#------------------------------------------------------------------------------
#$Date: 2016-08-06 09:22:25 +0300 (Sat, 06 Aug 2016) $
#$Revision: 185059 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/01/7040184.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7040184
loop_
_publ_author_name
'Perlepe, Panagiota S.'
'Cunha-Silva, Luís'
'Bekiari, Vlasoula'
'Gagnon, Kevin J.'
'Teat, Simon J.'
'Escuer, Albert'
'Stamatatos, Theocharis C.'
_publ_section_title
;
 Structural diversity in Ni(II) cluster chemistry: Ni5, Ni6, and {NiNa2}n
 complexes bearing the Schiff-base ligand
 N-naphthalidene-2-amino-5-chlorobenzoic acid.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10256
_journal_page_last               10270
_journal_paper_doi               10.1039/c6dt01162d
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C84 H70 Cl4 N8 Ni5 O18, 3(C3 H7 N O)'
_chemical_formula_sum            'C93 H91 Cl4 N11 Ni5 O21'
_chemical_formula_weight         2134.11
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             '19 May 2016'
_audit_creation_method           'SHELXL-2014/7 and enCIFer'
_audit_update_record
;
2016-05-20 deposited with the CCDC.
2016-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                92.408(2)
_cell_angle_beta                 99.389(2)
_cell_angle_gamma                116.998(2)
_cell_formula_units_Z            1
_cell_length_a                   14.1417(10)
_cell_length_b                   14.1587(10)
_cell_length_c                   14.7117(11)
_cell_measurement_reflns_used    8253
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.42
_cell_measurement_theta_min      2.62
_cell_volume                     2566.8(3)
_computing_cell_refinement       'SAINT (Bruker AXS Inc., 2012)'
_computing_data_collection       'APEX2 (Bruker AXS Inc., 2012)'
_computing_data_reduction        'SAINT (Bruker AXS Inc., 2012)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.924
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device_type  'Bruker X8 Kappa CCD APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0628
_diffrn_reflns_Laue_measured_fraction_full 0.924
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20519
_diffrn_reflns_point_group_measured_fraction_full 0.924
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.977
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.075
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_correction_T_min  0.879
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
'SADABS V2012/1 (Bruker AXS Inc.)' 
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_description       plate
_exptl_crystal_F_000             1102
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.699
_refine_diff_density_min         -1.008
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     607
_refine_ls_number_reflns         8395
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.1143
_refine_ls_R_factor_gt           0.0974
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0722P)²+26.5167P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2184
_refine_ls_wR_factor_ref         0.2268
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7062
_reflns_number_total             8395
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt01162d1.cif
_cod_data_source_block           comp2_rev
_cod_database_code               7040184
_shelx_shelxl_version_number     2014/7
_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.
;
_shelx_estimated_absorpt_t_min   0.739
_shelx_estimated_absorpt_t_max   0.968
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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 0.5000 0.5000 0.0000 0.0108(3) Uani 1 2 d S . P . .
Ni2 Ni 0.26885(8) 0.39960(7) -0.11519(6) 0.0133(2) Uani 1 1 d . . . . .
Ni3 Ni 0.33513(8) 0.32313(8) 0.07662(6) 0.0150(3) Uani 1 1 d . . . . .
Cl1 Cl 0.3211(3) 0.6780(2) 0.44932(19) 0.0582(8) Uani 1 1 d . . . . .
Cl2 Cl 0.3427(2) 0.85211(19) -0.35563(16) 0.0367(6) Uani 1 1 d . . . . .
O1 O 0.3735(4) 0.3521(4) -0.0506(3) 0.0137(11) Uani 1 1 d . . . . .
H1 H 0.3874 0.2994 -0.0861 0.016 Uiso 1 1 calc R U . . .
O2 O 0.3977(4) 0.5535(4) -0.0661(3) 0.0127(10) Uani 1 1 d . . . . .
O3 O 0.5213(4) 0.6895(4) -0.1230(4) 0.0189(12) Uani 1 1 d . . . . .
O4 O 0.2128(4) 0.3618(4) 0.0045(4) 0.0174(11) Uani 1 1 d . . . . .
O5 O 0.4288(4) 0.4832(4) 0.1106(3) 0.0144(11) Uani 1 1 d . . . . .
O6 O 0.4864(5) 0.6524(5) 0.1695(4) 0.0311(14) Uani 1 1 d . . . . .
O7 O 0.2515(4) 0.1638(4) 0.0586(4) 0.0209(12) Uani 1 1 d . . . . .
O8 O 0.3256(4) 0.4282(4) -0.2371(3) 0.0191(12) Uani 1 1 d . . . . .
O9 O 0.1472(5) 0.2540(4) -0.1851(4) 0.0242(13) Uani 1 1 d . . . . .
N1 N 0.1838(5) 0.4813(5) -0.1403(4) 0.0169(14) Uani 1 1 d . . . . .
N2 N 0.3078(5) 0.3236(5) 0.2088(4) 0.0197(14) Uani 1 1 d . . . . .
N3 N 0.3729(6) 0.3956(6) -0.3696(5) 0.0301(17) Uani 1 1 d . . . . .
N4 N 0.0394(5) 0.0783(5) -0.1801(5) 0.0239(15) Uani 1 1 d . . . . .
C1 C 0.4262(6) 0.6283(6) -0.1188(5) 0.0138(16) Uani 1 1 d . . . . .
C2 C 0.3363(6) 0.6390(6) -0.1814(5) 0.0162(16) Uani 1 1 d . . . . .
C3 C 0.2248(7) 0.5731(7) -0.1894(5) 0.0213(18) Uani 1 1 d . . . . .
C4 C 0.1023(6) 0.4632(7) -0.1038(5) 0.0199(17) Uani 1 1 d . . . . .
H4 H 0.0705 0.5091 -0.1152 0.024 Uiso 1 1 calc R U . . .
C5 C 0.0527(6) 0.3800(6) -0.0466(5) 0.0192(17) Uani 1 1 d . . . . .
C6 C 0.1138(6) 0.3401(6) 0.0085(5) 0.0125(15) Uani 1 1 d . . . . .
C7 C 0.4304(6) 0.5536(7) 0.1692(5) 0.0193(17) Uani 1 1 d . . . . .
C8 C 0.3638(7) 0.5165(7) 0.2428(5) 0.0231(18) Uani 1 1 d . . . . .
C9 C 0.3040(7) 0.4107(6) 0.2560(5) 0.0196(17) Uani 1 1 d . . . . .
C10 C 0.3090(6) 0.2487(6) 0.2551(5) 0.0192(17) Uani 1 1 d . . . . .
H10 H 0.3131 0.2597 0.3201 0.023 Uiso 1 1 calc R U . . .
C11 C 0.3048(6) 0.1512(6) 0.2196(5) 0.0156(16) Uani 1 1 d . . . . .
C12 C 0.2688(6) 0.1100(6) 0.1234(6) 0.0197(17) Uani 1 1 d . . . . .
C13 C 0.2453(7) 0.0022(7) 0.0958(6) 0.029(2) Uani 1 1 d . . . . .
H13 H 0.2160 -0.0276 0.0324 0.034 Uiso 1 1 calc R U . . .
C14 C 0.2638(7) -0.0589(6) 0.1584(6) 0.0259(19) Uani 1 1 d . . . . .
H14 H 0.2467 -0.1303 0.1373 0.031 Uiso 1 1 calc R U . . .
C15 C 0.3078(7) -0.0193(6) 0.2541(6) 0.0228(18) Uani 1 1 d . . . . .
C16 C 0.3287(6) 0.0868(6) 0.2865(5) 0.0191(17) Uani 1 1 d . . . . .
C17 C 0.3748(7) 0.1237(7) 0.3807(6) 0.0250(19) Uani 1 1 d . . . . .
H17 H 0.3931 0.1948 0.4037 0.030 Uiso 1 1 calc R U . . .
C18 C 0.3944(8) 0.0608(8) 0.4404(6) 0.035(2) Uani 1 1 d . . . . .
H18 H 0.4237 0.0888 0.5042 0.042 Uiso 1 1 calc R U . . .
C19 C 0.3726(8) -0.0438(8) 0.4109(7) 0.037(2) Uani 1 1 d . . . . .
H19 H 0.3862 -0.0862 0.4543 0.045 Uiso 1 1 calc R U . . .
C20 C 0.3327(7) -0.0830(7) 0.3214(6) 0.030(2) Uani 1 1 d . . . . .
H20 H 0.3202 -0.1529 0.3006 0.036 Uiso 1 1 calc R U . . .
C21 C 0.2357(7) 0.3883(7) 0.3218(6) 0.027(2) Uani 1 1 d . . . . .
H21 H 0.1887 0.3159 0.3269 0.033 Uiso 1 1 calc R U . . .
C22 C 0.2357(8) 0.4676(7) 0.3779(6) 0.032(2) Uani 1 1 d . . . . .
H22 H 0.1887 0.4513 0.4208 0.038 Uiso 1 1 calc R U . . .
C23 C 0.3072(9) 0.5738(8) 0.3704(6) 0.037(2) Uani 1 1 d . . . . .
C24 C 0.3663(8) 0.5991(7) 0.3020(6) 0.028(2) Uani 1 1 d . . . . .
H24 H 0.4089 0.6718 0.2945 0.033 Uiso 1 1 calc R U . . .
C25 C 0.0643(6) 0.2757(6) 0.0784(6) 0.0217(17) Uani 1 1 d . . . . .
H25 H 0.1050 0.2501 0.1182 0.026 Uiso 1 1 calc R U . . .
C26 C -0.0375(7) 0.2507(7) 0.0891(6) 0.0228(18) Uani 1 1 d . . . . .
H26 H -0.0655 0.2097 0.1368 0.027 Uiso 1 1 calc R U . . .
C27 C -0.1030(6) 0.2847(6) 0.0301(5) 0.0198(17) Uani 1 1 d . . . . .
C28 C -0.0581(6) 0.3495(6) -0.0391(5) 0.0199(17) Uani 1 1 d . . . . .
C29 C -0.1274(7) 0.3784(7) -0.0977(6) 0.0263(19) Uani 1 1 d . . . . .
H29 H -0.1007 0.4202 -0.1454 0.032 Uiso 1 1 calc R U . . .
C30 C -0.2316(7) 0.3486(8) -0.0885(6) 0.033(2) Uani 1 1 d . . . . .
H30 H -0.2753 0.3706 -0.1289 0.039 Uiso 1 1 calc R U . . .
C31 C -0.2741(7) 0.2858(7) -0.0197(6) 0.029(2) Uani 1 1 d . . . . .
H31 H -0.3463 0.2657 -0.0132 0.035 Uiso 1 1 calc R U . . .
C32 C -0.2116(7) 0.2537(7) 0.0378(6) 0.0259(19) Uani 1 1 d . . . . .
H32 H -0.2411 0.2100 0.0836 0.031 Uiso 1 1 calc R U . . .
C33 C 0.1516(7) 0.5935(8) -0.2503(6) 0.034(2) Uani 1 1 d . . . . .
H33 H 0.0760 0.5478 -0.2573 0.040 Uiso 1 1 calc R U . . .
C34 C 0.1871(8) 0.6790(8) -0.3007(7) 0.036(2) Uani 1 1 d . . . . .
H34 H 0.1364 0.6924 -0.3415 0.043 Uiso 1 1 calc R U . . .
C35 C 0.2966(8) 0.7444(7) -0.2914(6) 0.029(2) Uani 1 1 d . . . . .
C36 C 0.3708(7) 0.7258(6) -0.2333(5) 0.0206(17) Uani 1 1 d . . . . .
H36 H 0.4461 0.7718 -0.2280 0.025 Uiso 1 1 calc R U . . .
C37 C 0.3287(7) 0.3656(7) -0.2958(5) 0.0223(18) Uani 1 1 d . . . . .
H37 H 0.2978 0.2920 -0.2880 0.027 Uiso 1 1 calc R U . . .
C38 C 0.3685(9) 0.3173(10) -0.4405(7) 0.050(3) Uani 1 1 d . . . . .
H38A H 0.3432 0.2475 -0.4180 0.074 Uiso 1 1 calc R U . . .
H38B H 0.4410 0.3404 -0.4536 0.074 Uiso 1 1 calc R U . . .
H38C H 0.3184 0.3116 -0.4975 0.074 Uiso 1 1 calc R U . . .
C39 C 0.4190(9) 0.5072(9) -0.3847(7) 0.043(3) Uani 1 1 d . . . . .
H39A H 0.3706 0.5159 -0.4355 0.065 Uiso 1 1 calc R U . . .
H39B H 0.4900 0.5296 -0.4008 0.065 Uiso 1 1 calc R U . . .
H39C H 0.4274 0.5513 -0.3278 0.065 Uiso 1 1 calc R U . . .
C40 C 0.1204(7) 0.1721(7) -0.1448(5) 0.0208(18) Uani 1 1 d . . . . .
H40 H 0.1616 0.1785 -0.0849 0.025 Uiso 1 1 calc R U . . .
C41 C 0.0140(8) -0.0138(7) -0.1304(7) 0.038(2) Uani 1 1 d . . . . .
H41A H 0.0674 0.0065 -0.0721 0.057 Uiso 1 1 calc R U . . .
H41B H 0.0159 -0.0709 -0.1687 0.057 Uiso 1 1 calc R U . . .
H41C H -0.0586 -0.0391 -0.1168 0.057 Uiso 1 1 calc R U . . .
C42 C -0.0280(9) 0.0632(9) -0.2692(7) 0.049(3) Uani 1 1 d . . . . .
H42A H -0.0974 0.0580 -0.2607 0.073 Uiso 1 1 calc R U . . .
H42B H -0.0408 -0.0028 -0.3052 0.073 Uiso 1 1 calc R U . . .
H42C H 0.0082 0.1240 -0.3024 0.073 Uiso 1 1 calc R U . . .
O12 O -0.0100(19) 0.1656(19) 0.3147(15) 0.091(6) Uiso 0.5 1 d . . P . .
N7 N -0.053(2) 0.087(2) 0.4350(17) 0.073(6) Uiso 0.5 1 d . . P . .
C51 C -0.072(3) 0.117(3) 0.363(2) 0.079(8) Uiso 0.5 1 d . . P . .
H51 H -0.1458 0.1003 0.3414 0.095 Uiso 0.5 1 calc R U P . .
C50 C 0.057(3) 0.115(3) 0.475(2) 0.103(11) Uiso 0.5 1 d . . P . .
H50A H 0.1052 0.1650 0.4385 0.154 Uiso 0.5 1 calc R U P A 2
H50B H 0.0664 0.0504 0.4739 0.154 Uiso 0.5 1 calc R U P A 2
H50C H 0.0752 0.1488 0.5389 0.154 Uiso 0.5 1 calc R U P A 2
C49 C -0.141(4) 0.016(4) 0.482(3) 0.150(17) Uiso 0.5 1 d . . P . .
H49A H -0.1087 0.0000 0.5394 0.225 Uiso 0.25 1 calc R U P . .
H49B H -0.1824 0.0521 0.4957 0.225 Uiso 0.25 1 calc R U P . .
H49C H -0.1887 -0.0509 0.4402 0.225 Uiso 0.25 1 calc R U P . .
H49D H -0.2112 0.0008 0.4442 0.225 Uiso 0.25 1 calc R U P . .
H49E H -0.1374 -0.0513 0.4878 0.225 Uiso 0.25 1 calc R U P . .
H49F H -0.1312 0.0517 0.5433 0.225 Uiso 0.25 1 calc R U P . .
N5 N 0.6103(15) 0.9224(14) 0.1775(12) 0.044(4) Uiso 0.5 1 d . . P . .
O10 O 0.6395(18) 0.8782(18) 0.3098(15) 0.090(6) Uiso 0.5 1 d . . P . .
C44 C 0.698(2) 0.935(2) 0.1556(19) 0.067(7) Uiso 0.5 1 d . . P . .
H44A H 0.7486 1.0116 0.1619 0.101 Uiso 0.5 1 calc R U P . .
H44B H 0.6829 0.9032 0.0911 0.101 Uiso 0.5 1 calc R U P . .
H44C H 0.7303 0.9001 0.1968 0.101 Uiso 0.5 1 calc R U P . .
C45 C 0.569(3) 0.897(3) 0.248(2) 0.089(9) Uiso 0.5 1 d . . P . .
H45 H 0.5017 0.8923 0.2570 0.107 Uiso 0.5 1 calc R U P . .
C43 C 0.548(4) 0.953(4) 0.113(3) 0.145(17) Uiso 0.5 1 d . . P . .
H43A H 0.5865 1.0305 0.1128 0.217 Uiso 0.5 1 calc R U P . .
H43B H 0.4782 0.9337 0.1313 0.217 Uiso 0.5 1 calc R U P . .
H43C H 0.5350 0.9161 0.0513 0.217 Uiso 0.5 1 calc R U P . .
N6 N -0.0100(17) 0.3450(17) 0.6046(13) 0.057(5) Uiso 0.5 1 d . . P . .
C48 C 0.0902(18) 0.3594(18) 0.6133(15) 0.043(5) Uiso 0.5 1 d . . P . .
H48 H 0.1220 0.3491 0.6716 0.052 Uiso 0.5 1 calc R U P . .
O11 O 0.137(2) 0.380(2) 0.5650(17) 0.106(7) Uiso 0.5 1 d . . P . .
C47 C -0.068(2) 0.311(2) 0.6794(16) 0.055(6) Uiso 0.5 1 d . . P . .
H47A H -0.0165 0.3202 0.7367 0.082 Uiso 0.5 1 calc R U P . .
H47B H -0.1220 0.2357 0.6636 0.082 Uiso 0.5 1 calc R U P . .
H47C H -0.1040 0.3546 0.6885 0.082 Uiso 0.5 1 calc R U P . .
C46 C -0.034(5) 0.414(5) 0.524(4) 0.19(2) Uiso 0.5 1 d . . P . .
H46A H -0.0464 0.4700 0.5527 0.283 Uiso 0.5 1 calc R U P . .
H46B H -0.0975 0.3663 0.4767 0.283 Uiso 0.5 1 calc R U P . .
H46C H 0.0294 0.4476 0.4947 0.283 Uiso 0.5 1 calc R U P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O5 Ni1 O5 180.0 . 2_665
O5 Ni1 O1 95.9(2) . 2_665
O5 Ni1 O1 84.1(2) 2_665 2_665
O5 Ni1 O1 84.1(2) . .
O5 Ni1 O1 95.9(2) 2_665 .
O1 Ni1 O1 180.0 2_665 .
O5 Ni1 O2 90.67(18) . 2_665
O5 Ni1 O2 89.33(18) 2_665 2_665
O1 Ni1 O2 83.92(19) 2_665 2_665
O1 Ni1 O2 96.08(19) . 2_665
O5 Ni1 O2 89.33(18) . .
O5 Ni1 O2 90.67(18) 2_665 .
O1 Ni1 O2 96.08(19) 2_665 .
O1 Ni1 O2 83.92(19) . .
O2 Ni1 O2 180.00(19) 2_665 .
O5 Ni1 Ni3 136.98(14) . 2_665
O5 Ni1 Ni3 43.02(14) 2_665 2_665
O1 Ni1 Ni3 43.46(13) 2_665 2_665
O1 Ni1 Ni3 136.54(13) . 2_665
O2 Ni1 Ni3 96.67(13) 2_665 2_665
O2 Ni1 Ni3 83.33(13) . 2_665
O5 Ni1 Ni3 43.02(14) . .
O5 Ni1 Ni3 136.98(14) 2_665 .
O1 Ni1 Ni3 136.54(13) 2_665 .
O1 Ni1 Ni3 43.46(13) . .
O2 Ni1 Ni3 83.33(13) 2_665 .
O2 Ni1 Ni3 96.67(13) . .
Ni3 Ni1 Ni3 180.0 2_665 .
O1 Ni2 N1 160.8(2) . .
O1 Ni2 O4 79.54(19) . .
N1 Ni2 O4 89.8(2) . .
O1 Ni2 O8 97.9(2) . .
N1 Ni2 O8 93.4(2) . .
O4 Ni2 O8 176.2(2) . .
O1 Ni2 O9 99.8(2) . .
N1 Ni2 O9 96.1(2) . .
O4 Ni2 O9 90.2(2) . .
O8 Ni2 O9 87.5(2) . .
O1 Ni2 O2 83.40(19) . .
N1 Ni2 O2 82.6(2) . .
O4 Ni2 O2 99.2(2) . .
O8 Ni2 O2 83.2(2) . .
O9 Ni2 O2 170.5(2) . .
O7 Ni3 O5 172.9(2) . .
O7 Ni3 O1 101.4(2) . .
O5 Ni3 O1 83.9(2) . .
O7 Ni3 N2 88.9(2) . .
O5 Ni3 N2 85.9(2) . .
O1 Ni3 N2 169.6(2) . .
O7 Ni3 O3 88.8(2) . 2_665
O5 Ni3 O3 86.4(2) . 2_665
O1 Ni3 O3 90.64(19) . 2_665
N2 Ni3 O3 91.1(2) . 2_665
O7 Ni3 O4 100.1(2) . .
O5 Ni3 O4 85.7(2) . .
O1 Ni3 O4 75.85(18) . .
N2 Ni3 O4 101.0(2) . .
O3 Ni3 O4 165.00(19) 2_665 .
O7 Ni3 Ni1 140.64(16) . .
O5 Ni3 Ni1 42.78(13) . .
O1 Ni3 Ni1 43.54(14) . .
N2 Ni3 Ni1 127.20(19) . .
O3 Ni3 Ni1 76.83(14) 2_665 .
O4 Ni3 Ni1 88.74(13) . .
Ni2 O1 Ni3 105.0(2) . .
Ni2 O1 Ni1 97.9(2) . .
Ni3 O1 Ni1 93.0(2) . .
Ni2 O1 H1 118.8 . .
Ni3 O1 H1 118.8 . .
Ni1 O1 H1 118.8 . .
C1 O2 Ni1 123.9(5) . .
C1 O2 Ni2 121.7(5) . .
Ni1 O2 Ni2 94.74(19) . .
C1 O3 Ni3 130.0(4) . 2_665
C6 O4 Ni2 120.8(4) . .
C6 O4 Ni3 136.6(4) . .
Ni2 O4 Ni3 99.3(2) . .
C7 O5 Ni1 130.5(5) . .
C7 O5 Ni3 134.2(5) . .
Ni1 O5 Ni3 94.2(2) . .
C12 O7 Ni3 119.8(5) . .
C37 O8 Ni2 129.4(5) . .
C40 O9 Ni2 119.4(5) . .
C4 N1 C3 118.0(6) . .
C4 N1 Ni2 121.9(5) . .
C3 N1 Ni2 119.4(5) . .
C10 N2 C9 118.5(7) . .
C10 N2 Ni3 118.3(5) . .
C9 N2 Ni3 122.5(5) . .
C37 N3 C39 119.7(7) . .
C37 N3 C38 121.4(8) . .
C39 N3 C38 118.7(8) . .
C40 N4 C42 121.1(7) . .
C40 N4 C41 121.3(7) . .
C42 N4 C41 117.6(8) . .
O3 C1 O2 124.5(6) . .
O3 C1 C2 118.3(6) . .
O2 C1 C2 117.1(7) . .
C3 C2 C36 118.8(7) . .
C3 C2 C1 125.9(7) . .
C36 C2 C1 115.3(7) . .
C33 C3 C2 119.1(7) . .
C33 C3 N1 119.1(7) . .
C2 C3 N1 121.7(7) . .
N1 C4 C5 127.1(7) . .
N1 C4 H4 116.4 . .
C5 C4 H4 116.4 . .
C6 C5 C28 120.8(7) . .
C6 C5 C4 121.2(7) . .
C28 C5 C4 117.6(6) . .
O4 C6 C5 124.6(6) . .
O4 C6 C25 118.4(6) . .
C5 C6 C25 116.9(6) . .
O6 C7 O5 123.3(7) . .
O6 C7 C8 118.1(7) . .
O5 C7 C8 118.6(7) . .
C9 C8 C24 119.9(8) . .
C9 C8 C7 125.1(7) . .
C24 C8 C7 115.0(8) . .
C8 C9 N2 124.0(7) . .
C8 C9 C21 118.1(7) . .
N2 C9 C21 117.9(7) . .
N2 C10 C11 127.2(7) . .
N2 C10 H10 116.4 . .
C11 C10 H10 116.4 . .
C12 C11 C10 122.3(7) . .
C12 C11 C16 119.3(7) . .
C10 C11 C16 118.1(7) . .
O7 C12 C11 123.6(7) . .
O7 C12 C13 117.6(7) . .
C11 C12 C13 118.8(7) . .
C14 C13 C12 121.6(8) . .
C14 C13 H13 119.2 . .
C12 C13 H13 119.2 . .
C13 C14 C15 122.1(8) . .
C13 C14 H14 118.9 . .
C15 C14 H14 118.9 . .
C14 C15 C16 118.7(7) . .
C14 C15 C20 122.4(7) . .
C16 C15 C20 118.8(7) . .
C17 C16 C15 116.9(7) . .
C17 C16 C11 124.0(7) . .
C15 C16 C11 119.1(7) . .
C18 C17 C16 122.0(8) . .
C18 C17 H17 119.0 . .
C16 C17 H17 119.0 . .
C17 C18 C19 122.2(9) . .
C17 C18 H18 118.9 . .
C19 C18 H18 118.9 . .
C20 C19 C18 119.2(8) . .
C20 C19 H19 120.4 . .
C18 C19 H19 120.4 . .
C19 C20 C15 120.8(8) . .
C19 C20 H20 119.6 . .
C15 C20 H20 119.6 . .
C22 C21 C9 122.1(8) . .
C22 C21 H21 119.0 . .
C9 C21 H21 119.0 . .
C21 C22 C23 118.0(8) . .
C21 C22 H22 121.0 . .
C23 C22 H22 121.0 . .
C24 C23 C22 121.6(8) . .
C24 C23 Cl1 118.6(8) . .
C22 C23 Cl1 119.8(7) . .
C23 C24 C8 119.6(9) . .
C23 C24 H24 120.2 . .
C8 C24 H24 120.2 . .
C26 C25 C6 122.7(7) . .
C26 C25 H25 118.6 . .
C6 C25 H25 118.6 . .
C25 C26 C27 121.1(7) . .
C25 C26 H26 119.4 . .
C27 C26 H26 119.4 . .
C32 C27 C26 121.3(7) . .
C32 C27 C28 120.0(7) . .
C26 C27 C28 118.7(7) . .
C29 C28 C27 116.5(7) . .
C29 C28 C5 123.9(7) . .
C27 C28 C5 119.6(7) . .
C30 C29 C28 122.5(8) . .
C30 C29 H29 118.8 . .
C28 C29 H29 118.8 . .
C29 C30 C31 120.4(8) . .
C29 C30 H30 119.8 . .
C31 C30 H30 119.8 . .
C32 C31 C30 119.8(7) . .
C32 C31 H31 120.1 . .
C30 C31 H31 120.1 . .
C31 C32 C27 120.8(8) . .
C31 C32 H32 119.6 . .
C27 C32 H32 119.6 . .
C34 C33 C3 121.2(9) . .
C34 C33 H33 119.4 . .
C3 C33 H33 119.4 . .
C35 C34 C33 119.4(8) . .
C35 C34 H34 120.3 . .
C33 C34 H34 120.3 . .
C36 C35 C34 121.0(7) . .
C36 C35 Cl2 119.1(7) . .
C34 C35 Cl2 119.8(6) . .
C35 C36 C2 120.5(8) . .
C35 C36 H36 119.7 . .
C2 C36 H36 119.7 . .
O8 C37 N3 123.4(8) . .
O8 C37 H37 118.3 . .
N3 C37 H37 118.3 . .
N3 C38 H38A 109.5 . .
N3 C38 H38B 109.5 . .
H38A C38 H38B 109.5 . .
N3 C38 H38C 109.5 . .
H38A C38 H38C 109.5 . .
H38B C38 H38C 109.5 . .
N3 C39 H39A 109.5 . .
N3 C39 H39B 109.5 . .
H39A C39 H39B 109.5 . .
N3 C39 H39C 109.5 . .
H39A C39 H39C 109.5 . .
H39B C39 H39C 109.5 . .
O9 C40 N4 124.2(7) . .
O9 C40 H40 117.9 . .
N4 C40 H40 117.9 . .
N4 C41 H41A 109.5 . .
N4 C41 H41B 109.5 . .
H41A C41 H41B 109.5 . .
N4 C41 H41C 109.5 . .
H41A C41 H41C 109.5 . .
H41B C41 H41C 109.5 . .
N4 C42 H42A 109.5 . .
N4 C42 H42B 109.5 . .
H42A C42 H42B 109.5 . .
N4 C42 H42C 109.5 . .
H42A C42 H42C 109.5 . .
H42B C42 H42C 109.5 . .
C51 N7 C50 119(3) . .
C51 N7 C49 121(3) . .
C50 N7 C49 119(3) . .
N7 C51 O12 128(3) . .
N7 C51 H51 116.1 . .
O12 C51 H51 116.1 . .
N7 C50 H50A 109.5 . .
N7 C50 H50B 109.5 . .
H50A C50 H50B 109.5 . .
N7 C50 H50C 109.5 . .
H50A C50 H50C 109.5 . .
H50B C50 H50C 109.5 . .
N7 C49 H49A 109.5 . .
N7 C49 H49B 109.5 . .
H49A C49 H49B 109.5 . .
N7 C49 H49C 109.5 . .
H49A C49 H49C 109.5 . .
H49B C49 H49C 109.5 . .
N7 C49 H49D 109.5 . .
H49A C49 H49D 141.1 . .
H49B C49 H49D 56.3 . .
H49C C49 H49D 56.3 . .
N7 C49 H49E 109.5 . .
H49A C49 H49E 56.3 . .
H49B C49 H49E 141.1 . .
H49C C49 H49E 56.3 . .
H49D C49 H49E 109.5 . .
N7 C49 H49F 109.5 . .
H49A C49 H49F 56.3 . .
H49B C49 H49F 56.3 . .
H49C C49 H49F 141.1 . .
H49D C49 H49F 109.5 . .
H49E C49 H49F 109.5 . .
C45 N5 C44 135(3) . .
C45 N5 C43 111(3) . .
C44 N5 C43 114(3) . .
N5 C44 H44A 109.5 . .
N5 C44 H44B 109.5 . .
H44A C44 H44B 109.5 . .
N5 C44 H44C 109.5 . .
H44A C44 H44C 109.5 . .
H44B C44 H44C 109.5 . .
N5 C45 O10 106(3) . .
N5 C45 H45 126.8 . .
O10 C45 H45 126.8 . .
N5 C43 H43A 109.5 . .
N5 C43 H43B 109.5 . .
H43A C43 H43B 109.5 . .
N5 C43 H43C 109.5 . .
H43A C43 H43C 109.5 . .
H43B C43 H43C 109.5 . .
C48 N6 C47 121(2) . .
C48 N6 C46 110(3) . .
C47 N6 C46 125(3) . .
O11 C48 N6 127(3) . .
O11 C48 H48 116.3 . .
N6 C48 H48 116.3 . .
N6 C47 H47A 109.5 . .
N6 C47 H47B 109.5 . .
H47A C47 H47B 109.5 . .
N6 C47 H47C 109.5 . .
H47A C47 H47C 109.5 . .
H47B C47 H47C 109.5 . .
N6 C46 H46A 109.5 . .
N6 C46 H46B 109.5 . .
H46A C46 H46B 109.5 . .
N6 C46 H46C 109.5 . .
H46A C46 H46C 109.5 . .
H46B C46 H46C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O5 2.017(5) .
Ni1 O5 2.017(5) 2_665
Ni1 O1 2.043(5) 2_665
Ni1 O1 2.043(5) .
Ni1 O2 2.052(4) 2_665
Ni1 O2 2.052(4) .
Ni1 Ni3 2.9616(9) 2_665
Ni1 Ni3 2.9616(9) .
Ni2 O1 2.011(5) .
Ni2 N1 2.018(6) .
Ni2 O4 2.042(5) .
Ni2 O8 2.064(5) .
Ni2 O9 2.072(6) .
Ni2 O2 2.104(5) .
Ni3 O7 1.996(5) .
Ni3 O5 2.026(5) .
Ni3 O1 2.040(5) .
Ni3 N2 2.044(6) .
Ni3 O3 2.122(5) 2_665
Ni3 O4 2.175(5) .
Cl1 C23 1.756(9) .
Cl2 C35 1.750(8) .
O1 H1 1.0000 .
O2 C1 1.291(8) .
O3 C1 1.240(9) .
O3 Ni3 2.122(5) 2_665
O4 C6 1.301(8) .
O5 C7 1.279(9) .
O6 C7 1.256(10) .
O7 C12 1.305(9) .
O8 C37 1.231(9) .
O9 C40 1.253(9) .
N1 C4 1.277(10) .
N1 C3 1.442(10) .
N2 C10 1.289(10) .
N2 C9 1.416(10) .
N3 C37 1.331(10) .
N3 C39 1.453(12) .
N3 C38 1.463(12) .
N4 C40 1.309(11) .
N4 C42 1.432(12) .
N4 C41 1.450(11) .
C1 C2 1.514(10) .
C2 C3 1.402(11) .
C2 C36 1.410(10) .
C3 C33 1.397(11) .
C4 C5 1.452(10) .
C4 H4 0.9500 .
C5 C6 1.407(10) .
C5 C28 1.449(11) .
C6 C25 1.453(10) .
C7 C8 1.506(11) .
C8 C9 1.387(12) .
C8 C24 1.412(11) .
C9 C21 1.422(11) .
C10 C11 1.428(11) .
C10 H10 0.9500 .
C11 C12 1.425(11) .
C11 C16 1.470(10) .
C12 C13 1.431(12) .
C13 C14 1.364(11) .
C13 H13 0.9500 .
C14 C15 1.419(12) .
C14 H14 0.9500 .
C15 C16 1.436(11) .
C15 C20 1.471(11) .
C16 C17 1.398(12) .
C17 C18 1.359(11) .
C17 H17 0.9500 .
C18 C19 1.402(14) .
C18 H18 0.9500 .
C19 C20 1.332(13) .
C19 H19 0.9500 .
C20 H20 0.9500 .
C21 C22 1.365(12) .
C21 H21 0.9500 .
C22 C23 1.402(14) .
C22 H22 0.9500 .
C23 C24 1.368(12) .
C24 H24 0.9500 .
C25 C26 1.356(11) .
C25 H25 0.9500 .
C26 C27 1.421(11) .
C26 H26 0.9500 .
C27 C32 1.419(11) .
C27 C28 1.429(11) .
C28 C29 1.411(11) .
C29 C30 1.368(12) .
C29 H29 0.9500 .
C30 C31 1.402(13) .
C30 H30 0.9500 .
C31 C32 1.363(12) .
C31 H31 0.9500 .
C32 H32 0.9500 .
C33 C34 1.383(12) .
C33 H33 0.9500 .
C34 C35 1.376(13) .
C34 H34 0.9500 .
C35 C36 1.371(11) .
C36 H36 0.9500 .
C37 H37 0.9500 .
C38 H38A 0.9800 .
C38 H38B 0.9800 .
C38 H38C 0.9800 .
C39 H39A 0.9800 .
C39 H39B 0.9800 .
C39 H39C 0.9800 .
C40 H40 0.9500 .
C41 H41A 0.9800 .
C41 H41B 0.9800 .
C41 H41C 0.9800 .
C42 H42A 0.9800 .
C42 H42B 0.9800 .
C42 H42C 0.9800 .
O12 C51 1.20(3) .
N7 C51 1.20(3) .
N7 C50 1.42(4) .
N7 C49 1.49(5) .
C51 H51 0.9500 .
C50 H50A 0.9800 .
C50 H50B 0.9800 .
C50 H50C 0.9800 .
C49 H49A 0.9800 .
C49 H49B 0.9800 .
C49 H49C 0.9800 .
C49 H49D 0.9800 .
C49 H49E 0.9800 .
C49 H49F 0.9800 .
N5 C45 1.26(3) .
N5 C44 1.27(3) .
N5 C43 1.40(4) .
O10 C45 1.36(4) .
C44 H44A 0.9800 .
C44 H44B 0.9800 .
C44 H44C 0.9800 .
C45 H45 0.9500 .
C43 H43A 0.9800 .
C43 H43B 0.9800 .
C43 H43C 0.9800 .
N6 C48 1.32(3) .
N6 C47 1.44(3) .
N6 C46 1.66(5) .
C48 O11 1.01(3) .
C48 H48 0.9500 .
C47 H47A 0.9800 .
C47 H47B 0.9800 .
C47 H47C 0.9800 .
C46 H46A 0.9800 .
C46 H46B 0.9800 .
C46 H46C 0.9800 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
Ni3 O3 C1 O2 16.1(11) 2_665
Ni3 O3 C1 C2 -162.2(5) 2_665
Ni1 O2 C1 O3 -13.6(10) .
Ni2 O2 C1 O3 -135.8(6) .
Ni1 O2 C1 C2 164.7(4) .
Ni2 O2 C1 C2 42.5(8) .
O3 C1 C2 C3 176.4(7) .
O2 C1 C2 C3 -2.0(11) .
O3 C1 C2 C36 -5.6(10) .
O2 C1 C2 C36 176.0(6) .
C36 C2 C3 C33 1.9(12) .
C1 C2 C3 C33 179.9(8) .
C36 C2 C3 N1 178.3(7) .
C1 C2 C3 N1 -3.8(12) .
C4 N1 C3 C33 -44.5(11) .
Ni2 N1 C3 C33 144.6(7) .
C4 N1 C3 C2 139.2(8) .
Ni2 N1 C3 C2 -31.8(10) .
C3 N1 C4 C5 -175.7(8) .
Ni2 N1 C4 C5 -5.0(12) .
N1 C4 C5 C6 28.7(13) .
N1 C4 C5 C28 -159.0(8) .
Ni2 O4 C6 C5 -27.4(9) .
Ni3 O4 C6 C5 177.8(5) .
Ni2 O4 C6 C25 156.6(5) .
Ni3 O4 C6 C25 1.9(11) .
C28 C5 C6 O4 178.5(7) .
C4 C5 C6 O4 -9.5(12) .
C28 C5 C6 C25 -5.5(11) .
C4 C5 C6 C25 166.5(7) .
Ni1 O5 C7 O6 -4.4(10) .
Ni3 O5 C7 O6 -169.1(5) .
Ni1 O5 C7 C8 176.9(4) .
Ni3 O5 C7 C8 12.1(10) .
O6 C7 C8 C9 -175.2(7) .
O5 C7 C8 C9 3.7(11) .
O6 C7 C8 C24 3.9(10) .
O5 C7 C8 C24 -177.3(7) .
C24 C8 C9 N2 -171.2(7) .
C7 C8 C9 N2 7.8(12) .
C24 C8 C9 C21 8.0(11) .
C7 C8 C9 C21 -173.0(7) .
C10 N2 C9 C8 138.7(8) .
Ni3 N2 C9 C8 -31.5(10) .
C10 N2 C9 C21 -40.5(10) .
Ni3 N2 C9 C21 149.3(6) .
C9 N2 C10 C11 175.1(8) .
Ni3 N2 C10 C11 -14.3(11) .
N2 C10 C11 C12 -17.8(13) .
N2 C10 C11 C16 168.1(8) .
Ni3 O7 C12 C11 28.7(10) .
Ni3 O7 C12 C13 -154.3(6) .
C10 C11 C12 O7 9.9(12) .
C16 C11 C12 O7 -176.0(7) .
C10 C11 C12 C13 -167.0(8) .
C16 C11 C12 C13 7.0(11) .
O7 C12 C13 C14 178.1(8) .
C11 C12 C13 C14 -4.8(12) .
C12 C13 C14 C15 -0.3(14) .
C13 C14 C15 C16 2.9(13) .
C13 C14 C15 C20 -177.1(8) .
C14 C15 C16 C17 -178.3(8) .
C20 C15 C16 C17 1.7(11) .
C14 C15 C16 C11 -0.5(12) .
C20 C15 C16 C11 179.5(7) .
C12 C11 C16 C17 173.2(8) .
C10 C11 C16 C17 -12.6(11) .
C12 C11 C16 C15 -4.5(11) .
C10 C11 C16 C15 169.8(7) .
C15 C16 C17 C18 -3.1(13) .
C11 C16 C17 C18 179.2(8) .
C16 C17 C18 C19 2.0(15) .
C17 C18 C19 C20 0.8(15) .
C18 C19 C20 C15 -2.2(14) .
C14 C15 C20 C19 -179.1(9) .
C16 C15 C20 C19 0.9(13) .
C8 C9 C21 C22 -6.6(12) .
N2 C9 C21 C22 172.7(8) .
C9 C21 C22 C23 -1.1(13) .
C21 C22 C23 C24 7.6(14) .
C21 C22 C23 Cl1 -173.1(7) .
C22 C23 C24 C8 -6.1(14) .
Cl1 C23 C24 C8 174.5(6) .
C9 C8 C24 C23 -1.9(12) .
C7 C8 C24 C23 179.0(8) .
O4 C6 C25 C26 178.7(8) .
C5 C6 C25 C26 2.5(12) .
C6 C25 C26 C27 1.4(13) .
C25 C26 C27 C32 176.5(8) .
C25 C26 C27 C28 -2.2(12) .
C32 C27 C28 C29 -0.6(11) .
C26 C27 C28 C29 178.1(7) .
C32 C27 C28 C5 -179.6(7) .
C26 C27 C28 C5 -0.9(11) .
C6 C5 C28 C29 -174.1(8) .
C4 C5 C28 C29 13.7(12) .
C6 C5 C28 C27 4.9(11) .
C4 C5 C28 C27 -167.4(7) .
C27 C28 C29 C30 1.3(13) .
C5 C28 C29 C30 -179.7(9) .
C28 C29 C30 C31 -0.8(14) .
C29 C30 C31 C32 -0.5(14) .
C30 C31 C32 C27 1.2(13) .
C26 C27 C32 C31 -179.3(8) .
C28 C27 C32 C31 -0.6(12) .
C2 C3 C33 C34 -1.8(14) .
N1 C3 C33 C34 -178.3(9) .
C3 C33 C34 C35 0.7(15) .
C33 C34 C35 C36 0.4(15) .
C33 C34 C35 Cl2 179.4(8) .
C34 C35 C36 C2 -0.3(13) .
Cl2 C35 C36 C2 -179.3(6) .
C3 C2 C36 C35 -0.9(12) .
C1 C2 C36 C35 -179.1(7) .
Ni2 O8 C37 N3 -176.3(6) .
C39 N3 C37 O8 -1.2(13) .
C38 N3 C37 O8 -176.1(8) .
Ni2 O9 C40 N4 174.6(6) .
C42 N4 C40 O9 -1.5(12) .
C41 N4 C40 O9 178.9(8) .
C50 N7 C51 O12 4(5) .
C49 N7 C51 O12 -173(4) .
C44 N5 C45 O10 -2(5) .
C43 N5 C45 O10 -175(3) .
C47 N6 C48 O11 178(3) .
C46 N6 C48 O11 -25(4) .
