 2
O12A O 0.8591(4) 0.7106(2) 0.4593(12) 0.060(3) Uani 0.199(12) 1 d D U P C 2
N21 N 0.52713(12) 1.0795(3) 0.12298(7) 0.068(3) Uani 1 1 d D U . D 2
O13 O 0.4623(3) 1.0694(8) 0.1576(2) 0.151(6) Uani 1 1 d D U . D 2
O14 O 0.5609(3) 1.1551(6) 0.1191(2) 0.148(6) Uani 1 1 d D U . D 2
O15 O 0.5566(3) 1.0115(5) 0.0925(2) 0.070(3) Uani 1 1 d D U . D 2
N22 N 0.21679(8) 1.08526(12) 0.2193(2) 0.114(11) Uani 0.388(12) 1 d D U P E 1
O16 O 0.2590(2) 1.1579(3) 0.2450(6) 0.137(13) Uani 0.388(12) 1 d D U P E 1
O17 O 0.1731(2) 1.0432(3) 0.2600(5) 0.106(14) Uani 0.388(12) 1 d D U P E 1
O18 O 0.2196(2) 1.0570(3) 0.1538(5) 0.124(12) Uani 0.388(12) 1 d D U P E 1
O15W O 0.5766(13) 0.4671(13) 0.5403(11) 0.038(5) Uiso 0.388(12) 1 d . . P E 1
O16W O 0.612(2) 0.3643(16) 0.4144(14) 0.061(8) Uani 0.388(12) 1 d . . P E 1
N22A N 0.56339(7) 0.3253(2) 0.4217(4) 0.157(10) Uani 0.612(12) 1 d D U P E 2
O16A O 0.5794(2) 0.3971(5) 0.4643(8) 0.186(12) Uani 0.612(12) 1 d D U P E 2
O17A O 0.5740(2) 0.3269(6) 0.3554(6) 0.188(12) Uani 0.612(12) 1 d D U P E 2
O18A O 0.5372(2) 0.2534(5) 0.4460(6) 0.090(6) Uani 0.612(12) 1 d D U P E 2
O17W O 0.1415(13) 1.0542(10) 0.2547(8) 0.042(4) Uani 0.612(12) 1 d . . P E 2
O18W O 0.2199(8) 1.1344(9) 0.1454(6) 0.035(3) Uani 0.612(12) 1 d . . P E 2
O1W O 0.6196(9) 0.7765(13) -0.2135(7) 0.122(6) Uani 1 1 d . . . . .
O2W O 0.9697(7) 0.8176(6) -0.2959(5) 0.058(3) Uani 1 1 d . . . . .
O3W O 0.6121(7) 1.1058(7) -0.0409(7) 0.075(3) Uani 1 1 d . . . . .
O4W O 0.9682(9) 0.6784(7) -0.2113(5) 0.079(4) Uani 1 1 d . . . . .
O5W O 0.7652(10) 0.6406(10) 0.5922(5) 0.106(5) Uani 1 1 d . . . . .
O6W O 0.2832(10) 1.0588(11) 0.3657(7) 0.106(5) Uani 1 1 d . . . . .
O7W O 1.1507(16) 0.4407(8) 0.2894(7) 0.148(8) Uani 1 1 d . . . . .
O8W O 0.2609(13) 0.5128(16) 0.2194(12) 0.167(8) Uani 1 1 d . . . . .
O9W O 0.6344(11) 0.7675(14) -0.3638(7) 0.139(7) Uani 1 1 d . . . . .
O10W O 0.5575(17) 1.0599(14) 0.4711(9) 0.179(10) Uani 1 1 d . . . . .
O11W O 0.565(3) 0.470(4) 0.6886(16) 0.26(3) Uani 0.5 1 d . . P . .
O12W O 0.473(2) 0.5415(17) 0.7069(14) 0.101(9) Uani 0.5 1 d . . P . .
O13W O 0.560(3) 0.654(3) -0.163(2) 0.144(12) Uiso 0.5 1 d . . P . .
O14W O 0.720(4) 0.691(3) -0.155(3) 0.196(19) Uiso 0.5 1 d . . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N15 2.044(8) . ?
Ni1 N2 2.057(8) . ?
Ni1 O1 2.081(6) . ?
Ni1 O4 2.082(7) . ?
Ni1 N1 2.082(8) . ?
Ni1 N16 2.083(9) . ?
Ni1 Ni4 3.4402(18) . ?
Ni1 Ni2 3.4481(17) . ?
Ni2 N3 2.041(8) . ?
Ni2 N6 2.047(8) . ?
Ni2 N5 2.053(10) . ?
Ni2 N4 2.067(8) . ?
Ni2 O1 2.078(7) . ?
Ni2 O2 2.089(7) . ?
Ni2 Ni3 3.449(2) . ?
Ni3 N7 2.039(10) . ?
Ni3 N10 2.046(10) . ?
Ni3 O2 2.070(7) . ?
Ni3 N8 2.077(9) . ?
Ni3 O3 2.085(7) . ?
Ni3 N9 2.088(9) . ?
Ni3 Ni4 3.4449(17) . ?
Ni4 N14 2.035(8) . ?
Ni4 N11 2.044(8) . ?
Ni4 O4 2.062(7) . ?
Ni4 O3 2.075(7) . ?
Ni4 N12 2.086(9) . ?
Ni4 N13 2.095(8) . ?
O4 O2 2.477(9) . ?
O3 O1 2.471(10) . ?
N1 C1 1.322(14) . ?
N1 C5 1.349(13) . ?
N2 C6 1.336(13) . ?
N2 N3 1.348(12) . ?
N3 C9 1.342(13) . ?
N4 C14 1.315(14) . ?
N4 C10 1.370(14) . ?
C1 C2 1.410(16) . ?
C1 H1A 0.9500 . ?
C2 C3 1.388(17) . ?
C2 H2A 0.9500 . ?
C3 C4 1.384(16) . ?
C3 H3A 0.9500 . ?
C4 C5 1.398(14) . ?
C4 H4A 0.9500 . ?
C5 C6 1.460(15) . ?
C6 C7 1.399(15) . ?
C7 C8 1.355(15) . ?
C7 H7A 0.9500 . ?
C8 C9 1.398(15) . ?
C8 H8A 0.9500 . ?
C9 C10 1.489(15) . ?
C10 C11 1.375(15) . ?
C11 C12 1.391(16) . ?
C11 H11A 0.9500 . ?
C12 C13 1.368(17) . ?
C12 H12A 0.9500 . ?
C13 C14 1.376(16) . ?
C13 H13A 0.9500 . ?
C14 H14A 0.9500 . ?
N5 C15 1.345(16) . ?
N5 C19 1.369(14) . ?
N6 C20 1.315(15) . ?
N6 N7 1.361(14) . ?
N7 C23 1.352(14) . ?
N8 C28 1.318(17) . ?
N8 C24 1.347(16) . ?
C15 C16 1.350(18) . ?
C15 H15A 0.9500 . ?
C16 C17 1.42(2) . ?
C16 H16A 0.9500 . ?
C17 C18 1.35(2) . ?
C17 H17A 0.9500 . ?
C18 C19 1.364(18) . ?
C18 H18A 0.9500 . ?
C19 C20 1.464(18) . ?
C20 C21 1.425(16) . ?
C21 C22 1.369(19) . ?
C21 H21A 0.9500 . ?
C22 C23 1.398(18) . ?
C22 H22A 0.9500 . ?
C23 C24 1.462(19) . ?
C24 C25 1.396(16) . ?
C25 C26 1.36(2) . ?
C25 H25A 0.9500 . ?
C26 C27 1.38(2) . ?
C26 H26A 0.9500 . ?
C27 C28 1.417(18) . ?
C27 H27A 0.9500 . ?
C28 H28A 0.9500 . ?
N9 C33 1.337(17) . ?
N9 C29 1.350(16) . ?
N10 N11 1.323(13) . ?
N10 C34 1.323(14) . ?
N11 C37 1.336(14) . ?
N12 C42 1.327(14) . ?
N12 C38 1.345(14) . ?
C29 C30 1.398(17) . ?
C29 H29 0.9500 . ?
C30 C31 1.36(2) . ?
C30 H30 0.9500 . ?
C31 C32 1.40(2) . ?
C31 H31 0.9500 . ?
C32 C33 1.364(17) . ?
C32 H32 0.9500 . ?
C33 C34 1.498(18) . ?
C34 C35 1.389(18) . ?
C35 C36 1.388(18) . ?
C35 H35 0.9500 . ?
C36 C37 1.385(15) . ?
C36 H36 0.9500 . ?
C37 C38 1.494(16) . ?
C38 C39 1.385(17) . ?
C39 C40 1.390(18) . ?
C39 H39 0.9500 . ?
C40 C41 1.398(17) . ?
C40 H40 0.9500 . ?
C41 C42 1.384(16) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
N13 C43 1.322(14) . ?
N13 C47 1.351(13) . ?
N14 N15 1.335(12) . ?
N14 C48 1.354(13) . ?
N15 C51 1.328(13) . ?
N16 C56 1.339(15) . ?
N16 C52 1.348(14) . ?
C43 C44 1.381(17) . ?
C43 H43 0.9500 . ?
C44 C45 1.398(17) . ?
C44 H44 0.9500 . ?
C45 C46 1.385(16) . ?
C45 H45 0.9500 . ?
C46 C47 1.372(15) . ?
C46 H46 0.9500 . ?
C47 C48 1.488(15) . ?
C48 C49 1.402(14) . ?
C49 C50 1.333(16) . ?
C49 H49 0.9500 . ?
C50 C51 1.406(15) . ?
C50 H50 0.9500 . ?
C51 C52 1.500(15) . ?
C52 C53 1.379(15) . ?
C53 C54 1.385(18) . ?
C53 H53 0.9500 . ?
C54 C55 1.382(18) . ?
C54 H54 0.9500 . ?
C55 C56 1.391(17) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
N17 O3N 1.212(7) . ?
N17 O2N 1.219(9) . ?
N17 O1A 1.219(10) . ?
N17 O2A 1.244(7) . ?
N17 O3A 1.262(12) . ?
N17 O1N 1.302(10) . ?
N18 O4N 1.207(5) . ?
N18 O5N 1.226(5) . ?
N18 O6N 1.240(5) . ?
N19 O7 1.218(5) . ?
N19 O8 1.247(7) . ?
N19 O9A 1.248(8) . ?
N19 O8A 1.253(11) . ?
N19 O9 1.269(5) . ?
N20 O10 1.223(5) . ?
N20 O11A 1.226(12) . ?
N20 O12 1.238(4) . ?
N20 O12A 1.251(10) . ?
N20 O10A 1.259(11) . ?
N20 O11 1.290(6) . ?
N21 O15 1.208(7) . ?
N21 O13 1.221(6) . ?
N21 O14 1.230(8) . ?
N22 O18 1.245(8) . ?
N22 O17 1.249(7) . ?
N22 O16 1.257(5) . ?
N22A O17A 1.254(11) . ?
N22A O16A 1.260(9) . ?
N22A O18A 1.267(7) . ?
O11W O12W 1.76(7) . ?

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
N15 Ni1 N2 177.3(3) . . ?
N15 Ni1 O1 90.4(3) . . ?
N2 Ni1 O1 92.3(3) . . ?
N15 Ni1 O4 91.7(3) . . ?
N2 Ni1 O4 88.7(3) . . ?
O1 Ni1 O4 82.6(3) . . ?
N15 Ni1 N1 99.7(3) . . ?
N2 Ni1 N1 77.7(3) . . ?
O1 Ni1 N1 169.6(3) . . ?
O4 Ni1 N1 94.8(3) . . ?
N15 Ni1 N16 77.5(3) . . ?
N2 Ni1 N16 102.3(3) . . ?
O1 Ni1 N16 93.6(3) . . ?
O4 Ni1 N16 168.6(3) . . ?
N1 Ni1 N16 90.9(3) . . ?
N15 Ni1 Ni4 58.9(2) . . ?
N2 Ni1 Ni4 121.8(2) . . ?
O1 Ni1 Ni4 77.0(2) . . ?
O4 Ni1 Ni4 33.70(17) . . ?
N1 Ni1 Ni4 106.3(2) . . ?
N16 Ni1 Ni4 134.9(2) . . ?
N15 Ni1 Ni2 123.6(2) . . ?
N2 Ni1 Ni2 59.1(2) . . ?
O1 Ni1 Ni2 33.96(18) . . ?
O4 Ni1 Ni2 76.47(18) . . ?
N1 Ni1 Ni2 135.7(2) . . ?
N16 Ni1 Ni2 106.2(2) . . ?
Ni4 Ni1 Ni2 90.23(4) . . ?
N3 Ni2 N6 178.7(4) . . ?
N3 Ni2 N5 100.4(4) . . ?
N6 Ni2 N5 78.3(4) . . ?
N3 Ni2 N4 78.7(3) . . ?
N6 Ni2 N4 100.9(3) . . ?
N5 Ni2 N4 91.0(3) . . ?
N3 Ni2 O1 92.6(3) . . ?
N6 Ni2 O1 87.8(3) . . ?
N5 Ni2 O1 94.7(3) . . ?
N4 Ni2 O1 170.4(3) . . ?
N3 Ni2 O2 88.8(3) . . ?
N6 Ni2 O2 92.5(3) . . ?
N5 Ni2 O2 170.4(3) . . ?
N4 Ni2 O2 93.4(3) . . ?
O1 Ni2 O2 82.2(3) . . ?
N3 Ni2 Ni1 59.3(2) . . ?
N6 Ni2 Ni1 121.3(2) . . ?
N5 Ni2 Ni1 105.8(2) . . ?
N4 Ni2 Ni1 136.6(2) . . ?
O1 Ni2 Ni1 34.01(18) . . ?
O2 Ni2 Ni1 76.60(18) . . ?
N3 Ni2 Ni3 121.9(2) . . ?
N6 Ni2 Ni3 59.4(3) . . ?
N5 Ni2 Ni3 136.6(3) . . ?
N4 Ni2 Ni3 105.2(3) . . ?
O1 Ni2 Ni3 75.8(2) . . ?
O2 Ni2 Ni3 33.80(17) . . ?
Ni1 Ni2 Ni3 89.70(4) . . ?
N7 Ni3 N10 177.6(3) . . ?
N7 Ni3 O2 92.5(3) . . ?
N10 Ni3 O2 89.5(3) . . ?
N7 Ni3 N8 78.0(4) . . ?
N10 Ni3 N8 100.0(4) . . ?
O2 Ni3 N8 170.2(4) . . ?
N7 Ni3 O3 89.7(3) . . ?
N10 Ni3 O3 91.9(3) . . ?
O2 Ni3 O3 82.7(2) . . ?
N8 Ni3 O3 94.7(3) . . ?
N7 Ni3 N9 101.2(4) . . ?
N10 Ni3 N9 77.3(4) . . ?
O2 Ni3 N9 95.3(3) . . ?
N8 Ni3 N9 89.0(3) . . ?
O3 Ni3 N9 169.0(4) . . ?
N7 Ni3 Ni4 122.9(2) . . ?
N10 Ni3 Ni4 58.9(2) . . ?
O2 Ni3 Ni4 76.15(19) . . ?
N8 Ni3 Ni4 106.9(3) . . ?
O3 Ni3 Ni4 33.99(19) . . ?
N9 Ni3 Ni4 135.0(3) . . ?
N7 Ni3 Ni2 59.1(3) . . ?
N10 Ni3 Ni2 123.0(2) . . ?
O2 Ni3 Ni2 34.1(2) . . ?
N8 Ni3 Ni2 136.1(3) . . ?
O3 Ni3 Ni2 77.1(2) . . ?
N9 Ni3 Ni2 107.3(3) . . ?
Ni4 Ni3 Ni2 90.14(4) . . ?
N14 Ni4 N11 176.6(4) . . ?
N14 Ni4 O4 91.9(3) . . ?
N11 Ni4 O4 91.1(3) . . ?
N14 Ni4 O3 90.3(3) . . ?
N11 Ni4 O3 91.7(3) . . ?
O4 Ni4 O3 82.7(3) . . ?
N14 Ni4 N12 99.4(3) . . ?
N11 Ni4 N12 78.6(3) . . ?
O4 Ni4 N12 96.4(3) . . ?
O3 Ni4 N12 170.3(3) . . ?
N14 Ni4 N13 78.4(3) . . ?
N11 Ni4 N13 98.7(3) . . ?
O4 Ni4 N13 170.2(3) . . ?
O3 Ni4 N13 96.4(3) . . ?
N12 Ni4 N13 86.1(3) . . ?
N14 Ni4 Ni1 58.9(2) . . ?
N11 Ni4 Ni1 124.3(2) . . ?
O4 Ni4 Ni1 34.07(18) . . ?
O3 Ni4 Ni1 76.07(19) . . ?
N12 Ni4 Ni1 108.5(2) . . ?
N13 Ni4 Ni1 136.2(2) . . ?
N14 Ni4 Ni3 123.8(2) . . ?
N11 Ni4 Ni3 58.6(3) . . ?
O4 Ni4 Ni3 76.75(18) . . ?
O3 Ni4 Ni3 34.18(18) . . ?
N12 Ni4 Ni3 136.2(2) . . ?
N13 Ni4 Ni3 107.9(2) . . ?
Ni1 Ni4 Ni3 89.89(4) . . ?
Ni4 O4 Ni1 112.2(3) . . ?
Ni4 O4 O2 103.3(3) . . ?
Ni1 O4 O2 103.7(3) . . ?
Ni4 O3 Ni3 111.8(3) . . ?
Ni4 O3 O1 104.2(3) . . ?
Ni3 O3 O1 102.5(3) . . ?
Ni3 O2 Ni2 112.1(3) . . ?
Ni3 O2 O4 103.8(3) . . ?
Ni2 O2 O4 103.2(3) . . ?
Ni2 O1 Ni1 112.0(3) . . ?
Ni2 O1 O3 104.6(3) . . ?
Ni1 O1 O3 102.7(3) . . ?
C1 N1 C5 119.7(8) . . ?
C1 N1 Ni1 125.6(7) . . ?
C5 N1 Ni1 114.4(6) . . ?
C6 N2 N3 120.1(8) . . ?
C6 N2 Ni1 117.1(7) . . ?
N3 N2 Ni1 120.6(6) . . ?
C9 N3 N2 120.1(8) . . ?
C9 N3 Ni2 117.1(6) . . ?
N2 N3 Ni2 121.1(6) . . ?
C14 N4 C10 117.5(9) . . ?
C14 N4 Ni2 127.2(7) . . ?
C10 N4 Ni2 115.3(6) . . ?
N1 C1 C2 122.4(10) . . ?
N1 C1 H1A 118.8 . . ?
C2 C1 H1A 118.8 . . ?
C3 C2 C1 118.0(11) . . ?
C3 C2 H2A 121.0 . . ?
C1 C2 H2A 121.0 . . ?
C4 C3 C2 119.6(10) . . ?
C4 C3 H3A 120.2 . . ?
C2 C3 H3A 120.2 . . ?
C3 C4 C5 118.9(10) . . ?
C3 C4 H4A 120.5 . . ?
C5 C4 H4A 120.5 . . ?
N1 C5 C4 121.4(9) . . ?
N1 C5 C6 115.9(8) . . ?
C4 C5 C6 122.5(9) . . ?
N2 C6 C7 121.4(9) . . ?
N2 C6 C5 113.3(9) . . ?
C7 C6 C5 125.3(9) . . ?
C8 C7 C6 118.5(9) . . ?
C8 C7 H7A 120.8 . . ?
C6 C7 H7A 120.8 . . ?
C7 C8 C9 118.6(10) . . ?
C7 C8 H8A 120.7 . . ?
C9 C8 H8A 120.7 . . ?
N3 C9 C8 121.2(9) . . ?
N3 C9 C10 114.3(8) . . ?
C8 C9 C10 124.3(9) . . ?
N4 C10 C11 122.8(10) . . ?
N4 C10 C9 114.1(9) . . ?
C11 C10 C9 123.1(9) . . ?
C10 C11 C12 117.8(10) . . ?
C10 C11 H11A 121.1 . . ?
C12 C11 H11A 121.1 . . ?
C13 C12 C11 119.3(10) . . ?
C13 C12 H12A 120.3 . . ?
C11 C12 H12A 120.3 . . ?
C12 C13 C14 119.2(10) . . ?
C12 C13 H13A 120.4 . . ?
C14 C13 H13A 120.4 . . ?
N4 C14 C13 123.3(11) . . ?
N4 C14 H14A 118.3 . . ?
C13 C14 H14A 118.3 . . ?
C15 N5 C19 117.7(10) . . ?
C15 N5 Ni2 127.0(7) . . ?
C19 N5 Ni2 115.2(8) . . ?
C20 N6 N7 121.9(9) . . ?
C20 N6 Ni2 116.8(8) . . ?
N7 N6 Ni2 120.1(6) . . ?
C23 N7 N6 120.1(10) . . ?
C23 N7 Ni3 117.2(9) . . ?
N6 N7 Ni3 121.4(6) . . ?
C28 N8 C24 119.2(10) . . ?
C28 N8 Ni3 125.6(8) . . ?
C24 N8 Ni3 115.0(8) . . ?
N5 C15 C16 124.3(12) . . ?
N5 C15 H15A 117.8 . . ?
C16 C15 H15A 117.8 . . ?
C15 C16 C17 115.9(14) . . ?
C15 C16 H16A 122.0 . . ?
C17 C16 H16A 122.0 . . ?
C18 C17 C16 121.5(13) . . ?
C18 C17 H17A 119.3 . . ?
C16 C17 H17A 119.3 . . ?
C17 C18 C19 118.7(13) . . ?
C17 C18 H18A 120.7 . . ?
C19 C18 H18A 120.7 . . ?
C18 C19 N5 121.9(13) . . ?
C18 C19 C20 124.1(11) . . ?
N5 C19 C20 114.0(10) . . ?
N6 C20 C21 119.4(12) . . ?
N6 C20 C19 115.4(9) . . ?
C21 C20 C19 125.2(11) . . ?
C22 C21 C20 119.5(12) . . ?
C22 C21 H21A 120.3 . . ?
C20 C21 H21A 120.3 . . ?
C21 C22 C23 118.4(10) . . ?
C21 C22 H22A 120.8 . . ?
C23 C22 H22A 120.8 . . ?
N7 C23 C22 120.5(12) . . ?
N7 C23 C24 113.7(11) . . ?
C22 C23 C24 125.7(10) . . ?
N8 C24 C25 121.7(13) . . ?
N8 C24 C23 115.4(9) . . ?
C25 C24 C23 122.8(12) . . ?
C26 C25 C24 118.7(14) . . ?
C26 C25 H25A 120.7 . . ?
C24 C25 H25A 120.7 . . ?
C25 C26 C27 120.7(12) . . ?
C25 C26 H26A 119.7 . . ?
C27 C26 H26A 119.7 . . ?
C26 C27 C28 117.0(15) . . ?
C26 C27 H27A 121.5 . . ?
C28 C27 H27A 121.5 . . ?
N8 C28 C27 122.7(14) . . ?
N8 C28 H28A 118.7 . . ?
C27 C28 H28A 118.7 . . ?
C33 N9 C29 118.6(10) . . ?
C33 N9 Ni3 116.5(8) . . ?
C29 N9 Ni3 124.7(9) . . ?
N11 N10 C34 120.6(10) . . ?
N11 N10 Ni3 120.8(6) . . ?
C34 N10 Ni3 118.0(8) . . ?
N10 N11 C37 120.8(9) . . ?
N10 N11 Ni4 121.6(7) . . ?
C37 N11 Ni4 116.8(7) . . ?
C42 N12 C38 118.2(9) . . ?
C42 N12 Ni4 126.6(7) . . ?
C38 N12 Ni4 114.6(7) . . ?
N9 C29 C30 121.6(14) . . ?
N9 C29 H29 119.2 . . ?
C30 C29 H29 119.2 . . ?
C31 C30 C29 118.3(14) . . ?
C31 C30 H30 120.9 . . ?
C29 C30 H30 120.9 . . ?
C30 C31 C32 120.6(12) . . ?
C30 C31 H31 119.7 . . ?
C32 C31 H31 119.7 . . ?
C33 C32 C31 117.6(15) . . ?
C33 C32 H32 121.2 . . ?
C31 C32 H32 121.2 . . ?
N9 C33 C32 123.3(13) . . ?
N9 C33 C34 113.5(9) . . ?
C32 C33 C34 123.2(13) . . ?
N10 C34 C35 121.6(11) . . ?
N10 C34 C33 114.5(11) . . ?
C35 C34 C33 123.8(10) . . ?
C36 C35 C34 117.9(10) . . ?
C36 C35 H35 121.1 . . ?
C34 C35 H35 121.1 . . ?
C37 C36 C35 117.7(12) . . ?
C37 C36 H36 121.1 . . ?
C35 C36 H36 121.1 . . ?
N11 C37 C36 121.2(11) . . ?
N11 C37 C38 114.5(9) . . ?
C36 C37 C38 124.4(11) . . ?
N12 C38 C39 123.5(11) . . ?
N12 C38 C37 114.7(10) . . ?
C39 C38 C37 121.9(10) . . ?
C38 C39 C40 117.8(11) . . ?
C38 C39 H39 121.1 . . ?
C40 C39 H39 121.1 . . ?
C39 C40 C41 118.8(11) . . ?
C39 C40 H40 120.6 . . ?
C41 C40 H40 120.6 . . ?
C42 C41 C40 118.8(11) . . ?
C42 C41 H41 120.6 . . ?
C40 C41 H41 120.6 . . ?
N12 C42 C41 122.8(10) . . ?
N12 C42 H42 118.6 . . ?
C41 C42 H42 118.6 . . ?
C43 N13 C47 119.2(9) . . ?
C43 N13 Ni4 125.7(7) . . ?
C47 N13 Ni4 114.3(7) . . ?
N15 N14 C48 119.9(8) . . ?
N15 N14 Ni4 121.3(6) . . ?
C48 N14 Ni4 117.8(7) . . ?
C51 N15 N14 120.7(8) . . ?
C51 N15 Ni1 118.1(7) . . ?
N14 N15 Ni1 120.8(6) . . ?
C56 N16 C52 117.8(9) . . ?
C56 N16 Ni1 125.8(7) . . ?
C52 N16 Ni1 116.3(7) . . ?
N13 C43 C44 122.3(11) . . ?
N13 C43 H43 118.9 . . ?
C44 C43 H43 118.9 . . ?
C43 C44 C45 118.7(11) . . ?
C43 C44 H44 120.7 . . ?
C45 C44 H44 120.7 . . ?
C46 C45 C44 118.8(11) . . ?
C46 C45 H45 120.6 . . ?
C44 C45 H45 120.6 . . ?
C47 C46 C45 118.8(10) . . ?
C47 C46 H46 120.6 . . ?
C45 C46 H46 120.6 . . ?
N13 C47 C46 122.2(10) . . ?
N13 C47 C48 115.4(9) . . ?
C46 C47 C48 122.3(9) . . ?
N14 C48 C49 120.6(10) . . ?
N14 C48 C47 113.2(8) . . ?
C49 C48 C47 126.0(9) . . ?
C50 C49 C48 118.7(10) . . ?
C50 C49 H49 120.7 . . ?
C48 C49 H49 120.7 . . ?
C49 C50 C51 119.1(10) . . ?
C49 C50 H50 120.5 . . ?
C51 C50 H50 120.5 . . ?
N15 C51 C50 120.8(10) . . ?
N15 C51 C52 114.2(9) . . ?
C50 C51 C52 124.8(9) . . ?
N16 C52 C53 123.4(11) . . ?
N16 C52 C51 113.5(9) . . ?
C53 C52 C51 123.0(10) . . ?
C52 C53 C54 118.1(11) . . ?
C52 C53 H53 120.9 . . ?
C54 C53 H53 120.9 . . ?
C55 C54 C53 119.4(11) . . ?
C55 C54 H54 120.3 . . ?
C53 C54 H54 120.3 . . ?
C54 C55 C56 118.9(12) . . ?
C54 C55 H55 120.5 . . ?
C56 C55 H55 120.5 . . ?
N16 C56 C55 122.3(11) . . ?
N16 C56 H56 118.8 . . ?
C55 C56 H56 118.8 . . ?
O3N N17 O2N 131.4(8) . . ?
O1A N17 O2A 129.3(11) . . ?
O1A N17 O3A 111.8(8) . . ?
O2A N17 O3A 118.9(9) . . ?
O3N N17 O1N 119.0(8) . . ?
O2N N17 O1N 109.6(7) . . ?
O4N N18 O5N 118.1(4) . . ?
O4N N18 O6N 118.3(4) . . ?
O5N N18 O6N 123.5(3) . . ?
O7 N19 O8 122.9(3) . . ?
O7 N19 O9A 124.1(10) . . ?
O7 N19 O8A 113.7(5) . . ?
O9A N19 O8A 122.2(10) . . ?
O7 N19 O9 115.7(4) . . ?
O8 N19 O9 121.5(4) . . ?
O10 N20 O12 120.0(4) . . ?
O11A N20 O12A 122.6(10) . . ?
O11A N20 O10A 123.7(7) . . ?
O12A N20 O10A 113.7(12) . . ?
O10 N20 O11 117.7(3) . . ?
O12 N20 O11 122.3(3) . . ?
O15 N21 O13 116.7(7) . . ?
O15 N21 O14 121.4(4) . . ?
O13 N21 O14 121.9(6) . . ?
O18 N22 O17 121.7(4) . . ?
O18 N22 O16 119.0(5) . . ?
O17 N22 O16 119.3(6) . . ?
O17A N22A O16A 118.7(6) . . ?
O17A N22A O18A 121.3(7) . . ?
O16A N22A O18A 120.0(8) . . ?

_refine_diff_density_max         2.999
_refine_diff_density_min         -1.329
_refine_diff_density_rms         0.252

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_RB15nad
_database_code_depnum_ccdc_archive 'CCDC 1868873'
_audit_update_record             
;
2018-12-20 deposited with the CCDC.
2019-01-04 downloaded from the CCDC.
;

_vrf_PLAT430_RB15nad             
;
PROBLEM: Short Inter D...A Contact  O5W      ..O12W     .       2.53 Ang.  
RESPONSE: The water molecules of crystallization are generally disordered  
over multiple sites (identified sites are 15). We defined a total of 10 
water molecules according to other experimental evidences. We first 
attemped to refine freely the disordered sites, then we fixed the occupancies
for convenience. Thus, the idea is that the solvent molecules are disordered
over multiple sites and the occupancy of each site may slightly differ from
the one approximately assigned by us. Note that also one of the four ethanol
molecules of crystallization [O4S-C7S-C8S], as well as five of the ten 
perchlorate counterions, are severely disordered (for these all disorders were 
refined freely till convergence), thus contributing to generating the same
type of alert.
;
_vrf_PLAT221_RB15nad             
;
PROBLEM: Solv./Anion  Resd12  O   Ueq(max)/Ueq(min) Range       10.0 Ratio 
RESPONSE: The great majority of the sites identifying anions and solvent
molecules of crystallization are disordered over multiple sites (with the 
assigned partially occupied sites often mutually excluding one another). Two 
perchlorate anions are even distributed over four sites, in which additional 
disorder is present. With all the disorders, even if the model does not 
behave horribly, we should take into account the possibility of some positional
uncertainty. However, we are pretty confident about the atomic assignements. 
;
_vrf_PLAT306_RB15nad             
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O1W Check 
RESPONSE: The hydrogen atoms of the coordinated water (1 H2O) and hydroxo 
groups (3 OH-) as well as those of all the crystallization water molecules 
(10 H2O in the asymmetric unit = formally 5 H2O molecules per tetramer) were 
neither found nor calculated. Note that they were obviously included in the  
UNIT instruction, so there would be a discrepancy between the calculated and 
the reported MW. 
;
_vrf_PLAT420_RB15nad             
;
PROBLEM: D-H Without Acceptor       O4S      --H4SD     .     Please Check 
RESPONSE: [O4S-C7S-C8S] is a solvent (ethanol) molecule of crystallization
disordered over two sites sharing the oxygen atom [O4S]. The hydrogen atoms
of this ethanol molecule were placed in calculated positions, for convenience.
In fact, only the H atoms on the hydroxo groups/water molecules of the 
tetramers' cores and those of the crystallization water molecules were not 
defined. Note that the H atom of the ethanolic hydroxy group has to be 
distributed over two sites according to the disorder of the rest of the 
molecule). One of such two calculated positions for the -OH hydrogen atom 
(i.e. H4SE) is compatible with ah hydrogen bond (but still not ideal), 
while the other (i. e. H4SD) is not. This would not be surprising in the 
presence of such disorder. However, the reason appears to reside in the 
crystal packing, as there are no great possibilities of establishing 
H-bonds from the cavity hosting this disordered ethanol molecule.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'2(C56 H45 N16 Ni4 O4), 10(Cl O4), 10(H2 O), 4(C2 H6 O)'
_chemical_formula_sum            'C120 H134 Cl10 N32 Ni8 O62'
_chemical_formula_weight         3840.76

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'
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                   12.4085(4)
_cell_length_b                   23.2955(8)
_cell_length_c                   28.0056(9)
_cell_angle_alpha                86.006(2)
_cell_angle_beta                 81.190(2)
_cell_angle_gamma                83.687(2)
_cell_volume                     7939.8(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9897
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      26.10

_exptl_crystal_description       LAMINAR
_exptl_crystal_colour            AMBER-YELLOW
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_F_000             3936
_exptl_transmission_factor_min   0.6320
_exptl_transmission_factor_max   0.7453
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    1.195
_shelx_estimated_absorpt_T_min   0.754
_shelx_estimated_absorpt_T_max   0.976
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   
'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker X8 Apex-II CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            178982
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         0.737
_diffrn_reflns_theta_max         26.233
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             31814
_reflns_number_gt                25744
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013, version 2013-4 (Sheldrick 2013)'
_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)+(0.1002P)²+28.6863P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     Patt
_atom_sites_solution_secondary   Difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         31814
_refine_ls_number_parameters     2248
_refine_ls_number_restraints     506
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0591
_refine_ls_wR_factor_ref         0.1863
_refine_ls_wR_factor_gt          0.1711
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.109
_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 0.25491(4) 0.61375(2) 0.35028(2) 0.01846(11) Uani 1 1 d . . . . .
Ni2 Ni 0.29384(4) 0.71715(2) 0.42349(2) 0.02133(12) Uani 1 1 d . . . . .
Ni3 Ni 0.22977(4) 0.82329(2) 0.33580(2) 0.02184(12) Uani 1 1 d . . . . .
Ni4 Ni 0.18467(4) 0.72011(2) 0.26436(2) 0.01877(12) Uani 1 1 d . . . . .
O1 O 0.1875(2) 0.67832(12) 0.39279(10) 0.0210(6) Uani 1 1 d . . . . .
O2 O 0.3414(2) 0.75413(12) 0.35413(10) 0.0233(6) Uani 1 1 d . . . . .
O3 O 0.1309(2) 0.76379(12) 0.32486(10) 0.0221(6) Uani 1 1 d . . . . .
O4 O 0.3075(2) 0.67902(12) 0.30087(10) 0.0200(6) Uani 1 1 d . . . . .
N1 N 0.3528(3) 0.54981(15) 0.31103(13) 0.0232(7) Uani 1 1 d . . . . .
C1 C 0.3215(4) 0.51894(19) 0.27816(16) 0.0285(9) Uani 1 1 d . . . . .
H1A H 0.2516 0.5295 0.2685 0.034 Uiso 1 1 calc R U . . .
C2 C 0.3864(4) 0.4721(2) 0.25744(19) 0.0357(11) Uani 1 1 d . . . . .
H2A H 0.3618 0.4512 0.2339 0.043 Uiso 1 1 calc R U . . .
C3 C 0.4876(4) 0.4566(2) 0.2719(2) 0.0387(12) Uani 1 1 d . . . . .
H3A H 0.5327 0.4239 0.2592 0.046 Uiso 1 1 calc R U . . .
C4 C 0.5233(4) 0.4893(2) 0.30535(18) 0.0310(10) Uani 1 1 d . . . . .
H4A H 0.5937 0.4800 0.3149 0.037 Uiso 1 1 calc R U . . .
C5 C 0.4543(3) 0.53530(18) 0.32419(16) 0.0240(8) Uani 1 1 d . . . . .
C6 C 0.4834(3) 0.57385(18) 0.35909(15) 0.0226(8) Uani 1 1 d . . . . .
N2 N 0.3998(3) 0.61007(14) 0.37808(12) 0.0207(7) Uani 1 1 d . . . . .
C7 C 0.5891(3) 0.57508(19) 0.37111(16) 0.0261(9) Uani 1 1 d . . . . .
H7A H 0.6484 0.5484 0.3584 0.031 Uiso 1 1 calc R U . . .
C8 C 0.6037(4) 0.61614(19) 0.40183(17) 0.0280(9) Uani 1 1 d . . . . .
H8A H 0.6734 0.6184 0.4112 0.034 Uiso 1 1 calc R U . . .
C9 C 0.5132(3) 0.65457(19) 0.41899(16) 0.0263(9) Uani 1 1 d . . . . .
N3 N 0.4144(3) 0.64998(15) 0.40739(13) 0.0228(7) Uani 1 1 d . . . . .
C10 C 0.5163(4) 0.7035(2) 0.4499(2) 0.0356(11) Uani 1 1 d . . . . .
C11 C 0.6028(5) 0.7094(3) 0.4742(3) 0.0559(17) Uani 1 1 d . . . . .
H11A H 0.6647 0.6813 0.4720 0.067 Uiso 1 1 calc R U . . .
C12 C 0.5976(6) 0.7567(3) 0.5017(3) 0.078(3) Uani 1 1 d . . . . .
H12A H 0.6557 0.7614 0.5191 0.094 Uiso 1 1 calc R U . . .
C13 C 0.5066(6) 0.7973(3) 0.5037(3) 0.079(3) Uani 1 1 d . . . . .
H13A H 0.5022 0.8307 0.5219 0.095 Uiso 1 1 calc R U . . .
C14 C 0.4231(4) 0.7884(2) 0.4790(2) 0.0489(15) Uani 1 1 d . . . . .
H14A H 0.3605 0.8160 0.4808 0.059 Uiso 1 1 calc R U . . .
N4 N 0.4259(3) 0.74250(17) 0.45254(15) 0.0317(9) Uani 1 1 d . . . . .
N5 N 0.2221(3) 0.69133(16) 0.49249(13) 0.0265(8) Uani 1 1 d . . . . .
C15 C 0.2516(4) 0.6424(2) 0.51735(17) 0.0299(10) Uani 1 1 d . . . . .
H15A H 0.3117 0.6171 0.5034 0.036 Uiso 1 1 calc R U . . .
C16 C 0.1970(4) 0.6275(2) 0.56299(18) 0.0381(11) Uani 1 1 d . . . . .
H16A H 0.2188 0.5924 0.5799 0.046 Uiso 1 1 calc R U . . .
C17 C 0.1107(5) 0.6646(3) 0.58312(18) 0.0445(13) Uani 1 1 d . . . . .
H17A H 0.0732 0.6557 0.6145 0.053 Uiso 1 1 calc R U . . .
C18 C 0.0790(4) 0.7145(3) 0.55784(18) 0.0403(12) Uani 1 1 d . . . . .
H18A H 0.0187 0.7401 0.5712 0.048 Uiso 1 1 calc R U . . .
C19 C 0.1365(4) 0.7272(2) 0.51219(16) 0.0298(10) Uani 1 1 d . . . . .
C20 C 0.1069(4) 0.7789(2) 0.48133(16) 0.0313(10) Uani 1 1 d . . . . .
N6 N 0.1756(3) 0.78482(16) 0.43970(13) 0.0245(7) Uani 1 1 d . . . . .
C21 C 0.0140(4) 0.8182(3) 0.49196(19) 0.0432(13) Uani 1 1 d . . . . .
H21A H -0.0341 0.8144 0.5216 0.052 Uiso 1 1 calc R U . . .
C22 C -0.0056(5) 0.8623(3) 0.4583(2) 0.0458(14) Uani 1 1 d . . . . .
H22A H -0.0669 0.8903 0.4646 0.055 Uiso 1 1 calc R U . . .
C23 C 0.0662(4) 0.8653(2) 0.41446(18) 0.0335(10) Uani 1 1 d . . . . .
N7 N 0.1545(3) 0.82691(16) 0.40674(13) 0.0264(8) Uani 1 1 d . . . . .
C24 C 0.0515(4) 0.9078(2) 0.37347(18) 0.0355(11) Uani 1 1 d . . . . .
C25 C -0.0170(5) 0.9586(3) 0.3779(2) 0.0538(16) Uani 1 1 d . . . . .
H25A H -0.0594 0.9678 0.4081 0.065 Uiso 1 1 calc R U . . .
C26 C -0.0226(6) 0.9959(3) 0.3376(2) 0.0615(19) Uani 1 1 d . . . . .
H26A H -0.0689 1.0312 0.3397 0.074 Uiso 1 1 calc R U . . .
C27 C 0.0395(5) 0.9814(2) 0.2942(2) 0.0450(13) Uani 1 1 d . . . . .
H27A H 0.0371 1.0066 0.2662 0.054 Uiso 1 1 calc R U . . .
C28 C 0.1053(4) 0.9297(2) 0.29224(18) 0.0330(10) Uani 1 1 d . . . . .
H28A H 0.1468 0.9194 0.2621 0.040 Uiso 1 1 calc R U . . .
N8 N 0.1130(3) 0.89358(15) 0.33117(14) 0.0275(8) Uani 1 1 d . . . . .
N9 N 0.3432(3) 0.88374(16) 0.33351(14) 0.0292(8) Uani 1 1 d . . . . .
C29 C 0.3507(5) 0.9171(3) 0.3692(2) 0.0520(15) Uani 1 1 d . . . . .
H29A H 0.3123 0.9086 0.4005 0.062 Uiso 1 1 calc R U . . .
C30 C 0.4124(7) 0.9640(4) 0.3624(3) 0.086(3) Uani 1 1 d . . . . .
H30A H 0.4152 0.9874 0.3886 0.104 Uiso 1 1 calc R U . . .
C31 C 0.4686(7) 0.9759(4) 0.3181(3) 0.090(3) Uani 1 1 d . . . . .
H31A H 0.5115 1.0077 0.3130 0.108 Uiso 1 1 calc R U . . .
C32 C 0.4634(5) 0.9413(3) 0.2801(2) 0.0550(17) Uani 1 1 d . . . . .
H32A H 0.5025 0.9489 0.2488 0.066 Uiso 1 1 calc R U . . .
C33 C 0.3996(4) 0.8957(2) 0.28922(18) 0.0316(10) Uani 1 1 d . . . . .
C34 C 0.3857(4) 0.85656(19) 0.25188(17) 0.0271(9) Uani 1 1 d . . . . .
N10 N 0.3052(3) 0.82289(15) 0.26541(13) 0.0228(7) Uani 1 1 d . . . . .
C35 C 0.4504(4) 0.8526(2) 0.20628(17) 0.0310(10) Uani 1 1 d . . . . .
H35A H 0.5045 0.8784 0.1958 0.037 Uiso 1 1 calc R U . . .
C36 C 0.4333(4) 0.8105(2) 0.17731(17) 0.0320(10) Uani 1 1 d . . . . .
H36A H 0.4756 0.8062 0.1463 0.038 Uiso 1 1 calc R U . . .
C37 C 0.3512(3) 0.77390(19) 0.19482(15) 0.0246(9) Uani 1 1 d . . . . .
N11 N 0.2879(3) 0.78207(15) 0.23705(12) 0.0218(7) Uani 1 1 d . . . . .
C38 C 0.3323(4) 0.72170(19) 0.17119(15) 0.0261(9) Uani 1 1 d . . . . .
C39 C 0.3864(4) 0.7063(2) 0.12629(18) 0.0370(11) Uani 1 1 d . . . . .
H39A H 0.4347 0.7311 0.1077 0.044 Uiso 1 1 calc R U . . .
C40 C 0.3695(5) 0.6547(2) 0.10873(18) 0.0432(13) Uani 1 1 d . . . . .
H40A H 0.4063 0.6433 0.0780 0.052 Uiso 1 1 calc R U . . .
C41 C 0.2980(5) 0.6195(2) 0.13670(18) 0.0391(11) Uani 1 1 d . . . . .
H41A H 0.2855 0.5835 0.1257 0.047 Uiso 1 1 calc R U . . .
C42 C 0.2452(4) 0.63801(19) 0.18101(16) 0.0273(9) Uani 1 1 d . . . . .
H42A H 0.1952 0.6143 0.1999 0.033 Uiso 1 1 calc R U . . .
N12 N 0.2617(3) 0.68773(15) 0.19824(13) 0.0234(7) Uani 1 1 d . . . . .
N13 N 0.0431(3) 0.74874(15) 0.23429(12) 0.0223(7) Uani 1 1 d . . . . .
C43 C 0.0283(4) 0.79583(18) 0.20484(17) 0.0278(9) Uani 1 1 d . . . . .
H43A H 0.0865 0.8197 0.1967 0.033 Uiso 1 1 calc R U . . .
C44 C -0.0676(4) 0.8112(2) 0.18579(18) 0.0343(11) Uani 1 1 d . . . . .
H44A H -0.0757 0.8453 0.1655 0.041 Uiso 1 1 calc R U . . .
C45 C -0.1520(4) 0.7760(2) 0.1967(2) 0.0418(12) Uani 1 1 d . . . . .
H45A H -0.2185 0.7851 0.1836 0.050 Uiso 1 1 calc R U . . .
C46 C -0.1374(4) 0.7270(2) 0.22707(19) 0.0369(11) Uani 1 1 d . . . . .
H46A H -0.1939 0.7021 0.2351 0.044 Uiso 1 1 calc R U . . .
C47 C -0.0403(3) 0.71488(18) 0.24545(15) 0.0240(8) Uani 1 1 d . . . . .
C48 C -0.0197(3) 0.66497(18) 0.28022(15) 0.0218(8) Uani 1 1 d . . . . .
N14 N 0.0824(3) 0.65662(14) 0.29017(12) 0.0195(7) Uani 1 1 d . . . . .
C49 C -0.1008(3) 0.63060(18) 0.30274(16) 0.0248(9) Uani 1 1 d . . . . .
H49A H -0.1727 0.6358 0.2944 0.030 Uiso 1 1 calc R U . . .
C50 C -0.0732(3) 0.58957(18) 0.33696(15) 0.0229(8) Uani 1 1 d . . . . .
H50A H -0.1259 0.5656 0.3535 0.027 Uiso 1 1 calc R U . . .
C51 C 0.0342(3) 0.58338(17) 0.34732(15) 0.0214(8) Uani 1 1 d . . . . .
N15 N 0.1093(3) 0.61590(14) 0.32318(12) 0.0200(7) Uani 1 1 d . . . . .
C52 C 0.0745(3) 0.54315(18) 0.38599(15) 0.0226(8) Uani 1 1 d . . . . .
C53 C 0.0126(4) 0.5024(2) 0.41192(17) 0.0323(10) Uani 1 1 d . . . . .
H53A H -0.0583 0.4977 0.4049 0.039 Uiso 1 1 calc R U . . .
C54 C 0.0566(4) 0.4684(2) 0.44861(19) 0.0411(12) Uani 1 1 d . . . . .
H54A H 0.0156 0.4402 0.4671 0.049 Uiso 1 1 calc R U . . .
C55 C 0.1596(4) 0.4759(2) 0.4577(2) 0.0424(13) Uani 1 1 d . . . . .
H55A H 0.1909 0.4530 0.4824 0.051 Uiso 1 1 calc R U . . .
C56 C 0.2173(4) 0.5177(2) 0.43013(17) 0.0312(10) Uani 1 1 d . . . . .
H56A H 0.2884 0.5230 0.4366 0.037 Uiso 1 1 calc R U . . .
N16 N 0.1762(3) 0.55046(15) 0.39482(13) 0.0226(7) Uani 1 1 d . . . . .
Ni5 Ni 0.71497(4) 0.21837(2) 0.07680(2) 0.02515(13) Uani 1 1 d . . . . .
Ni6 Ni 0.66537(4) 0.13240(2) 0.17974(2) 0.02342(12) Uani 1 1 d . . . . .
Ni7 Ni 0.70128(5) 0.24570(2) 0.24856(2) 0.02653(13) Uani 1 1 d . . . . .
Ni8 Ni 0.75135(4) 0.33175(2) 0.14523(2) 0.02594(13) Uani 1 1 d . . . . .
O5 O 0.6100(2) 0.20023(13) 0.13725(11) 0.0253(6) Uani 1 1 d . . . . .
O6 O 0.7713(2) 0.18622(13) 0.19875(11) 0.0271(6) Uani 1 1 d . . . . .
O7 O 0.6419(2) 0.29103(13) 0.19269(11) 0.0277(7) Uani 1 1 d . . . . .
O8 O 0.8122(2) 0.24917(13) 0.12265(12) 0.0304(7) Uani 1 1 d . . . . .
N17 N 0.8385(3) 0.22205(18) 0.01746(15) 0.0359(9) Uani 1 1 d . . . . .
C57 C 0.8476(4) 0.2650(2) -0.01687(18) 0.0377(11) Uani 1 1 d . . . . .
H57A H 0.7961 0.2983 -0.0140 0.045 Uiso 1 1 calc R U . . .
C58 C 0.9306(5) 0.2621(3) -0.0567(2) 0.0479(14) Uani 1 1 d . . . . .
H58A H 0.9356 0.2931 -0.0806 0.058 Uiso 1 1 calc R U . . .
C59 C 1.0040(5) 0.2143(3) -0.0608(2) 0.0517(15) Uani 1 1 d . . . . .
H59A H 1.0612 0.2117 -0.0876 0.062 Uiso 1 1 calc R U . . .
C60 C 0.9953(5) 0.1694(3) -0.0259(2) 0.0553(16) Uani 1 1 d . . . . .
H60A H 1.0458 0.1356 -0.0286 0.066 Uiso 1 1 calc R U . . .
C61 C 0.9119(5) 0.1743(2) 0.0131(2) 0.0453(13) Uani 1 1 d . . . . .
N18 N 0.8040(3) 0.13884(17) 0.08388(15) 0.0315(9) Uani 1 1 d . . . . .
C62 C 0.8970(5) 0.1296(2) 0.0537(2) 0.0476(14) Uani 1 1 d . . . . .
C63 C 0.9753(6) 0.0832(3) 0.0626(3) 0.078(3) Uani 1 1 d . . . . .
H63A H 1.0420 0.0768 0.0411 0.094 Uiso 1 1 calc R U . . .
C64 C 0.9534(5) 0.0477(3) 0.1028(3) 0.065(2) Uani 1 1 d . . . . .
H64A H 1.0033 0.0154 0.1097 0.078 Uiso 1 1 calc R U . . .
C65 C 0.8552(4) 0.0603(2) 0.13364(19) 0.0374(11) Uani 1 1 d . . . . .
N19 N 0.7836(3) 0.10465(16) 0.12360(14) 0.0284(8) Uani 1 1 d . . . . .
C66 C 0.8248(4) 0.0294(2) 0.18095(19) 0.0327(10) Uani 1 1 d . . . . .
C67 C 0.8746(4) -0.0245(2) 0.1943(2) 0.0359(11) Uani 1 1 d . . . . .
H67A H 0.9311 -0.0441 0.1726 0.043 Uiso 1 1 calc R U . . .
C68 C 0.8401(5) -0.0491(2) 0.2397(2) 0.0430(12) Uani 1 1 d . . . . .
H68A H 0.8711 -0.0865 0.2493 0.052 Uiso 1 1 calc R U . . .
C69 C 0.7605(5) -0.0191(2) 0.2710(2) 0.0413(12) Uani 1 1 d . . . . .
H69A H 0.7372 -0.0350 0.3025 0.050 Uiso 1 1 calc R U . . .
C70 C 0.7151(4) 0.0347(2) 0.25536(17) 0.0315(10) Uani 1 1 d . . . . .
H70A H 0.6609 0.0556 0.2771 0.038 Uiso 1 1 calc R U . . .
N20 N 0.7444(3) 0.05853(16) 0.21099(15) 0.0291(8) Uani 1 1 d . . . . .
N21 N 0.5368(3) 0.08392(15) 0.17289(14) 0.0262(8) Uani 1 1 d . . . . .
C71 C 0.5376(4) 0.0436(2) 0.14143(18) 0.0328(10) Uani 1 1 d . . . . .
H71A H 0.6017 0.0360 0.1186 0.039 Uiso 1 1 calc R U . . .
C72 C 0.4498(4) 0.0120(2) 0.1402(2) 0.0368(11) Uani 1 1 d . . . . .
H72A H 0.4533 -0.0159 0.1167 0.044 Uiso 1 1 calc R U . . .
C73 C 0.3570(4) 0.0221(2) 0.1739(2) 0.0358(11) Uani 1 1 d . . . . .
H73A H 0.2957 0.0009 0.1742 0.043 Uiso 1 1 calc R U . . .
C74 C 0.3550(4) 0.0637(2) 0.20728(18) 0.0311(10) Uani 1 1 d . . . . .
H74A H 0.2924 0.0713 0.2309 0.037 Uiso 1 1 calc R U . . .
C75 C 0.4455(3) 0.09401(18) 0.20568(16) 0.0251(9) Uani 1 1 d . . . . .
N22 N 0.5481(3) 0.15907(15) 0.23654(13) 0.0249(7) Uani 1 1 d . . . . .
C76 C 0.4498(3) 0.14028(19) 0.23918(16) 0.0261(9) Uani 1 1 d . . . . .
C77 C 0.3597(4) 0.1644(2) 0.26942(19) 0.0344(11) Uani 1 1 d . . . . .
H77A H 0.2896 0.1511 0.2706 0.041 Uiso 1 1 calc R U . . .
C78 C 0.3743(4) 0.2078(2) 0.29748(19) 0.0379(11) Uani 1 1 d . . . . .
H78A H 0.3148 0.2254 0.3188 0.045 Uiso 1 1 calc R U . . .
C79 C 0.4799(4) 0.2256(2) 0.29376(17) 0.0305(10) Uani 1 1 d . . . . .
N23 N 0.5625(3) 0.20162(16) 0.26368(14) 0.0264(8) Uani 1 1 d . . . . .
C80 C 0.5084(4) 0.2727(2) 0.32142(18) 0.0324(10) Uani 1 1 d . . . . .
C81 C 0.4421(5) 0.2932(2) 0.3625(2) 0.0420(12) Uani 1 1 d . . . . .
H81A H 0.3746 0.2778 0.3741 0.050 Uiso 1 1 calc R U . . .
C82 C 0.4766(5) 0.3368(2) 0.3861(2) 0.0457(13) Uani 1 1 d . . . . .
H82A H 0.4325 0.3520 0.4140 0.055 Uiso 1 1 calc R U . . .
C83 C 0.5746(5) 0.3575(2) 0.3688(2) 0.0434(13) Uani 1 1 d . . . . .
H83A H 0.5999 0.3870 0.3847 0.052 Uiso 1 1 calc R U . . .
C84 C 0.6368(5) 0.3349(2) 0.3277(2) 0.0384(11) Uani 1 1 d . . . . .
H84A H 0.7049 0.3496 0.3159 0.046 Uiso 1 1 calc R U . . .
N24 N 0.6051(3) 0.29331(17) 0.30403(15) 0.0323(9) Uani 1 1 d . . . . .
N25 N 0.7929(4) 0.20827(17) 0.30128(15) 0.0343(9) Uani 1 1 d . . . . .
C85 C 0.7595(5) 0.1687(2) 0.3358(2) 0.0431(12) Uani 1 1 d . . . . .
H85A H 0.6896 0.1553 0.3365 0.052 Uiso 1 1 calc R U . . .
C86 C 0.8245(6) 0.1463(3) 0.3710(2) 0.0550(16) Uani 1 1 d . . . . .
H86A H 0.7995 0.1180 0.3951 0.066 Uiso 1 1 calc R U . . .
C87 C 0.9255(7) 0.1663(3) 0.3698(2) 0.0618(19) Uani 1 1 d . . . . .
H87A H 0.9716 0.1515 0.3929 0.074 Uiso 1 1 calc R U . . .
C88 C 0.9595(5) 0.2080(2) 0.3348(2) 0.0488(14) Uani 1 1 d . . . . .
H88A H 1.0285 0.2225 0.3337 0.059 Uiso 1 1 calc R U . . .
C89 C 0.8908(4) 0.2282(2) 0.30131(19) 0.0363(11) Uani 1 1 d . . . . .
N26 N 0.8420(3) 0.28805(16) 0.23435(15) 0.0302(8) Uani 1 1 d . . . . .
C90 C 0.9216(4) 0.2709(2) 0.26115(19) 0.0338(11) Uani 1 1 d . . . . .
C91 C 1.0241(4) 0.2916(2) 0.2498(2) 0.0442(13) Uani 1 1 d . . . . .
H91A H 1.0795 0.2813 0.2697 0.053 Uiso 1 1 calc R U . . .
C92 C 1.0423(4) 0.3272(2) 0.2089(2) 0.0465(14) Uani 1 1 d . . . . .
H92A H 1.1107 0.3426 0.2001 0.056 Uiso 1 1 calc R U . . .
C93 C 0.9589(4) 0.3405(2) 0.1805(2) 0.0355(11) Uani 1 1 d . . . . .
N27 N 0.8604(3) 0.32168(16) 0.19458(15) 0.0294(8) Uani 1 1 d . . . . .
C94 C 0.9701(4) 0.3727(2) 0.1331(2) 0.0392(12) Uani 1 1 d . . . . .
C95 C 1.0600(5) 0.4024(3) 0.1147(3) 0.0529(15) Uani 1 1 d . . . . .
H95A H 1.1178 0.4039 0.1331 0.063 Uiso 1 1 calc R U . . .
C96 C 1.0638(5) 0.4297(3) 0.0690(3) 0.0656(19) Uani 1 1 d . . . . .
H96A H 1.1246 0.4501 0.0556 0.079 Uiso 1 1 calc R U . . .
C97 C 0.9780(5) 0.4269(3) 0.0430(3) 0.0565(16) Uani 1 1 d . . . . .
H97A H 0.9792 0.4455 0.0117 0.068 Uiso 1 1 calc R U . . .
C98 C 0.8905(4) 0.3966(2) 0.0633(2) 0.0437(13) Uani 1 1 d . . . . .
H98A H 0.8317 0.3949 0.0454 0.052 Uiso 1 1 calc R U . . .
N28 N 0.8866(3) 0.36974(17) 0.10738(16) 0.0353(9) Uani 1 1 d . . . . .
N29 N 0.6785(3) 0.41640(16) 0.15538(14) 0.0279(8) Uani 1 1 d . . . . .
C99 C 0.7081(4) 0.4540(2) 0.18342(18) 0.0343(10) Uani 1 1 d . . . . .
H99A H 0.7601 0.4408 0.2044 0.041 Uiso 1 1 calc R U . . .
C100 C 0.6663(4) 0.5119(2) 0.1833(2) 0.0398(12) Uani 1 1 d . . . . .
H10A H 0.6908 0.5378 0.2031 0.048 Uiso 1 1 calc R U . . .
C101 C 0.5886(4) 0.5311(2) 0.15391(19) 0.0388(11) Uani 1 1 d . . . . .
H10B H 0.5570 0.5701 0.1539 0.047 Uiso 1 1 calc R U . . .
C102 C 0.5576(4) 0.4926(2) 0.12444(18) 0.0329(10) Uani 1 1 d . . . . .
H10C H 0.5054 0.5051 0.1034 0.039 Uiso 1 1 calc R U . . .
C103 C 0.6038(3) 0.43538(19) 0.12589(17) 0.0271(9) Uani 1 1 d . . . . .
N30 N 0.6458(3) 0.34277(15) 0.09432(13) 0.0249(7) Uani 1 1 d . . . . .
C104 C 0.5786(4) 0.39160(19) 0.09463(17) 0.0271(9) Uani 1 1 d . . . . .
C105 C 0.4919(4) 0.3987(2) 0.06715(18) 0.0322(10) Uani 1 1 d . . . . .
H10D H 0.4458 0.4340 0.0665 0.039 Uiso 1 1 calc R U . . .
C106 C 0.4756(4) 0.3537(2) 0.04142(18) 0.0304(10) Uani 1 1 d . . . . .
H10E H 0.4176 0.3567 0.0226 0.036 Uiso 1 1 calc R U . . .
C107 C 0.5467(3) 0.30287(19) 0.04351(16) 0.0257(9) Uani 1 1 d . . . . .
N31 N 0.6302(3) 0.29882(15) 0.06910(13) 0.0244(7) Uani 1 1 d . . . . .
C108 C 0.5358(4) 0.2496(2) 0.01944(16) 0.0275(9) Uani 1 1 d . . . . .
C109 C 0.4592(4) 0.2466(2) -0.01115(16) 0.0321(10) Uani 1 1 d . . . . .
H10F H 0.4115 0.2797 -0.0185 0.039 Uiso 1 1 calc R U . . .
C110 C 0.4535(4) 0.1942(2) -0.03094(18) 0.0384(11) Uani 1 1 d . . . . .
H11B H 0.4015 0.1909 -0.0520 0.046 Uiso 1 1 calc R U . . .
C111 C 0.5236(5) 0.1472(2) -0.0198(2) 0.0427(12) Uani 1 1 d . . . . .
H11C H 0.5206 0.1110 -0.0330 0.051 Uiso 1 1 calc R U . . .
C112 C 0.5987(4) 0.1531(2) 0.01073(19) 0.0379(11) Uani 1 1 d . . . . .
H11D H 0.6477 0.1204 0.0178 0.045 Uiso 1 1 calc R U . . .
N32 N 0.6054(3) 0.20294(17) 0.03083(14) 0.0299(8) Uani 1 1 d . . . . .
Cl1 Cl -0.09697(8) 0.66468(5) 0.46469(4) 0.0294(2) Uani 1 1 d . . . . .
O1P O 0.0121(2) 0.63683(14) 0.46690(12) 0.0319(7) Uani 1 1 d . . . . .
O2P O -0.1553(3) 0.6689(2) 0.51308(14) 0.0578(12) Uani 1 1 d . . . . .
O3P O -0.1548(3) 0.6295(2) 0.43978(16) 0.0540(11) Uani 1 1 d . . . . .
O4P O -0.0915(4) 0.7212(2) 0.4429(2) 0.0741(15) Uani 1 1 d . . . . .
Cl2 Cl 0.58828(9) 0.66296(5) 0.23497(5) 0.0350(3) Uani 1 1 d . . . . .
O5P O 0.4930(3) 0.63326(15) 0.23408(13) 0.0355(8) Uani 1 1 d . . . . .
O6P O 0.6516(4) 0.6364(2) 0.2682(2) 0.088(2) Uani 1 1 d . . . . .
O7P O 0.5606(5) 0.7209(2) 0.2397(4) 0.127(3) Uani 1 1 d . . . . .
O8P O 0.6569(6) 0.6564(4) 0.1895(2) 0.132(3) Uani 1 1 d . . . . .
Cl3 Cl 1.04584(11) 0.12390(6) 0.21916(6) 0.0512(4) Uani 1 1 d . . . . .
O9P O 1.0999(3) 0.07746(19) 0.19024(18) 0.0572(11) Uani 1 1 d . . . . .
O10P O 0.9449(3) 0.10825(17) 0.24364(19) 0.0566(12) Uani 1 1 d . . . . .
O11P O 1.1142(4) 0.1367(3) 0.2533(2) 0.0820(17) Uani 1 1 d . . . . .
O12P O 1.0239(5) 0.1755(3) 0.1898(3) 0.101(2) Uani 1 1 d . . . . .
Cl4 Cl 0.35029(10) 0.33328(6) 0.19308(5) 0.0422(3) Uani 1 1 d . . . . .
O13P O 0.4270(3) 0.3437(2) 0.22323(19) 0.0631(13) Uani 1 1 d . . . . .
O14P O 0.2850(4) 0.2890(2) 0.21567(19) 0.0704(14) Uani 1 1 d . . . . .
O15P O 0.4102(4) 0.3130(2) 0.14887(17) 0.0680(13) Uani 1 1 d . . . . .
O16P O 0.2805(4) 0.3854(2) 0.1840(2) 0.0646(13) Uani 1 1 d . . . . .
Cl5 Cl 0.85955(9) 0.45824(4) 0.29972(4) 0.0269(2) Uani 1 1 d . . . . .
O17P O 0.7909(3) 0.46568(17) 0.34553(13) 0.0445(9) Uani 1 1 d . . . . .
O18P O 0.9714(3) 0.46107(17) 0.30554(15) 0.0440(9) Uani 1 1 d . . . . .
O19P O 0.8267(4) 0.50492(17) 0.26688(15) 0.0517(10) Uani 1 1 d . . . . .
O20P O 0.8460(4) 0.40418(16) 0.28087(16) 0.0510(10) Uani 1 1 d . . . . .
Cl6 Cl 0.20287(9) 0.89727(5) 0.12511(4) 0.0330(2) Uani 1 1 d . . . . .
O21P O 0.2005(3) 0.90188(16) 0.17642(13) 0.0441(9) Uani 1 1 d . . . . .
O22P O 0.0940(3) 0.91269(18) 0.11406(17) 0.0546(11) Uani 1 1 d . . . . .
O23P O 0.2346(3) 0.83794(17) 0.11319(15) 0.0515(10) Uani 1 1 d . . . . .
O24P O 0.2790(4) 0.9331(2) 0.09887(16) 0.0695(14) Uani 1 1 d . . . . .
Cl7 Cl 0.70812(9) 0.89350(5) 0.11501(4) 0.0317(2) Uani 1 1 d D . . . .
O25P O 0.6784(4) 0.9059(3) 0.16445(14) 0.0728(16) Uani 1 1 d D . . . .
O26P O 0.6327(8) 0.9198(4) 0.0837(4) 0.046(2) Uani 0.75(2) 1 d D U P A 1
O27P O 0.8128(6) 0.9128(5) 0.0983(3) 0.055(2) Uani 0.75(2) 1 d D U P A 1
O28P O 0.7130(13) 0.8318(3) 0.1124(4) 0.083(4) Uani 0.75(2) 1 d D U P A 1
O26A O 0.6018(12) 0.9025(9) 0.0998(8) 0.027(4) Uani 0.25(2) 1 d D U P A 2
O27A O 0.776(3) 0.9380(12) 0.0975(8) 0.052(6) Uani 0.25(2) 1 d D U P A 2
O28A O 0.7606(18) 0.8385(8) 0.1028(9) 0.053(7) Uani 0.25(2) 1 d D U P A 2
Cl8 Cl 0.2909(2) 0.53940(7) 0.02727(5) 0.0750(6) Uani 1 1 d D . . . .
O29P O 0.2983(16) 0.5111(8) -0.0169(5) 0.059(6) Uani 0.547(10) 1 d D U P B 1
O30P O 0.2677(11) 0.5969(4) 0.0231(5) 0.057(4) Uani 0.547(10) 1 d D U P B 1
O31P O 0.2635(9) 0.5054(6) 0.0683(4) 0.058(3) Uani 0.547(10) 1 d D U P B 1
O32P O 0.4202(6) 0.5345(4) 0.0301(4) 0.083(4) Uani 0.547(10) 1 d D U P B 1
O29A O 0.2635(19) 0.5064(9) -0.0098(6) 0.043(4) Uani 0.453(10) 1 d D U P B 2
O30A O 0.3128(12) 0.5959(5) 0.0132(7) 0.055(4) Uani 0.453(10) 1 d D U P B 2
O31A O 0.3102(12) 0.5106(6) 0.0689(4) 0.055(4) Uani 0.453(10) 1 d D U P B 2
O32A O 0.1599(6) 0.5605(5) 0.0458(4) 0.063(3) Uani 0.453(10) 1 d D U P B 2
Cl9 Cl 0.4977(2) 0.52065(10) 0.51656(9) 0.0363(5) Uani 0.5 1 d D U P . .
O33P O 0.4467(3) 0.53278(17) 0.47621(14) 0.0467(9) Uani 1 1 d D U . . .
O34P O 0.5722(8) 0.5637(4) 0.5154(3) 0.063(2) Uani 0.5 1 d D U P . .
O35P O 0.4163(8) 0.5304(4) 0.5586(3) 0.064(2) Uani 0.5 1 d D U P . .
Cl12 Cl 1.5287(6) 0.0982(2) 0.39391(19) 0.120(2) Uani 0.5 1 d D U P C 1
O45P O 1.5354(5) 0.0952(2) 0.3503(2) 0.0247(12) Uiso 0.5 1 d D U P C 1
O46P O 1.4928(16) 0.1587(6) 0.3993(7) 0.171(7) Uiso 0.5 1 d D U P C 1
O47P O 1.6203(15) 0.0942(11) 0.4149(8) 0.254(12) Uiso 0.5 1 d D U P C 1
O48P O 1.4514(9) 0.0714(5) 0.4260(4) 0.081(3) Uiso 0.5 1 d D U P C 1
O15W O 1.614(2) 0.0149(13) 0.4183(10) 0.217(11) Uiso 0.5 1 d . . P D 2
Cl10 Cl 1.2483(2) 0.14515(12) 0.41619(10) 0.0388(6) Uani 0.4548(18) 1 d D U P C
.
O37P O 1.2411(9) 0.1018(5) 0.3831(4) 0.092(4) Uani 0.4548(18) 1 d D U P . .
O38P O 1.3573(6) 0.1643(4) 0.4063(3) 0.053(2) Uani 0.4548(18) 1 d D U P . .
O39P O 1.1690(7) 0.1915(4) 0.4080(3) 0.058(2) Uani 0.4548(18) 1 d D U P . .
O40P O 1.2392(7) 0.1298(4) 0.4666(3) 0.056(2) Uani 0.4548(18) 1 d D U P . .
Cl11 Cl 0.8234(3) 0.05032(11) 0.49582(9) 0.0649(9) Uani 0.5453(18) 1 d D U P .
.
O41P O 0.8748(10) 0.0305(4) 0.5370(3) 0.096(3) Uani 0.5453(18) 1 d D U P E .
O42P O 0.7560(11) 0.0983(5) 0.5036(6) 0.057(3) Uani 0.323(3) 1 d D U P E 1
O43P O 0.9214(10) 0.0657(5) 0.4595(4) 0.066(2) Uani 0.323(3) 1 d D U P E 1
O44P O 0.7958(13) 0.0025(6) 0.4768(5) 0.080(3) Uani 0.323(3) 1 d D U P E 1
O42A O 0.789(2) 0.1104(6) 0.5015(10) 0.057(3) Uani 0.222(3) 1 d D U P E 2
O43A O 0.8221(19) 0.0330(8) 0.4503(5) 0.066(2) Uani 0.222(3) 1 d D U P E 2
O44A O 0.7184(14) 0.0287(9) 0.5203(7) 0.080(3) Uani 0.222(3) 1 d D U P E 2
O1W O -0.0860(3) 0.7827(2) 0.34739(17) 0.0685(14) Uani 1 1 d . . . . .
O2W O 0.5582(4) 0.7676(3) 0.3330(3) 0.102(2) Uani 1 1 d . . . . .
O3W O 0.3960(3) 0.1934(2) 0.12614(19) 0.0620(12) Uani 1 1 d . . . . .
O4W O 0.2176(5) 0.1422(3) 0.1064(2) 0.0910(18) Uani 1 1 d . . . . .
O5W O -0.2867(7) 0.8464(3) 0.3408(3) 0.133(3) Uani 1 1 d . . . . .
O6W O 1.2009(8) 0.2431(5) 0.4254(3) 0.075(3) Uani 0.5453(18) 1 d . . P C .
O7W O 1.1082(11) 0.0870(5) 0.4275(5) 0.080(3) Uani 0.4548(18) 1 d . . P . .
O8W O 1.2318(12) 0.0992(6) 0.0182(5) 0.216(5) Uiso 1 1 d . . . . .
O10W O 0.7310(12) 0.0224(7) 0.0364(5) 0.110(4) Uiso 0.5 1 d . . P . .
O11W O 1.3942(17) 0.0048(9) 0.0106(8) 0.159(7) Uiso 0.5 1 d . . P . .
O12W O -0.2809(18) 0.8985(10) 0.4166(8) 0.171(8) Uiso 0.5 1 d . . P . .
O13W O 0.9300(12) 0.0369(6) -0.0215(5) 0.097(4) Uiso 0.5 1 d . . P . .
O14W O 0.8383(15) 0.0307(7) -0.0075(6) 0.123(5) Uiso 0.5 1 d . . P . .
O1S O 1.0375(3) 0.23549(19) 0.09393(17) 0.0577(12) Uani 1 1 d D . . . .
H1SA H 0.9710 0.2475 0.0946 0.087 Uiso 1 1 calc R U . . .
C1S C 1.1020(5) 0.2656(3) 0.0549(2) 0.0597(17) Uani 1 1 d D . . . .
H1SB H 1.1194 0.2402 0.0272 0.072 Uiso 1 1 calc R U . . .
H1SC H 1.0564 0.3004 0.0445 0.072 Uiso 1 1 calc R U . . .
C2S C 1.2020(5) 0.2832(3) 0.0653(3) 0.0640(18) Uani 1 1 d D . . . .
H2SA H 1.2397 0.3026 0.0363 0.096 Uiso 1 1 calc R U . . .
H2SB H 1.2490 0.2492 0.0751 0.096 Uiso 1 1 calc R U . . .
H2SC H 1.1862 0.3100 0.0915 0.096 Uiso 1 1 calc R U . . .
O2S O 0.0818(3) 0.53924(18) 0.23043(15) 0.0505(10) Uani 1 1 d . . . . .
H2SD H 0.0517 0.5178 0.2527 0.076 Uiso 1 1 calc R U . . .
C3S C 0.0580(7) 0.5239(3) 0.1855(3) 0.073(2) Uani 1 1 d . . . . .
H3SA H 0.0245 0.4869 0.1898 0.087 Uiso 1 1 calc R U . . .
H3SB H 0.1266 0.5187 0.1623 0.087 Uiso 1 1 calc R U . . .
C4S C -0.0219(8) 0.5720(5) 0.1652(4) 0.103(3) Uani 1 1 d . . . . .
H4SA H -0.0384 0.5610 0.1341 0.154 Uiso 1 1 calc R U . . .
H4SB H 0.0120 0.6084 0.1605 0.154 Uiso 1 1 calc R U . . .
H4SC H -0.0899 0.5769 0.1881 0.154 Uiso 1 1 calc R U . . .
O3S O 0.6851(4) 0.61257(19) 0.04001(17) 0.0646(13) Uani 1 1 d . . . . .
H3SC H 0.6887 0.5787 0.0309 0.097 Uiso 1 1 calc R U . . .
C5S C 0.7728(6) 0.6171(3) 0.0670(3) 0.0614(17) Uani 1 1 d . . . . .
H5SA H 0.8439 0.6048 0.0474 0.074 Uiso 1 1 calc R U . . .
H5SB H 0.7643 0.5916 0.0968 0.074 Uiso 1 1 calc R U . . .
C6S C 0.7701(8) 0.6790(4) 0.0797(3) 0.083(2) Uani 1 1 d . . . . .
H6SA H 0.8295 0.6826 0.0984 0.124 Uiso 1 1 calc R U . . .
H6SB H 0.6995 0.6908 0.0991 0.124 Uiso 1 1 calc R U . . .
H6SC H 0.7795 0.7038 0.0500 0.124 Uiso 1 1 calc R U . . .
O4S O 0.1518(4) 0.2957(2) 0.3472(2) 0.0825(16) Uani 1 1 d D U . . .
H4SD H 0.1578 0.2692 0.3278 0.124 Uiso 0.501(11) 1 calc R U P F 1
H4SE H 0.1142 0.2748 0.3674 0.124 Uiso 0.499(11) 1 calc R U P F 2
C7SA C 0.1946(11) 0.3473(5) 0.3217(5) 0.056(3) Uani 0.501(11) 1 d D U P F 1
H7SA H 0.2688 0.3311 0.3076 0.068 Uiso 0.501(11) 1 calc R U P F 1
H7SB H 0.1526 0.3521 0.2941 0.068 Uiso 0.501(11) 1 calc R U P F 1
C8SA C 0.2088(10) 0.3916(5) 0.3255(6) 0.058(4) Uani 0.501(11) 1 d D U P F 1
H8SX H 0.2417 0.4081 0.2942 0.087 Uiso 0.501(11) 1 calc R U P F 1
H8SY H 0.2585 0.3927 0.3494 0.087 Uiso 0.501(11) 1 calc R U P F 1
H8SZ H 0.1389 0.4141 0.3364 0.087 Uiso 0.501(11) 1 calc R U P F 1
C7SB C 0.1612(12) 0.3499(5) 0.3684(6) 0.071(4) Uani 0.499(11) 1 d D U P F 2
H7SC H 0.0834 0.3625 0.3801 0.085 Uiso 0.499(11) 1 calc R U P F 2
H7SD H 0.1925 0.3358 0.3980 0.085 Uiso 0.499(11) 1 calc R U P F 2
C8SB C 0.1946(11) 0.3909(5) 0.3605(6) 0.055(3) Uani 0.499(11) 1 d D U P F 2
H8SR H 0.1723 0.4152 0.3882 0.082 Uiso 0.499(11) 1 calc R U P F 2
H8SS H 0.1673 0.4103 0.3319 0.082 Uiso 0.499(11) 1 calc R U P F 2
H8ST H 0.2748 0.3845 0.3543 0.082 Uiso 0.499(11) 1 calc R U P F 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
Ni1 O1 2.012(3) . ?
Ni1 N2 2.057(3) . ?
Ni1 N15 2.059(3) . ?
Ni1 O4 2.074(3) . ?
Ni1 N1 2.080(4) . ?
Ni1 N16 2.090(3) . ?
Ni2 O1 2.004(3) . ?
Ni2 N6 2.057(4) . ?
Ni2 N3 2.066(3) . ?
Ni2 N5 2.078(4) . ?
Ni2 N4 2.093(4) . ?
Ni2 O2 2.096(3) . ?
Ni3 O3 2.017(3) . ?
Ni3 N10 2.049(4) . ?
Ni3 N7 2.065(4) . ?
Ni3 N8 2.075(4) . ?
Ni3 N9 2.089(4) . ?
Ni3 O2 2.095(3) . ?
Ni4 O3 2.024(3) . ?
Ni4 N11 2.064(3) . ?
Ni4 N14 2.074(3) . ?
Ni4 O4 2.075(3) . ?
Ni4 N13 2.087(3) . ?
Ni4 N12 2.099(4) . ?
N1 C1 1.334(6) . ?
N1 C5 1.366(5) . ?
C1 C2 1.389(7) . ?
C2 C3 1.381(7) . ?
C3 C4 1.398(7) . ?
C4 C5 1.378(6) . ?
C5 C6 1.481(6) . ?
C6 N2 1.331(5) . ?
C6 C7 1.408(6) . ?
N2 N3 1.327(5) . ?
C7 C8 1.374(6) . ?
C8 C9 1.402(6) . ?
C9 N3 1.333(5) . ?
C9 C10 1.487(6) . ?
C10 N4 1.359(6) . ?
C10 C11 1.378(7) . ?
C11 C12 1.378(8) . ?
C12 C13 1.388(10) . ?
C13 C14 1.373(8) . ?
C14 N4 1.337(6) . ?
N5 C15 1.339(6) . ?
N5 C19 1.349(6) . ?
C15 C16 1.392(7) . ?
C16 C17 1.375(8) . ?
C17 C18 1.371(8) . ?
C18 C19 1.395(7) . ?
C19 C20 1.478(7) . ?
C20 N6 1.343(6) . ?
C20 C21 1.399(7) . ?
N6 N7 1.332(5) . ?
C21 C22 1.372(8) . ?
C22 C23 1.406(7) . ?
C23 N7 1.336(6) . ?
C23 C24 1.482(7) . ?
C24 N8 1.348(6) . ?
C24 C25 1.381(7) . ?
C25 C26 1.381(9) . ?
C26 C27 1.377(9) . ?
C27 C28 1.378(7) . ?
C28 N8 1.339(6) . ?
N9 C29 1.328(7) . ?
N9 C33 1.354(6) . ?
C29 C30 1.387(8) . ?
C30 C31 1.353(11) . ?
C31 C32 1.392(9) . ?
C32 C33 1.380(7) . ?
C33 C34 1.476(6) . ?
C34 N10 1.331(6) . ?
C34 C35 1.404(6) . ?
N10 N11 1.336(5) . ?
C35 C36 1.368(7) . ?
C36 C37 1.409(6) . ?
C37 N11 1.329(5) . ?
C37 C38 1.481(6) . ?
C38 N12 1.354(6) . ?
C38 C39 1.382(6) . ?
C39 C40 1.380(7) . ?
C40 C41 1.389(7) . ?
C41 C42 1.385(7) . ?
C42 N12 1.333(6) . ?
N13 C43 1.339(6) . ?
N13 C47 1.355(5) . ?
C43 C44 1.380(7) . ?
C44 C45 1.385(7) . ?
C45 C46 1.388(7) . ?
C46 C47 1.376(6) . ?
C47 C48 1.490(6) . ?
C48 N14 1.329(5) . ?
C48 C49 1.402(6) . ?
N14 N15 1.330(5) . ?
C49 C50 1.360(6) . ?
C50 C51 1.397(6) . ?
C51 N15 1.338(5) . ?
C51 C52 1.491(6) . ?
C52 N16 1.353(5) . ?
C52 C53 1.382(6) . ?
C53 C54 1.395(7) . ?
C54 C55 1.373(7) . ?
C55 C56 1.390(7) . ?
C56 N16 1.336(6) . ?
Ni5 O5 2.022(3) . ?
Ni5 N31 2.061(4) . ?
Ni5 N18 2.064(4) . ?
Ni5 N32 2.084(4) . ?
Ni5 N17 2.085(4) . ?
Ni5 O8 2.100(3) . ?
Ni6 O5 2.033(3) . ?
Ni6 O6 2.063(3) . ?
Ni6 N22 2.065(4) . ?
Ni6 N19 2.066(4) . ?
Ni6 N20 2.091(4) . ?
Ni6 N21 2.092(4) . ?
Ni7 O7 2.015(3) . ?
Ni7 O6 2.063(3) . ?
Ni7 N26 2.071(4) . ?
Ni7 N23 2.074(4) . ?
Ni7 N25 2.086(4) . ?
Ni7 N24 2.109(4) . ?
Ni8 O7 2.016(3) . ?
Ni8 N27 2.062(4) . ?
Ni8 N30 2.064(4) . ?
Ni8 O8 2.092(3) . ?
Ni8 N28 2.092(4) . ?
Ni8 N29 2.096(4) . ?
N17 C57 1.339(6) . ?
N17 C61 1.357(7) . ?
C57 C58 1.399(7) . ?
C58 C59 1.360(9) . ?
C59 C60 1.383(9) . ?
C60 C61 1.385(7) . ?
C61 C62 1.491(8) . ?
N18 C62 1.328(6) . ?
N18 N19 1.331(5) . ?
C62 C63 1.409(8) . ?
C63 C64 1.360(9) . ?
C64 C65 1.396(7) . ?
C65 N19 1.331(6) . ?
C65 C66 1.479(7) . ?
C66 N20 1.356(6) . ?
C66 C67 1.391(7) . ?
C67 C68 1.385(8) . ?
C68 C69 1.378(8) . ?
C69 C70 1.388(7) . ?
C70 N20 1.340(6) . ?
N21 C71 1.330(6) . ?
N21 C75 1.355(6) . ?
C71 C72 1.385(7) . ?
C72 C73 1.383(7) . ?
C73 C74 1.390(7) . ?
C74 C75 1.383(6) . ?
C75 C76 1.488(6) . ?
N22 C76 1.330(6) . ?
N22 N23 1.334(5) . ?
C76 C77 1.386(6) . ?
C77 C78 1.366(7) . ?
C78 C79 1.404(7) . ?
C79 N23 1.322(6) . ?
C79 C80 1.489(6) . ?
C80 N24 1.350(6) . ?
C80 C81 1.389(7) . ?
C81 C82 1.388(7) . ?
C82 C83 1.364(8) . ?
C83 C84 1.384(8) . ?
C84 N24 1.336(6) . ?
N25 C85 1.340(7) . ?
N25 C89 1.347(7) . ?
C85 C86 1.406(8) . ?
C86 C87 1.379(10) . ?
C87 C88 1.384(9) . ?
C88 C89 1.387(7) . ?
C89 C90 1.482(7) . ?
N26 N27 1.321(6) . ?
N26 C90 1.341(6) . ?
C90 C91 1.393(7) . ?
C91 C92 1.370(8) . ?
C92 C93 1.396(7) . ?
C93 N27 1.338(6) . ?
C93 C94 1.474(8) . ?
C94 N28 1.359(7) . ?
C94 C95 1.390(7) . ?
C95 C96 1.384(10) . ?
C96 C97 1.388(10) . ?
C97 C98 1.386(7) . ?
C98 N28 1.343(7) . ?
N29 C99 1.333(6) . ?
N29 C103 1.354(6) . ?
C99 C100 1.390(7) . ?
C100 C101 1.380(7) . ?
C101 C102 1.382(7) . ?
C102 C103 1.392(6) . ?
C103 C104 1.477(6) . ?
N30 N31 1.331(5) . ?
N30 C104 1.334(6) . ?
C104 C105 1.405(6) . ?
C105 C106 1.362(7) . ?
C106 C107 1.399(6) . ?
C107 N31 1.339(6) . ?
C107 C108 1.481(6) . ?
C108 N32 1.364(6) . ?
C108 C109 1.384(7) . ?
C109 C110 1.389(7) . ?
C110 C111 1.370(8) . ?
C111 C112 1.382(8) . ?
C112 N32 1.342(6) . ?
Cl1 O4P 1.416(4) . ?
Cl1 O3P 1.427(4) . ?
Cl1 O2P 1.439(4) . ?
Cl1 O1P 1.443(3) . ?
Cl2 O7P 1.367(5) . ?
Cl2 O6P 1.379(5) . ?
Cl2 O8P 1.427(6) . ?
Cl2 O5P 1.438(3) . ?
Cl3 O10P 1.405(4) . ?
Cl3 O12P 1.432(6) . ?
Cl3 O11P 1.438(5) . ?
Cl3 O9P 1.440(5) . ?
Cl4 O13P 1.416(4) . ?
Cl4 O15P 1.425(5) . ?
Cl4 O14P 1.434(5) . ?
Cl4 O16P 1.443(5) . ?
Cl5 O18P 1.431(4) . ?
Cl5 O20P 1.435(4) . ?
Cl5 O17P 1.437(4) . ?
Cl5 O19P 1.440(4) . ?
Cl6 O24P 1.415(4) . ?
Cl6 O22P 1.433(4) . ?
Cl6 O23P 1.443(4) . ?
Cl6 O21P 1.444(4) . ?
Cl7 O28A 1.412(12) . ?
Cl7 O25P 1.418(4) . ?
Cl7 O27P 1.422(6) . ?
Cl7 O27A 1.423(12) . ?
Cl7 O26A 1.437(11) . ?
Cl7 O28P 1.438(6) . ?
Cl7 O26P 1.440(6) . ?
Cl8 O30P 1.339(8) . ?
Cl8 O31A 1.344(10) . ?
Cl8 O31P 1.370(9) . ?
Cl8 O30A 1.390(11) . ?
Cl8 O29P 1.429(9) . ?
Cl8 O29A 1.435(10) . ?
Cl8 O32P 1.609(7) . ?
Cl8 O32A 1.660(8) . ?
Cl9 O33P 1.373(4) 2_666 ?
Cl9 Cl9 1.373(5) 2_666 ?
Cl9 O33P 1.376(4) . ?
Cl9 O34P 1.432(7) . ?
Cl9 O35P 1.443(8) . ?
O33P Cl9 1.373(4) 2_666 ?
Cl12 O45P 1.218(7) . ?
Cl12 O47P 1.350(14) . ?
Cl12 O48P 1.381(10) . ?
Cl12 O46P 1.440(14) . ?
O46P O38P 1.65(2) . ?
Cl10 O39P 1.410(8) . ?
Cl10 O40P 1.422(8) . ?
Cl10 O37P 1.435(9) . ?
Cl10 O38P 1.452(8) . ?
O39P O6W 1.444(14) . ?
Cl11 O42P 1.330(10) . ?
Cl11 O44P 1.367(10) . ?
Cl11 O43A 1.368(12) . ?
Cl11 O41P 1.426(8) . ?
Cl11 O42A 1.429(12) . ?
Cl11 O44A 1.498(13) . ?
Cl11 O43P 1.519(11) . ?
O10W O14W 1.69(2) . ?
O13W O14W 1.167(19) . ?
O1S C1S 1.440(7) . ?
C1S C2S 1.426(9) . ?
O2S C3S 1.413(8) . ?
C3S C4S 1.549(13) . ?
O3S C5S 1.433(8) . ?
C5S C6S 1.505(11) . ?
O4S C7SB 1.456(12) . ?
O4S C7SA 1.462(11) . ?
C7SA C8SA 1.081(13) . ?
C7SB C8SB 1.078(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 N2 91.35(12) . . ?
O1 Ni1 N15 89.02(12) . . ?
N2 Ni1 N15 178.87(14) . . ?
O1 Ni1 O4 85.34(11) . . ?
N2 Ni1 O4 89.35(12) . . ?
N15 Ni1 O4 91.75(12) . . ?
O1 Ni1 N1 168.78(13) . . ?
N2 Ni1 N1 77.59(14) . . ?
N15 Ni1 N1 102.08(14) . . ?
O4 Ni1 N1 92.58(12) . . ?
O1 Ni1 N16 93.71(13) . . ?
N2 Ni1 N16 100.73(13) . . ?
N15 Ni1 N16 78.18(13) . . ?
O4 Ni1 N16 169.90(12) . . ?
N1 Ni1 N16 90.24(14) . . ?
O1 Ni2 N6 89.79(13) . . ?
O1 Ni2 N3 91.05(13) . . ?
N6 Ni2 N3 179.13(15) . . ?
O1 Ni2 N5 91.73(13) . . ?
N6 Ni2 N5 78.18(15) . . ?
N3 Ni2 N5 102.04(14) . . ?
O1 Ni2 N4 168.44(13) . . ?
N6 Ni2 N4 101.74(14) . . ?
N3 Ni2 N4 77.43(14) . . ?
N5 Ni2 N4 89.85(15) . . ?
O1 Ni2 O2 85.71(11) . . ?
N6 Ni2 O2 91.79(13) . . ?
N3 Ni2 O2 88.02(13) . . ?
N5 Ni2 O2 169.67(13) . . ?
N4 Ni2 O2 94.66(14) . . ?
O3 Ni3 N10 92.17(13) . . ?
O3 Ni3 N7 89.59(13) . . ?
N10 Ni3 N7 177.88(14) . . ?
O3 Ni3 N8 95.23(13) . . ?
N10 Ni3 N8 100.19(15) . . ?
N7 Ni3 N8 78.47(15) . . ?
O3 Ni3 N9 169.37(14) . . ?
N10 Ni3 N9 77.21(14) . . ?
N7 Ni3 N9 101.02(15) . . ?
N8 Ni3 N9 86.44(15) . . ?
O3 Ni3 O2 87.21(11) . . ?
N10 Ni3 O2 89.88(13) . . ?
N7 Ni3 O2 91.38(13) . . ?
N8 Ni3 O2 169.53(13) . . ?
N9 Ni3 O2 93.04(13) . . ?
O3 Ni4 N11 91.63(13) . . ?
O3 Ni4 N14 89.90(12) . . ?
N11 Ni4 N14 178.47(14) . . ?
O3 Ni4 O4 86.84(11) . . ?
N11 Ni4 O4 89.04(12) . . ?
N14 Ni4 O4 91.03(12) . . ?
O3 Ni4 N13 92.33(13) . . ?
N11 Ni4 N13 102.16(14) . . ?
N14 Ni4 N13 77.78(13) . . ?
O4 Ni4 N13 168.79(12) . . ?
O3 Ni4 N12 168.58(13) . . ?
N11 Ni4 N12 76.98(14) . . ?
N14 Ni4 N12 101.49(14) . . ?
O4 Ni4 N12 92.02(12) . . ?
N13 Ni4 N12 90.96(13) . . ?
Ni2 O1 Ni1 115.14(13) . . ?
Ni3 O2 Ni2 112.19(13) . . ?
Ni3 O3 Ni4 113.34(13) . . ?
Ni1 O4 Ni4 113.40(12) . . ?
C1 N1 C5 118.4(4) . . ?
C1 N1 Ni1 125.8(3) . . ?
C5 N1 Ni1 115.5(3) . . ?
N1 C1 C2 123.0(4) . . ?
C3 C2 C1 118.3(4) . . ?
C2 C3 C4 119.6(4) . . ?
C5 C4 C3 118.6(4) . . ?
N1 C5 C4 122.0(4) . . ?
N1 C5 C6 114.2(4) . . ?
C4 C5 C6 123.7(4) . . ?
N2 C6 C7 121.0(4) . . ?
N2 C6 C5 113.9(4) . . ?
C7 C6 C5 125.0(4) . . ?
N3 N2 C6 121.1(3) . . ?
N3 N2 Ni1 119.9(3) . . ?
C6 N2 Ni1 117.9(3) . . ?
C8 C7 C6 117.7(4) . . ?
C7 C8 C9 118.4(4) . . ?
N3 C9 C8 120.9(4) . . ?
N3 C9 C10 113.8(4) . . ?
C8 C9 C10 125.3(4) . . ?
N2 N3 C9 120.8(3) . . ?
N2 N3 Ni2 120.1(3) . . ?
C9 N3 Ni2 117.7(3) . . ?
N4 C10 C11 122.3(5) . . ?
N4 C10 C9 114.3(4) . . ?
C11 C10 C9 123.4(4) . . ?
C12 C11 C10 118.7(5) . . ?
C11 C12 C13 119.4(6) . . ?
C14 C13 C12 118.7(6) . . ?
N4 C14 C13 122.9(5) . . ?
C14 N4 C10 118.0(4) . . ?
C14 N4 Ni2 125.9(3) . . ?
C10 N4 Ni2 115.4(3) . . ?
C15 N5 C19 119.0(4) . . ?
C15 N5 Ni2 125.7(3) . . ?
C19 N5 Ni2 115.3(3) . . ?
N5 C15 C16 122.0(4) . . ?
C17 C16 C15 118.7(5) . . ?
C18 C17 C16 119.9(5) . . ?
C17 C18 C19 119.0(5) . . ?
N5 C19 C18 121.4(5) . . ?
N5 C19 C20 115.2(4) . . ?
C18 C19 C20 123.3(4) . . ?
N6 C20 C21 120.8(5) . . ?
N6 C20 C19 114.2(4) . . ?
C21 C20 C19 124.9(4) . . ?
N7 N6 C20 120.7(4) . . ?
N7 N6 Ni2 121.4(3) . . ?
C20 N6 Ni2 116.6(3) . . ?
C22 C21 C20 118.1(5) . . ?
C21 C22 C23 119.0(5) . . ?
N7 C23 C22 120.0(5) . . ?
N7 C23 C24 114.8(4) . . ?
C22 C23 C24 125.2(4) . . ?
N6 N7 C23 121.3(4) . . ?
N6 N7 Ni3 121.2(3) . . ?
C23 N7 Ni3 115.5(3) . . ?
N8 C24 C25 122.1(5) . . ?
N8 C24 C23 114.5(4) . . ?
C25 C24 C23 123.4(5) . . ?
C24 C25 C26 118.7(5) . . ?
C27 C26 C25 119.4(5) . . ?
C26 C27 C28 118.8(5) . . ?
N8 C28 C27 122.5(5) . . ?
C28 N8 C24 118.4(4) . . ?
C28 N8 Ni3 125.7(3) . . ?
C24 N8 Ni3 115.1(3) . . ?
C29 N9 C33 118.3(4) . . ?
C29 N9 Ni3 125.3(3) . . ?
C33 N9 Ni3 115.4(3) . . ?
N9 C29 C30 122.4(6) . . ?
C31 C30 C29 119.1(6) . . ?
C30 C31 C32 119.8(6) . . ?
C33 C32 C31 118.0(6) . . ?
N9 C33 C32 122.3(5) . . ?
N9 C33 C34 114.4(4) . . ?
C32 C33 C34 123.3(5) . . ?
N10 C34 C35 121.0(4) . . ?
N10 C34 C33 113.7(4) . . ?
C35 C34 C33 125.2(4) . . ?
C34 N10 N11 120.8(4) . . ?
C34 N10 Ni3 118.3(3) . . ?
N11 N10 Ni3 119.7(3) . . ?
C36 C35 C34 118.1(4) . . ?
C35 C36 C37 118.1(4) . . ?
N11 C37 C36 120.9(4) . . ?
N11 C37 C38 114.0(4) . . ?
C36 C37 C38 124.9(4) . . ?
C37 N11 N10 120.7(4) . . ?
C37 N11 Ni4 118.3(3) . . ?
N10 N11 Ni4 119.8(3) . . ?
N12 C38 C39 121.7(4) . . ?
N12 C38 C37 114.7(4) . . ?
C39 C38 C37 123.5(4) . . ?
C40 C39 C38 119.4(5) . . ?
C39 C40 C41 118.9(5) . . ?
C42 C41 C40 118.7(5) . . ?
N12 C42 C41 122.6(4) . . ?
C42 N12 C38 118.7(4) . . ?
C42 N12 Ni4 125.6(3) . . ?
C38 N12 Ni4 115.7(3) . . ?
C43 N13 C47 118.0(4) . . ?
C43 N13 Ni4 126.6(3) . . ?
C47 N13 Ni4 115.4(3) . . ?
N13 C43 C44 122.9(4) . . ?
C43 C44 C45 119.0(4) . . ?
C44 C45 C46 118.6(4) . . ?
C47 C46 C45 119.4(5) . . ?
N13 C47 C46 122.2(4) . . ?
N13 C47 C48 114.8(4) . . ?
C46 C47 C48 123.0(4) . . ?
N14 C48 C49 121.7(4) . . ?
N14 C48 C47 114.4(4) . . ?
C49 C48 C47 123.8(4) . . ?
C48 N14 N15 120.2(3) . . ?
C48 N14 Ni4 117.0(3) . . ?
N15 N14 Ni4 121.5(3) . . ?
C50 C49 C48 117.8(4) . . ?
C49 C50 C51 118.6(4) . . ?
N15 C51 C50 120.8(4) . . ?
N15 C51 C52 114.4(4) . . ?
C50 C51 C52 124.7(4) . . ?
N14 N15 C51 120.8(3) . . ?
N14 N15 Ni1 120.8(2) . . ?
C51 N15 Ni1 116.8(3) . . ?
N16 C52 C53 122.1(4) . . ?
N16 C52 C51 114.8(4) . . ?
C53 C52 C51 123.1(4) . . ?
C52 C53 C54 118.5(4) . . ?
C55 C54 C53 119.4(4) . . ?
C54 C55 C56 119.0(4) . . ?
N16 C56 C55 122.2(4) . . ?
C56 N16 C52 118.8(4) . . ?
C56 N16 Ni1 126.0(3) . . ?
C52 N16 Ni1 115.2(3) . . ?
O5 Ni5 N31 90.11(13) . . ?
O5 Ni5 N18 91.16(13) . . ?
N31 Ni5 N18 178.38(15) . . ?
O5 Ni5 N32 93.30(14) . . ?
N31 Ni5 N32 78.10(15) . . ?
N18 Ni5 N32 102.83(16) . . ?
O5 Ni5 N17 169.28(14) . . ?
N31 Ni5 N17 100.59(15) . . ?
N18 Ni5 N17 78.13(16) . . ?
N32 Ni5 N17 89.62(16) . . ?
O5 Ni5 O8 86.72(12) . . ?
N31 Ni5 O8 91.68(13) . . ?
N18 Ni5 O8 87.39(14) . . ?
N32 Ni5 O8 169.77(14) . . ?
N17 Ni5 O8 92.24(15) . . ?
O5 Ni6 O6 86.78(12) . . ?
O5 Ni6 N22 89.85(13) . . ?
O6 Ni6 N22 90.48(13) . . ?
O5 Ni6 N19 91.05(13) . . ?
O6 Ni6 N19 89.58(14) . . ?
N22 Ni6 N19 179.10(15) . . ?
O5 Ni6 N20 168.51(14) . . ?
O6 Ni6 N20 93.28(13) . . ?
N22 Ni6 N20 101.63(15) . . ?
N19 Ni6 N20 77.46(15) . . ?
O5 Ni6 N21 93.61(13) . . ?
O6 Ni6 N21 168.34(13) . . ?
N22 Ni6 N21 77.87(14) . . ?
N19 Ni6 N21 102.06(15) . . ?
N20 Ni6 N21 88.65(14) . . ?
O7 Ni7 O6 86.01(13) . . ?
O7 Ni7 N26 90.13(14) . . ?
O6 Ni7 N26 89.32(14) . . ?
O7 Ni7 N23 91.19(13) . . ?
O6 Ni7 N23 90.23(13) . . ?
N26 Ni7 N23 178.57(15) . . ?
O7 Ni7 N25 167.47(15) . . ?
O6 Ni7 N25 92.97(14) . . ?
N26 Ni7 N25 77.37(16) . . ?
N23 Ni7 N25 101.30(16) . . ?
O7 Ni7 N24 96.81(14) . . ?
O6 Ni7 N24 167.62(14) . . ?
N26 Ni7 N24 102.70(16) . . ?
N23 Ni7 N24 77.68(15) . . ?
N25 Ni7 N24 86.85(16) . . ?
O7 Ni8 N27 90.12(14) . . ?
O7 Ni8 N30 91.56(13) . . ?
N27 Ni8 N30 178.30(15) . . ?
O7 Ni8 O8 85.70(13) . . ?
N27 Ni8 O8 88.05(14) . . ?
N30 Ni8 O8 91.87(14) . . ?
O7 Ni8 N28 167.72(15) . . ?
N27 Ni8 N28 77.62(16) . . ?
N30 Ni8 N28 100.69(15) . . ?
O8 Ni8 N28 93.00(14) . . ?
O7 Ni8 N29 97.41(14) . . ?
N27 Ni8 N29 102.31(15) . . ?
N30 Ni8 N29 77.67(15) . . ?
O8 Ni8 N29 169.13(14) . . ?
N28 Ni8 N29 86.13(15) . . ?
Ni5 O5 Ni6 114.42(13) . . ?
Ni6 O6 Ni7 115.03(13) . . ?
Ni7 O7 Ni8 116.06(14) . . ?
Ni8 O8 Ni5 112.04(14) . . ?
C57 N17 C61 118.8(4) . . ?
C57 N17 Ni5 126.2(3) . . ?
C61 N17 Ni5 114.9(3) . . ?
N17 C57 C58 121.9(5) . . ?
C59 C58 C57 119.0(5) . . ?
C58 C59 C60 119.8(5) . . ?
C59 C60 C61 119.1(5) . . ?
N17 C61 C60 121.4(5) . . ?
N17 C61 C62 114.8(4) . . ?
C60 C61 C62 123.7(5) . . ?
C62 N18 N19 120.6(4) . . ?
C62 N18 Ni5 116.9(3) . . ?
N19 N18 Ni5 120.6(3) . . ?
N18 C62 C63 120.8(5) . . ?
N18 C62 C61 114.2(5) . . ?
C63 C62 C61 124.9(5) . . ?
C64 C63 C62 118.5(5) . . ?
C63 C64 C65 118.0(5) . . ?
N19 C65 C64 121.3(5) . . ?
N19 C65 C66 114.2(4) . . ?
C64 C65 C66 124.3(5) . . ?
N18 N19 C65 120.8(4) . . ?
N18 N19 Ni6 119.8(3) . . ?
C65 N19 Ni6 117.0(3) . . ?
N20 C66 C67 122.2(5) . . ?
N20 C66 C65 114.2(4) . . ?
C67 C66 C65 123.5(5) . . ?
C68 C67 C66 118.5(5) . . ?
C69 C68 C67 119.6(5) . . ?
C68 C69 C70 118.7(5) . . ?
N20 C70 C69 122.8(5) . . ?
C70 N20 C66 118.1(4) . . ?
C70 N20 Ni6 126.1(3) . . ?
C66 N20 Ni6 115.4(3) . . ?
C71 N21 C75 117.9(4) . . ?
C71 N21 Ni6 127.0(3) . . ?
C75 N21 Ni6 115.0(3) . . ?
N21 C71 C72 123.5(4) . . ?
C73 C72 C71 118.5(4) . . ?
C72 C73 C74 118.8(4) . . ?
C75 C74 C73 119.2(4) . . ?
N21 C75 C74 122.1(4) . . ?
N21 C75 C76 114.9(4) . . ?
C74 C75 C76 122.9(4) . . ?
C76 N22 N23 120.3(4) . . ?
C76 N22 Ni6 117.0(3) . . ?
N23 N22 Ni6 121.4(3) . . ?
N22 C76 C77 121.5(4) . . ?
N22 C76 C75 114.2(4) . . ?
C77 C76 C75 124.2(4) . . ?
C78 C77 C76 118.3(4) . . ?
C77 C78 C79 117.9(4) . . ?
N23 C79 C78 121.2(4) . . ?
N23 C79 C80 114.6(4) . . ?
C78 C79 C80 124.2(4) . . ?
C79 N23 N22 120.7(4) . . ?
C79 N23 Ni7 116.6(3) . . ?
N22 N23 Ni7 121.1(3) . . ?
N24 C80 C81 122.3(4) . . ?
N24 C80 C79 114.8(4) . . ?
C81 C80 C79 122.9(4) . . ?
C82 C81 C80 118.5(5) . . ?
C83 C82 C81 119.3(5) . . ?
C82 C83 C84 119.2(5) . . ?
N24 C84 C83 122.8(5) . . ?
C84 N24 C80 117.9(4) . . ?
C84 N24 Ni7 126.7(4) . . ?
C80 N24 Ni7 114.6(3) . . ?
C85 N25 C89 118.6(5) . . ?
C85 N25 Ni7 125.1(4) . . ?
C89 N25 Ni7 116.2(3) . . ?
N25 C85 C86 122.1(6) . . ?
C87 C86 C85 118.4(6) . . ?
C86 C87 C88 119.7(6) . . ?
C87 C88 C89 118.7(6) . . ?
N25 C89 C88 122.4(5) . . ?
N25 C89 C90 114.6(4) . . ?
C88 C89 C90 122.9(5) . . ?
N27 N26 C90 121.2(4) . . ?
N27 N26 Ni7 120.3(3) . . ?
C90 N26 Ni7 117.1(3) . . ?
N26 C90 C91 120.7(5) . . ?
N26 C90 C89 114.2(4) . . ?
C91 C90 C89 125.0(4) . . ?
C92 C91 C90 117.7(5) . . ?
C91 C92 C93 119.2(5) . . ?
N27 C93 C92 120.3(5) . . ?
N27 C93 C94 114.3(4) . . ?
C92 C93 C94 125.3(5) . . ?
N26 N27 C93 120.6(4) . . ?
N26 N27 Ni8 120.7(3) . . ?
C93 N27 Ni8 117.3(3) . . ?
N28 C94 C95 121.7(5) . . ?
N28 C94 C93 114.7(4) . . ?
C95 C94 C93 123.5(5) . . ?
C96 C95 C94 118.7(6) . . ?
C95 C96 C97 119.4(5) . . ?
C98 C97 C96 119.3(6) . . ?
N28 C98 C97 121.7(6) . . ?
C98 N28 C94 119.2(4) . . ?
C98 N28 Ni8 125.2(3) . . ?
C94 N28 Ni8 115.1(3) . . ?
C99 N29 C103 118.4(4) . . ?
C99 N29 Ni8 126.1(3) . . ?
C103 N29 Ni8 115.0(3) . . ?
N29 C99 C100 122.8(5) . . ?
C101 C100 C99 118.8(5) . . ?
C100 C101 C102 118.9(5) . . ?
C101 C102 C103 119.3(4) . . ?
N29 C103 C102 121.7(4) . . ?
N29 C103 C104 115.0(4) . . ?
C102 C103 C104 123.2(4) . . ?
N31 N30 C104 120.7(4) . . ?
N31 N30 Ni8 121.0(3) . . ?
C104 N30 Ni8 117.0(3) . . ?
N30 C104 C105 120.9(4) . . ?
N30 C104 C103 114.3(4) . . ?
C105 C104 C103 124.7(4) . . ?
C106 C105 C104 118.4(4) . . ?
C105 C106 C107 118.2(4) . . ?
N31 C107 C106 121.2(4) . . ?
N31 C107 C108 114.6(4) . . ?
C106 C107 C108 124.2(4) . . ?
N30 N31 C107 120.5(4) . . ?
N30 N31 Ni5 121.7(3) . . ?
C107 N31 Ni5 117.0(3) . . ?
N32 C108 C109 122.3(4) . . ?
N32 C108 C107 114.7(4) . . ?
C109 C108 C107 123.0(4) . . ?
C108 C109 C110 118.6(5) . . ?
C111 C110 C109 119.4(5) . . ?
C110 C111 C112 119.2(5) . . ?
N32 C112 C111 122.8(5) . . ?
C112 N32 C108 117.6(4) . . ?
C112 N32 Ni5 127.0(3) . . ?
C108 N32 Ni5 115.3(3) . . ?
O4P Cl1 O3P 112.7(3) . . ?
O4P Cl1 O2P 108.6(3) . . ?
O3P Cl1 O2P 107.1(3) . . ?
O4P Cl1 O1P 110.0(2) . . ?
O3P Cl1 O1P 109.2(2) . . ?
O2P Cl1 O1P 109.1(2) . . ?
O7P Cl2 O6P 115.0(4) . . ?
O7P Cl2 O8P 107.0(6) . . ?
O6P Cl2 O8P 104.1(5) . . ?
O7P Cl2 O5P 111.3(3) . . ?
O6P Cl2 O5P 111.2(3) . . ?
O8P Cl2 O5P 107.8(3) . . ?
O10P Cl3 O12P 107.6(3) . . ?
O10P Cl3 O11P 110.1(3) . . ?
O12P Cl3 O11P 108.0(4) . . ?
O10P Cl3 O9P 109.8(3) . . ?
O12P Cl3 O9P 111.4(4) . . ?
O11P Cl3 O9P 109.8(3) . . ?
O13P Cl4 O15P 107.7(3) . . ?
O13P Cl4 O14P 109.6(3) . . ?
O15P Cl4 O14P 108.4(3) . . ?
O13P Cl4 O16P 110.7(3) . . ?
O15P Cl4 O16P 110.5(3) . . ?
O14P Cl4 O16P 109.9(3) . . ?
O18P Cl5 O20P 110.8(2) . . ?
O18P Cl5 O17P 109.4(2) . . ?
O20P Cl5 O17P 110.4(2) . . ?
O18P Cl5 O19P 109.2(2) . . ?
O20P Cl5 O19P 109.3(2) . . ?
O17P Cl5 O19P 107.7(3) . . ?
O24P Cl6 O22P 112.1(3) . . ?
O24P Cl6 O23P 109.6(3) . . ?
O22P Cl6 O23P 107.8(2) . . ?
O24P Cl6 O21P 109.9(3) . . ?
O22P Cl6 O21P 108.2(3) . . ?
O23P Cl6 O21P 109.2(2) . . ?
O28A Cl7 O25P 119.4(11) . . ?
O25P Cl7 O27P 108.5(4) . . ?
O28A Cl7 O27A 111.2(13) . . ?
O25P Cl7 O27A 101.7(10) . . ?
O28A Cl7 O26A 110.9(12) . . ?
O25P Cl7 O26A 99.5(9) . . ?
O27A Cl7 O26A 113.5(11) . . ?
O25P Cl7 O28P 107.2(5) . . ?
O27P Cl7 O28P 110.3(5) . . ?
O25P Cl7 O26P 114.8(4) . . ?
O27P Cl7 O26P 108.3(5) . . ?
O28P Cl7 O26P 107.7(4) . . ?
O30P Cl8 O31P 125.1(8) . . ?
O31A Cl8 O30A 126.2(10) . . ?
O30P Cl8 O29P 114.3(9) . . ?
O31P Cl8 O29P 114.7(8) . . ?
O31A Cl8 O29A 117.2(10) . . ?
O30A Cl8 O29A 115.7(11) . . ?
O30P Cl8 O32P 100.9(6) . . ?
O31P Cl8 O32P 96.2(5) . . ?
O29P Cl8 O32P 97.2(8) . . ?
O31A Cl8 O32A 96.0(7) . . ?
O30A Cl8 O32A 91.7(7) . . ?
O29A Cl8 O32A 91.8(10) . . ?
O33P Cl9 Cl9 60.2(2) 2_666 2_666 ?
O33P Cl9 O33P 120.1(2) 2_666 . ?
Cl9 Cl9 O33P 59.9(2) 2_666 . ?
O33P Cl9 O34P 108.6(4) 2_666 . ?
Cl9 Cl9 O34P 126.5(5) 2_666 . ?
O33P Cl9 O34P 106.0(4) . . ?
O33P Cl9 O35P 107.4(4) 2_666 . ?
Cl9 Cl9 O35P 127.3(5) 2_666 . ?
O33P Cl9 O35P 107.8(4) . . ?
O34P Cl9 O35P 106.3(6) . . ?
Cl9 O33P Cl9 59.9(2) 2_666 . ?
O45P Cl12 O47P 120.3(12) . . ?
O45P Cl12 O48P 122.0(7) . . ?
O47P Cl12 O48P 106.6(11) . . ?
O45P Cl12 O46P 101.1(9) . . ?
O47P Cl12 O46P 99.6(11) . . ?
O48P Cl12 O46P 102.7(9) . . ?
Cl12 O46P O38P 106.2(12) . . ?
O39P Cl10 O40P 109.5(5) . . ?
O39P Cl10 O37P 107.3(7) . . ?
O40P Cl10 O37P 119.3(7) . . ?
O39P Cl10 O38P 110.3(6) . . ?
O40P Cl10 O38P 101.6(5) . . ?
O37P Cl10 O38P 108.7(5) . . ?
Cl10 O38P O46P 157.5(9) . . ?
Cl10 O39P O6W 108.4(8) . . ?
O42P Cl11 O44P 124.1(9) . . ?
O42P Cl11 O41P 112.3(8) . . ?
O44P Cl11 O41P 106.8(8) . . ?
O43A Cl11 O41P 137.7(10) . . ?
O43A Cl11 O42A 113.8(13) . . ?
O41P Cl11 O42A 106.1(12) . . ?
O43A Cl11 O44A 98.8(12) . . ?
O41P Cl11 O44A 90.2(10) . . ?
O42A Cl11 O44A 96.2(12) . . ?
O42P Cl11 O43P 108.0(8) . . ?
O44P Cl11 O43P 101.5(7) . . ?
O41P Cl11 O43P 101.2(7) . . ?
O13W O14W O10W 153.4(17) . . ?
C2S C1S O1S 116.2(6) . . ?
O2S C3S C4S 109.9(7) . . ?
O3S C5S C6S 108.7(6) . . ?
C8SA C7SA O4S 144.6(14) . . ?
C8SB C7SB O4S 142.6(15) . . ?

_refine_diff_density_max         2.029
_refine_diff_density_min         -1.315
_refine_diff_density_rms         0.123

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_NINO3DP_SQ
_database_code_depnum_ccdc_archive 'CCDC 1868874'
_audit_update_record             
;
2018-12-20 deposited with the CCDC.
2019-01-04 downloaded from the CCDC.
;

_vrf_THETM01_NINO3DP_SQ          
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Crystals of compound 2 were difficult to handle out of the 
mother solution because of the rapid loss of lattice solvent molecules. 
To slow down the degradation process, the crystals were collected at 
low T in Paratone oil. However, a partial solvent loss (and crystal 
degradation) occurred anyway, so the collected crystal(s) diffracted 
poorly.
;
_vrf_PLAT043_NINO3DP_SQ          
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..     630.41 Check 
RESPONSE: The unit cell contains 6 nitrate anions and (at least) 14 water 
molecules which have been treated as a diffuse contribution to the overall 
scattering without specific atom positions by SQUEEZE/PLATON. The 
counterion/solvent portion of the structure was obviously included in the 
UNIT instruction. Note that as the available data are far from ideal, the
SQUEEZE procedure brought the R1 value from about 11 (best model with the 
unsqueezed data) to about 7, but still large residual density was observed
after squeezing, the highest peaks being located very close to some of the 
coordinated dppn ligands.
;
_vrf_PLAT602_NINO3DP_SQ          
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure        ! Info 
RESPONSE: See the SQUEEZE RESULTS appended in the cif file.
;


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C56 H46 N16 Ni4 O4, 6(N O3), 14(H2 O)'
_chemical_formula_sum            'C56 H74 N22 Ni4 O36'
_chemical_formula_weight         1866.21

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                   14.5870(10)
_cell_length_b                   14.7541(9)
_cell_length_c                   18.4452(12)
_cell_angle_alpha                95.571(3)
_cell_angle_beta                 97.055(3)
_cell_angle_gamma                90.120(3)
_cell_volume                     3920.7(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9928
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      22.41

_exptl_crystal_description       LAMINAR
_exptl_crystal_colour            AMBER-YELLOW
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_F_000             1928
_exptl_transmission_factor_min   0.6627
_exptl_transmission_factor_max   0.7448
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    1.049
_shelx_estimated_absorpt_T_min   0.758
_shelx_estimated_absorpt_T_max   0.969
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   
'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker X8 Apex-II CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            59861
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.118
_diffrn_reflns_theta_max         22.459
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.711
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.711
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.711
_reflns_number_total             10097
_reflns_number_gt                8285
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013, version 2013-4 (Sheldrick 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
# SQUEEZE RESULTS (Version = 160117)
# 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  0.500  0.278  0.424      1182       757 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           

The unit cell contains 6 nitrate anions and (at least) 14 water molecules which have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1315P)²+9.6345P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     PATT
_atom_sites_solution_secondary   DIFMAP
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10097
_refine_ls_number_parameters     727
_refine_ls_number_restraints     665
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0712
_refine_ls_wR_factor_ref         0.2149
_refine_ls_wR_factor_gt          0.2078
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_restrained_S_all      1.074
_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
Ni1 Ni 0.82830(5) 0.90798(4) 0.21200(3) 0.0239(2) Uani 1 1 d . . . . .
Ni2 Ni 0.65704(5) 0.74721(5) 0.21414(4) 0.0297(2) Uani 1 1 d . . . . .
Ni3 Ni 0.82353(6) 0.58803(5) 0.25497(4) 0.0313(3) Uani 1 1 d . . . . .
Ni4 Ni 0.99418(5) 0.74769(4) 0.24828(3) 0.0239(2) Uani 1 1 d . . . . .
O4 O 0.8876(3) 0.7869(2) 0.17446(19) 0.0255(8) Uani 1 1 d . . . . .
O3 O 0.8861(3) 0.7100(2) 0.30307(19) 0.0280(9) Uani 1 1 d . . . . .
O2 O 0.7651(3) 0.6709(2) 0.17718(19) 0.0284(9) Uani 1 1 d . . . . .
O1 O 0.7655(3) 0.8226(2) 0.27489(19) 0.0289(9) Uani 1 1 d . . . . .
N1 N 0.8735(3) 0.9830(3) 0.1332(2) 0.0251(10) Uani 1 1 d . U . . .
N2 N 0.7238(3) 0.8856(3) 0.1258(2) 0.0278(10) Uani 1 1 d . U . . .
N3 N 0.6586(3) 0.8216(3) 0.1264(2) 0.0246(10) Uani 1 1 d . U . . .
N4 N 0.5587(3) 0.6790(3) 0.1380(2) 0.0297(10) Uani 1 1 d . U . . .
C1 C 0.9509(4) 1.0343(4) 0.1423(3) 0.0365(14) Uani 1 1 d . U . . .
H1A H 0.9920 1.0338 0.1864 0.044 Uiso 1 1 calc R U . . .
C2 C 0.9723(5) 1.0890(5) 0.0881(4) 0.0478(17) Uani 1 1 d . U . . .
H2A H 1.0274 1.1249 0.0952 0.057 Uiso 1 1 calc R U . . .
C3 C 0.9118(5) 1.0895(4) 0.0245(3) 0.0419(15) Uani 1 1 d . U . . .
H3A H 0.9247 1.1262 -0.0126 0.050 Uiso 1 1 calc R U . . .
C4 C 0.8325(4) 1.0365(4) 0.0151(3) 0.0344(13) Uani 1 1 d . U . . .
H4A H 0.7905 1.0357 -0.0286 0.041 Uiso 1 1 calc R U . . .
C5 C 0.8151(4) 0.9836(4) 0.0712(3) 0.0285(12) Uani 1 1 d . U . . .
C6 C 0.7368(4) 0.9191(4) 0.0630(3) 0.0301(12) Uani 1 1 d . U . . .
C7 C 0.6804(4) 0.8932(4) -0.0020(3) 0.0328(13) Uani 1 1 d . U . . .
H7A H 0.6863 0.9215 -0.0453 0.039 Uiso 1 1 calc R U . . .
C8 C 0.6166(4) 0.8265(4) -0.0017(3) 0.0366(14) Uani 1 1 d . U . . .
H8A H 0.5791 0.8045 -0.0457 0.044 Uiso 1 1 calc R U . . .
C9 C 0.6068(4) 0.7909(4) 0.0638(3) 0.0273(12) Uani 1 1 d . U . . .
C10 C 0.5446(4) 0.7126(4) 0.0715(3) 0.0309(12) Uani 1 1 d . U . . .
C11 C 0.4814(4) 0.6757(4) 0.0150(3) 0.0353(13) Uani 1 1 d . U . . .
H11A H 0.4717 0.7017 -0.0304 0.042 Uiso 1 1 calc R U . . .
C12 C 0.4316(4) 0.5983(4) 0.0270(4) 0.0408(14) Uani 1 1 d . U . . .
H12A H 0.3885 0.5695 -0.0111 0.049 Uiso 1 1 calc R U . . .
C13 C 0.4457(4) 0.5647(4) 0.0938(3) 0.0397(14) Uani 1 1 d . U . . .
H13A H 0.4117 0.5128 0.1028 0.048 Uiso 1 1 calc R U . . .
C14 C 0.5097(4) 0.6067(4) 0.1481(4) 0.0389(14) Uani 1 1 d . U . . .
H14A H 0.5189 0.5829 0.1944 0.047 Uiso 1 1 calc R U . . .
N5 N 0.5560(4) 0.8131(4) 0.2664(3) 0.0375(11) Uani 1 1 d . U . . .
N6 N 0.6531(4) 0.6731(3) 0.3025(2) 0.0345(10) Uani 1 1 d . U . . .
N7 N 0.7180(4) 0.6106(3) 0.3176(2) 0.0349(11) Uani 1 1 d . U . . .
N8 N 0.8657(4) 0.5151(3) 0.3440(3) 0.0401(11) Uani 1 1 d . U . . .
C15 C 0.5073(4) 0.8845(5) 0.2451(4) 0.0444(14) Uani 1 1 d . U . . .
H15A H 0.5199 0.9086 0.2014 0.053 Uiso 1 1 calc R U . . .
C16 C 0.4400(5) 0.9253(6) 0.2827(4) 0.0561(17) Uani 1 1 d . U . . .
H16A H 0.4076 0.9770 0.2667 0.067 Uiso 1 1 calc R U . . .
C17 C 0.4219(5) 0.8862(6) 0.3463(4) 0.0628(18) Uani 1 1 d . U . . .
H17A H 0.3755 0.9113 0.3739 0.075 Uiso 1 1 calc R U . . .
C18 C 0.4707(5) 0.8122(6) 0.3688(4) 0.0604(18) Uani 1 1 d . U . . .
H18A H 0.4583 0.7859 0.4117 0.073 Uiso 1 1 calc R U . . .
C19 C 0.5369(4) 0.7772(5) 0.3289(3) 0.0428(13) Uani 1 1 d . U . . .
C20 C 0.5960(5) 0.7018(4) 0.3500(3) 0.0381(12) Uani 1 1 d . U . . .
C21 C 0.5993(5) 0.6613(5) 0.4168(3) 0.0473(14) Uani 1 1 d . U . . .
H21A H 0.5563 0.6783 0.4502 0.057 Uiso 1 1 calc R U . . .
C22 C 0.6647(5) 0.5979(5) 0.4329(3) 0.0472(14) Uani 1 1 d . U . . .
H22A H 0.6683 0.5706 0.4778 0.057 Uiso 1 1 calc R U . . .
C23 C 0.7262(5) 0.5738(4) 0.3819(3) 0.0422(12) Uani 1 1 d . U . . .
C24 C 0.8060(5) 0.5137(4) 0.3931(3) 0.0427(13) Uani 1 1 d . U . . .
C25 C 0.8216(6) 0.4619(5) 0.4533(4) 0.0576(17) Uani 1 1 d . U . . .
H25A H 0.7782 0.4615 0.4877 0.069 Uiso 1 1 calc R U . . .
C26 C 0.8999(7) 0.4122(6) 0.4614(4) 0.071(2) Uani 1 1 d . U . . .
H26A H 0.9112 0.3762 0.5015 0.085 Uiso 1 1 calc R U . . .
C27 C 0.9629(7) 0.4139(6) 0.4117(4) 0.069(2) Uani 1 1 d . U . . .
H27A H 1.0185 0.3805 0.4171 0.083 Uiso 1 1 calc R U . . .
C28 C 0.9416(6) 0.4670(5) 0.3524(4) 0.0513(16) Uani 1 1 d . U . . .
H28A H 0.9838 0.4681 0.3171 0.062 Uiso 1 1 calc R U . . .
N9 N 0.7805(4) 0.4659(3) 0.1941(3) 0.0399(11) Uani 1 1 d . U . . .
N10 N 0.9297(4) 0.5605(3) 0.1935(2) 0.0320(11) Uani 1 1 d . U . . .
N11 N 0.9957(4) 0.6215(3) 0.1920(2) 0.0304(10) Uani 1 1 d . U . . .
N12 N 1.0993(3) 0.7637(3) 0.1830(2) 0.0286(10) Uani 1 1 d . U . . .
C29 C 0.6999(5) 0.4207(4) 0.1994(4) 0.0509(15) Uani 1 1 d . U . . .
H29 H 0.6563 0.4482 0.2286 0.061 Uiso 1 1 calc R U . . .
C30 C 0.6813(6) 0.3342(5) 0.1620(4) 0.0606(18) Uani 1 1 d . U . . .
H30 H 0.6260 0.3022 0.1665 0.073 Uiso 1 1 calc R U . . .
C31 C 0.7436(6) 0.2965(5) 0.1192(5) 0.068(2) Uani 1 1 d . U . . .
H31 H 0.7312 0.2380 0.0934 0.082 Uiso 1 1 calc R U . . .
C32 C 0.8260(6) 0.3429(4) 0.1127(4) 0.0572(17) Uani 1 1 d . U . . .
H32 H 0.8699 0.3174 0.0829 0.069 Uiso 1 1 calc R U . . .
C33 C 0.8398(5) 0.4270(4) 0.1514(3) 0.0429(13) Uani 1 1 d . U . . .
C34 C 0.9242(5) 0.4841(4) 0.1483(3) 0.0391(12) Uani 1 1 d . U . . .
C35 C 0.9884(5) 0.4648(4) 0.1004(3) 0.0425(13) Uani 1 1 d . U . . .
H35 H 0.9843 0.4099 0.0687 0.051 Uiso 1 1 calc R U . . .
C36 C 1.0591(5) 0.5274(4) 0.0994(3) 0.0405(13) Uani 1 1 d . U . . .
H36 H 1.1064 0.5156 0.0688 0.049 Uiso 1 1 calc R U . . .
C37 C 1.0582(5) 0.6082(4) 0.1451(3) 0.0342(12) Uani 1 1 d . U . . .
C38 C 1.1227(5) 0.6867(4) 0.1448(3) 0.0349(12) Uani 1 1 d . U . . .
C39 C 1.1996(5) 0.6804(4) 0.1074(3) 0.0402(13) Uani 1 1 d . U . . .
H39 H 1.2146 0.6245 0.0816 0.048 Uiso 1 1 calc R U . . .
C40 C 1.2540(5) 0.7578(5) 0.1085(4) 0.0455(14) Uani 1 1 d . U . . .
H40 H 1.3075 0.7562 0.0838 0.055 Uiso 1 1 calc R U . . .
C41 C 1.2282(4) 0.8387(5) 0.1469(3) 0.0380(13) Uani 1 1 d . U . . .
H41 H 1.2632 0.8932 0.1477 0.046 Uiso 1 1 calc R U . . .
C42 C 1.1513(4) 0.8379(4) 0.1833(3) 0.0348(13) Uani 1 1 d . U . . .
H42 H 1.1347 0.8926 0.2098 0.042 Uiso 1 1 calc R U . . .
N13 N 1.1003(3) 0.7299(3) 0.3330(2) 0.0275(10) Uani 1 1 d . U . . .
N14 N 1.0009(3) 0.8729(3) 0.3065(2) 0.0239(9) Uani 1 1 d . U . . .
N15 N 0.9355(3) 0.9337(3) 0.2945(2) 0.0244(9) Uani 1 1 d . U . . .
N16 N 0.7864(3) 1.0267(3) 0.2692(2) 0.0299(10) Uani 1 1 d . U . . .
C43 C 1.1495(5) 0.6558(4) 0.3402(3) 0.0367(13) Uani 1 1 d . U . . .
H43 H 1.1297 0.6016 0.3102 0.044 Uiso 1 1 calc R U . . .
C44 C 1.2294(5) 0.6537(5) 0.3901(3) 0.0408(14) Uani 1 1 d . U . . .
H44 H 1.2641 0.5995 0.3937 0.049 Uiso 1 1 calc R U . . .
C45 C 1.2567(4) 0.7329(4) 0.4341(3) 0.0399(13) Uani 1 1 d . U . . .
H45 H 1.3106 0.7339 0.4688 0.048 Uiso 1 1 calc R U . . .
C46 C 1.2041(4) 0.8115(4) 0.4269(3) 0.0338(12) Uani 1 1 d . U . . .
H46 H 1.2218 0.8666 0.4564 0.041 Uiso 1 1 calc R U . . .
C47 C 1.1262(4) 0.8073(4) 0.3765(3) 0.0281(11) Uani 1 1 d . U . . .
C48 C 1.0662(4) 0.8867(4) 0.3652(3) 0.0288(11) Uani 1 1 d . U . . .
C49 C 1.0666(4) 0.9666(4) 0.4130(3) 0.0296(12) Uani 1 1 d . U . . .
H49 H 1.1131 0.9772 0.4538 0.035 Uiso 1 1 calc R U . . .
C50 C 1.0005(4) 1.0277(4) 0.4001(3) 0.0290(11) Uani 1 1 d . U . . .
H50 H 1.0001 1.0832 0.4309 0.035 Uiso 1 1 calc R U . . .
C51 C 0.9317(4) 1.0084(4) 0.3403(3) 0.0269(11) Uani 1 1 d . U . . .
C52 C 0.8470(4) 1.0638(4) 0.3249(3) 0.0284(11) Uani 1 1 d . U . . .
C53 C 0.8314(5) 1.1440(4) 0.3665(4) 0.0414(14) Uani 1 1 d . U . . .
H53 H 0.8761 1.1684 0.4053 0.050 Uiso 1 1 calc R U . . .
C54 C 0.7478(5) 1.1880(5) 0.3498(4) 0.0489(15) Uani 1 1 d . U . . .
H54 H 0.7344 1.2433 0.3772 0.059 Uiso 1 1 calc R U . . .
C55 C 0.6843(5) 1.1495(5) 0.2920(4) 0.0489(15) Uani 1 1 d . U . . .
H55 H 0.6268 1.1777 0.2797 0.059 Uiso 1 1 calc R U . . .
C56 C 0.7067(5) 1.0697(4) 0.2532(3) 0.0422(14) Uani 1 1 d . U . . .
H56 H 0.6639 1.0442 0.2134 0.051 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 N15 2.050(5) . ?
Ni1 N2 2.065(5) . ?
Ni1 O1 2.076(3) . ?
Ni1 N1 2.078(4) . ?
Ni1 O4 2.082(4) . ?
Ni1 N16 2.088(5) . ?
Ni1 Ni4 3.4394(10) . ?
Ni1 Ni2 3.4477(9) . ?
Ni2 N3 2.043(4) . ?
Ni2 N5 2.054(6) . ?
Ni2 N6 2.055(5) . ?
Ni2 N4 2.066(5) . ?
Ni2 O1 2.077(4) . ?
Ni2 O2 2.084(4) . ?
Ni2 Ni3 3.4495(11) . ?
Ni3 N7 2.044(5) . ?
Ni3 N10 2.047(5) . ?
Ni3 O2 2.080(4) . ?
Ni3 N8 2.081(5) . ?
Ni3 N9 2.081(5) . ?
Ni3 O3 2.083(4) . ?
Ni3 Ni4 3.4449(10) . ?
Ni4 N14 2.040(4) . ?
Ni4 N11 2.043(5) . ?
Ni4 O4 2.059(4) . ?
Ni4 O3 2.077(4) . ?
Ni4 N12 2.089(5) . ?
Ni4 N13 2.097(5) . ?
O4 O2 2.480(5) . ?
O3 O1 2.466(6) . ?
N1 C5 1.339(7) . ?
N1 C1 1.342(8) . ?
N2 C6 1.336(7) . ?
N2 N3 1.341(6) . ?
N3 C9 1.339(7) . ?
N4 C14 1.324(8) . ?
N4 C10 1.360(7) . ?
C1 C2 1.408(9) . ?
C1 H1A 0.9500 . ?
C2 C3 1.379(9) . ?
C2 H2A 0.9500 . ?
C3 C4 1.379(9) . ?
C3 H3A 0.9500 . ?
C4 C5 1.402(8) . ?
C4 H4A 0.9500 . ?
C5 C6 1.469(8) . ?
C6 C7 1.388(8) . ?
C7 C8 1.354(8) . ?
C7 H7A 0.9500 . ?
C8 C9 1.387(8) . ?
C8 H8A 0.9500 . ?
C9 C10 1.495(8) . ?
C10 C11 1.372(8) . ?
C11 C12 1.402(9) . ?
C11 H11A 0.9500 . ?
C12 C13 1.365(9) . ?
C12 H12A 0.9500 . ?
C13 C14 1.381(9) . ?
C13 H13A 0.9500 . ?
C14 H14A 0.9500 . ?
N5 C15 1.335(9) . ?
N5 C19 1.373(8) . ?
N6 C20 1.323(8) . ?
N6 N7 1.347(7) . ?
N7 C23 1.345(8) . ?
N8 C28 1.318(9) . ?
N8 C24 1.333(9) . ?
C15 C16 1.377(10) . ?
C15 H15A 0.9500 . ?
C16 C17 1.409(11) . ?
C16 H16A 0.9500 . ?
C17 C18 1.375(12) . ?
C17 H17A 0.9500 . ?
C18 C19 1.359(10) . ?
C18 H18A 0.9500 . ?
C19 C20 1.461(10) . ?
C20 C21 1.416(9) . ?
C21 C22 1.365(10) . ?
C21 H21A 0.9500 . ?
C22 C23 1.401(10) . ?
C22 H22A 0.9500 . ?
C23 C24 1.471(10) . ?
C24 C25 1.404(9) . ?
C25 C26 1.359(12) . ?
C25 H25A 0.9500 . ?
C26 C27 1.377(12) . ?
C26 H26A 0.9500 . ?
C27 C28 1.411(10) . ?
C27 H27A 0.9500 . ?
C28 H28A 0.9500 . ?
N9 C33 1.333(9) . ?
N9 C29 1.371(9) . ?
N10 N11 1.321(7) . ?
N10 C34 1.332(7) . ?
N11 C37 1.335(8) . ?
N12 C42 1.329(8) . ?
N12 C38 1.346(8) . ?
C29 C30 1.400(10) . ?
C29 H29 0.9500 . ?
C30 C31 1.360(12) . ?
C30 H30 0.9500 . ?
C31 C32 1.406(12) . ?
C31 H31 0.9500 . ?
C32 C33 1.371(9) . ?
C32 H32 0.9500 . ?
C33 C34 1.501(10) . ?
C34 C35 1.376(10) . ?
C35 C36 1.386(10) . ?
C35 H35 0.9500 . ?
C36 C37 1.392(8) . ?
C36 H36 0.9500 . ?
C37 C38 1.491(9) . ?
C38 C39 1.387(9) . ?
C39 C40 1.387(10) . ?
C39 H39 0.9500 . ?
C40 C41 1.404(10) . ?
C40 H40 0.9500 . ?
C41 C42 1.378(9) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
N13 C43 1.317(8) . ?
N13 C47 1.355(7) . ?
N14 N15 1.325(6) . ?
N14 C48 1.350(7) . ?
N15 C51 1.328(7) . ?
N16 C56 1.341(8) . ?
N16 C52 1.342(7) . ?
C43 C44 1.397(9) . ?
C43 H43 0.9500 . ?
C44 C45 1.385(9) . ?
C44 H44 0.9500 . ?
C45 C46 1.401(9) . ?
C45 H45 0.9500 . ?
C46 C47 1.374(8) . ?
C46 H46 0.9500 . ?
C47 C48 1.480(8) . ?
C48 C49 1.402(8) . ?
C49 C50 1.337(8) . ?
C49 H49 0.9500 . ?
C50 C51 1.404(8) . ?
C50 H50 0.9500 . ?
C51 C52 1.496(9) . ?
C52 C53 1.382(8) . ?
C53 C54 1.398(10) . ?
C53 H53 0.9500 . ?
C54 C55 1.398(10) . ?
C54 H54 0.9500 . ?
C55 C56 1.378(10) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?

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
N15 Ni1 N2 177.24(17) . . ?
N15 Ni1 O1 90.64(15) . . ?
N2 Ni1 O1 92.10(16) . . ?
N15 Ni1 N1 99.73(17) . . ?
N2 Ni1 N1 77.51(17) . . ?
O1 Ni1 N1 169.36(16) . . ?
N15 Ni1 O4 91.51(16) . . ?
N2 Ni1 O4 88.57(16) . . ?
O1 Ni1 O4 82.44(14) . . ?
N1 Ni1 O4 94.85(15) . . ?
N15 Ni1 N16 77.53(18) . . ?
N2 Ni1 N16 102.56(19) . . ?
O1 Ni1 N16 93.73(16) . . ?
N1 Ni1 N16 90.81(17) . . ?
O4 Ni1 N16 168.40(17) . . ?
N15 Ni1 Ni4 58.80(13) . . ?
N2 Ni1 Ni4 121.63(13) . . ?
O1 Ni1 Ni4 76.89(11) . . ?
N1 Ni1 Ni4 106.46(13) . . ?
O4 Ni1 Ni4 33.64(10) . . ?
N16 Ni1 Ni4 134.81(13) . . ?
N15 Ni1 Ni2 123.75(12) . . ?
N2 Ni1 Ni2 58.93(12) . . ?
O1 Ni1 Ni2 33.89(10) . . ?
N1 Ni1 Ni2 135.48(13) . . ?
O4 Ni1 Ni2 76.52(10) . . ?
N16 Ni1 Ni2 106.27(13) . . ?
Ni4 Ni1 Ni2 90.25(2) . . ?
N3 Ni2 N5 100.52(19) . . ?
N3 Ni2 N6 179.0(2) . . ?
N5 Ni2 N6 78.5(2) . . ?
N3 Ni2 N4 78.38(18) . . ?
N5 Ni2 N4 91.04(19) . . ?
N6 Ni2 N4 101.19(18) . . ?
N3 Ni2 O1 92.61(16) . . ?
N5 Ni2 O1 94.91(17) . . ?
N6 Ni2 O1 87.88(16) . . ?
N4 Ni2 O1 170.00(16) . . ?
N3 Ni2 O2 88.52(16) . . ?
N5 Ni2 O2 170.64(17) . . ?
N6 Ni2 O2 92.44(18) . . ?
N4 Ni2 O2 93.18(17) . . ?
O1 Ni2 O2 82.15(15) . . ?
N3 Ni2 Ni1 59.37(12) . . ?
N5 Ni2 Ni1 105.83(14) . . ?
N6 Ni2 Ni1 121.23(13) . . ?
N4 Ni2 Ni1 136.40(13) . . ?
O1 Ni2 Ni1 33.87(10) . . ?
O2 Ni2 Ni1 76.60(10) . . ?
N3 Ni2 Ni3 121.82(13) . . ?
N5 Ni2 Ni3 136.65(14) . . ?
N6 Ni2 Ni3 59.19(16) . . ?
N4 Ni2 Ni3 105.25(14) . . ?
O1 Ni2 Ni3 75.70(11) . . ?
O2 Ni2 Ni3 34.01(9) . . ?
Ni1 Ni2 Ni3 89.69(2) . . ?
N7 Ni3 N10 177.78(19) . . ?
N7 Ni3 O2 92.38(18) . . ?
N10 Ni3 O2 89.49(16) . . ?
N7 Ni3 N8 78.1(2) . . ?
N10 Ni3 N8 100.1(2) . . ?
O2 Ni3 N8 170.2(2) . . ?
N7 Ni3 N9 101.1(2) . . ?
N10 Ni3 N9 77.5(2) . . ?
O2 Ni3 N9 95.36(16) . . ?
N8 Ni3 N9 88.81(18) . . ?
N7 Ni3 O3 89.59(17) . . ?
N10 Ni3 O3 91.85(17) . . ?
O2 Ni3 O3 82.71(14) . . ?
N8 Ni3 O3 94.80(16) . . ?
N9 Ni3 O3 169.2(2) . . ?
N7 Ni3 Ni4 122.88(13) . . ?
N10 Ni3 Ni4 58.78(13) . . ?
O2 Ni3 Ni4 76.24(10) . . ?
N8 Ni3 Ni4 106.90(15) . . ?
N9 Ni3 Ni4 135.17(16) . . ?
O3 Ni3 Ni4 34.05(10) . . ?
N7 Ni3 Ni2 59.09(14) . . ?
N10 Ni3 Ni2 122.91(12) . . ?
O2 Ni3 Ni2 34.08(11) . . ?
N8 Ni3 Ni2 136.11(17) . . ?
N9 Ni3 Ni2 107.32(15) . . ?
O3 Ni3 Ni2 76.94(11) . . ?
Ni4 Ni3 Ni2 90.13(2) . . ?
N14 Ni4 N11 176.6(2) . . ?
N14 Ni4 O4 91.84(16) . . ?
N11 Ni4 O4 91.18(16) . . ?
N14 Ni4 O3 90.24(16) . . ?
N11 Ni4 O3 91.76(18) . . ?
O4 Ni4 O3 82.60(14) . . ?
N14 Ni4 N12 99.57(18) . . ?
N11 Ni4 N12 78.47(19) . . ?
O4 Ni4 N12 96.43(16) . . ?
O3 Ni4 N12 170.17(17) . . ?
N14 Ni4 N13 78.36(18) . . ?
N11 Ni4 N13 98.64(18) . . ?
O4 Ni4 N13 170.16(16) . . ?
O3 Ni4 N13 96.52(16) . . ?
N12 Ni4 N13 86.10(17) . . ?
N14 Ni4 Ni1 58.92(13) . . ?
N11 Ni4 Ni1 124.31(14) . . ?
O4 Ni4 Ni1 34.06(10) . . ?
O3 Ni4 Ni1 75.98(10) . . ?
N12 Ni4 Ni1 108.59(12) . . ?
N13 Ni4 Ni1 136.22(13) . . ?
N14 Ni4 Ni3 123.72(13) . . ?
N11 Ni4 Ni3 58.66(15) . . ?
O4 Ni4 Ni3 76.78(10) . . ?
O3 Ni4 Ni3 34.17(10) . . ?
N12 Ni4 Ni3 136.08(13) . . ?
N13 Ni4 Ni3 107.92(12) . . ?
Ni1 Ni4 Ni3 89.90(2) . . ?
Ni4 O4 Ni1 112.31(16) . . ?
Ni4 O4 O2 103.56(16) . . ?
Ni1 O4 O2 103.53(18) . . ?
Ni4 O3 Ni3 111.79(17) . . ?
Ni4 O3 O1 104.15(16) . . ?
Ni3 O3 O1 102.65(17) . . ?
Ni3 O2 Ni2 111.91(16) . . ?
Ni3 O2 O4 103.40(17) . . ?
Ni2 O2 O4 103.34(17) . . ?
Ni1 O1 Ni2 112.24(16) . . ?
Ni1 O1 O3 102.94(18) . . ?
Ni2 O1 O3 104.69(17) . . ?
C5 N1 C1 119.5(5) . . ?
C5 N1 Ni1 115.0(4) . . ?
C1 N1 Ni1 125.2(4) . . ?
C6 N2 N3 120.3(5) . . ?
C6 N2 Ni1 116.9(4) . . ?
N3 N2 Ni1 120.6(3) . . ?
C9 N3 N2 119.7(4) . . ?
C9 N3 Ni2 117.5(3) . . ?
N2 N3 Ni2 121.1(3) . . ?
C14 N4 C10 118.1(5) . . ?
C14 N4 Ni2 126.2(4) . . ?
C10 N4 Ni2 115.7(4) . . ?
N1 C1 C2 121.4(6) . . ?
N1 C1 H1A 119.3 . . ?
C2 C1 H1A 119.3 . . ?
C3 C2 C1 118.7(6) . . ?
C3 C2 H2A 120.6 . . ?
C1 C2 H2A 120.6 . . ?
C2 C3 C4 119.8(5) . . ?
C2 C3 H3A 120.1 . . ?
C4 C3 H3A 120.1 . . ?
C3 C4 C5 118.7(5) . . ?
C3 C4 H4A 120.7 . . ?
C5 C4 H4A 120.7 . . ?
N1 C5 C4 121.8(5) . . ?
N1 C5 C6 115.7(5) . . ?
C4 C5 C6 122.2(5) . . ?
N2 C6 C7 121.5(5) . . ?
N2 C6 C5 113.1(5) . . ?
C7 C6 C5 125.5(5) . . ?
C8 C7 C6 118.0(5) . . ?
C8 C7 H7A 121.0 . . ?
C6 C7 H7A 121.0 . . ?
C7 C8 C9 118.9(5) . . ?
C7 C8 H8A 120.5 . . ?
C9 C8 H8A 120.5 . . ?
N3 C9 C8 121.3(5) . . ?
N3 C9 C10 113.7(5) . . ?
C8 C9 C10 124.9(5) . . ?
N4 C10 C11 123.1(5) . . ?
N4 C10 C9 114.2(5) . . ?
C11 C10 C9 122.6(5) . . ?
C10 C11 C12 117.4(6) . . ?
C10 C11 H11A 121.3 . . ?
C12 C11 H11A 121.3 . . ?
C13 C12 C11 119.5(6) . . ?
C13 C12 H12A 120.2 . . ?
C11 C12 H12A 120.2 . . ?
C12 C13 C14 119.4(6) . . ?
C12 C13 H13A 120.3 . . ?
C14 C13 H13A 120.3 . . ?
N4 C14 C13 122.5(6) . . ?
N4 C14 H14A 118.8 . . ?
C13 C14 H14A 118.8 . . ?
C15 N5 C19 118.1(6) . . ?
C15 N5 Ni2 127.0(4) . . ?
C19 N5 Ni2 114.9(5) . . ?
C20 N6 N7 122.0(5) . . ?
C20 N6 Ni2 116.4(4) . . ?
N7 N6 Ni2 120.3(4) . . ?
C23 N7 N6 120.7(5) . . ?
C23 N7 Ni3 116.6(5) . . ?
N6 N7 Ni3 121.4(3) . . ?
C28 N8 C24 119.0(5) . . ?
C28 N8 Ni3 125.7(5) . . ?
C24 N8 Ni3 115.1(5) . . ?
N5 C15 C16 124.0(6) . . ?
N5 C15 H15A 118.0 . . ?
C16 C15 H15A 118.0 . . ?
C15 C16 C17 116.3(8) . . ?
C15 C16 H16A 121.8 . . ?
C17 C16 H16A 121.8 . . ?
C18 C17 C16 120.6(7) . . ?
C18 C17 H17A 119.7 . . ?
C16 C17 H17A 119.7 . . ?
C19 C18 C17 119.0(7) . . ?
C19 C18 H18A 120.5 . . ?
C17 C18 H18A 120.5 . . ?
C18 C19 N5 121.9(7) . . ?
C18 C19 C20 123.4(6) . . ?
N5 C19 C20 114.6(6) . . ?
N6 C20 C21 118.9(7) . . ?
N6 C20 C19 115.2(5) . . ?
C21 C20 C19 125.8(6) . . ?
C22 C21 C20 119.7(6) . . ?
C22 C21 H21A 120.1 . . ?
C20 C21 H21A 120.1 . . ?
C21 C22 C23 118.5(6) . . ?
C21 C22 H22A 120.7 . . ?
C23 C22 H22A 120.7 . . ?
N7 C23 C22 119.9(7) . . ?
N7 C23 C24 114.1(6) . . ?
C22 C23 C24 125.9(6) . . ?
N8 C24 C25 121.8(7) . . ?
N8 C24 C23 115.3(5) . . ?
C25 C24 C23 122.9(7) . . ?
C26 C25 C24 118.8(7) . . ?
C26 C25 H25A 120.6 . . ?
C24 C25 H25A 120.6 . . ?
C25 C26 C27 120.1(7) . . ?
C25 C26 H26A 119.9 . . ?
C27 C26 H26A 119.9 . . ?
C26 C27 C28 117.5(8) . . ?
C26 C27 H27A 121.3 . . ?
C28 C27 H27A 121.3 . . ?
N8 C28 C27 122.7(8) . . ?
N8 C28 H28A 118.6 . . ?
C27 C28 H28A 118.6 . . ?
C33 N9 C29 118.8(6) . . ?
C33 N9 Ni3 116.5(4) . . ?
C29 N9 Ni3 124.5(5) . . ?
N11 N10 C34 120.7(5) . . ?
N11 N10 Ni3 121.0(4) . . ?
C34 N10 Ni3 117.9(4) . . ?
N10 N11 C37 120.9(5) . . ?
N10 N11 Ni4 121.6(4) . . ?
C37 N11 Ni4 116.8(4) . . ?
C42 N12 C38 118.3(5) . . ?
C42 N12 Ni4 126.4(4) . . ?
C38 N12 Ni4 114.6(4) . . ?
N9 C29 C30 120.4(8) . . ?
N9 C29 H29 119.8 . . ?
C30 C29 H29 119.8 . . ?
C31 C30 C29 119.1(8) . . ?
C31 C30 H30 120.4 . . ?
C29 C30 H30 120.4 . . ?
C30 C31 C32 120.9(7) . . ?
C30 C31 H31 119.5 . . ?
C32 C31 H31 119.5 . . ?
C33 C32 C31 116.7(8) . . ?
C33 C32 H32 121.6 . . ?
C31 C32 H32 121.6 . . ?
N9 C33 C32 124.1(7) . . ?
N9 C33 C34 113.9(5) . . ?
C32 C33 C34 122.0(7) . . ?
N10 C34 C35 121.3(6) . . ?
N10 C34 C33 113.9(6) . . ?
C35 C34 C33 124.7(5) . . ?
C34 C35 C36 118.5(6) . . ?
C34 C35 H35 120.7 . . ?
C36 C35 H35 120.7 . . ?
C35 C36 C37 117.4(6) . . ?
C35 C36 H36 121.3 . . ?
C37 C36 H36 121.3 . . ?
N11 C37 C36 121.0(6) . . ?
N11 C37 C38 114.7(5) . . ?
C36 C37 C38 124.3(6) . . ?
N12 C38 C39 123.2(6) . . ?
N12 C38 C37 114.4(5) . . ?
C39 C38 C37 122.4(6) . . ?
C40 C39 C38 118.2(6) . . ?
C40 C39 H39 120.9 . . ?
C38 C39 H39 120.9 . . ?
C39 C40 C41 118.5(6) . . ?
C39 C40 H40 120.7 . . ?
C41 C40 H40 120.7 . . ?
C42 C41 C40 119.1(6) . . ?
C42 C41 H41 120.5 . . ?
C40 C41 H41 120.5 . . ?
N12 C42 C41 122.7(6) . . ?
N12 C42 H42 118.6 . . ?
C41 C42 H42 118.6 . . ?
C43 N13 C47 119.5(5) . . ?
C43 N13 Ni4 125.7(4) . . ?
C47 N13 Ni4 114.0(4) . . ?
N15 N14 C48 120.4(4) . . ?
N15 N14 Ni4 121.3(3) . . ?
C48 N14 Ni4 117.6(4) . . ?
N14 N15 C51 120.9(5) . . ?
N14 N15 Ni1 120.9(3) . . ?
C51 N15 Ni1 117.8(4) . . ?
C56 N16 C52 118.3(5) . . ?
C56 N16 Ni1 125.6(4) . . ?
C52 N16 Ni1 116.1(4) . . ?
N13 C43 C44 122.6(6) . . ?
N13 C43 H43 118.7 . . ?
C44 C43 H43 118.7 . . ?
C45 C44 C43 118.0(6) . . ?
C45 C44 H44 121.0 . . ?
C43 C44 H44 121.0 . . ?
C44 C45 C46 119.3(6) . . ?
C44 C45 H45 120.3 . . ?
C46 C45 H45 120.3 . . ?
C47 C46 C45 118.7(6) . . ?
C47 C46 H46 120.7 . . ?
C45 C46 H46 120.7 . . ?
N13 C47 C46 121.8(5) . . ?
N13 C47 C48 115.7(5) . . ?
C46 C47 C48 122.6(5) . . ?
N14 C48 C49 120.3(5) . . ?
N14 C48 C47 113.6(5) . . ?
C49 C48 C47 125.8(5) . . ?
C50 C49 C48 118.8(5) . . ?
C50 C49 H49 120.6 . . ?
C48 C49 H49 120.6 . . ?
C49 C50 C51 118.8(5) . . ?
C49 C50 H50 120.6 . . ?
C51 C50 H50 120.6 . . ?
N15 C51 C50 120.7(5) . . ?
N15 C51 C52 114.4(5) . . ?
C50 C51 C52 124.8(5) . . ?
N16 C52 C53 123.3(6) . . ?
N16 C52 C51 114.0(5) . . ?
C53 C52 C51 122.6(5) . . ?
C52 C53 C54 118.0(6) . . ?
C52 C53 H53 121.0 . . ?
C54 C53 H53 121.0 . . ?
C55 C54 C53 118.9(6) . . ?
C55 C54 H54 120.6 . . ?
C53 C54 H54 120.6 . . ?
C56 C55 C54 118.8(7) . . ?
C56 C55 H55 120.6 . . ?
C54 C55 H55 120.6 . . ?
N16 C56 C55 122.7(6) . . ?
N16 C56 H56 118.6 . . ?
C55 C56 H56 118.6 . . ?

_refine_diff_density_max         2.165
_refine_diff_density_min         -0.895
_refine_diff_density_rms         0.142

_shelxl_version_number           2013-4

