#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:26:45 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179246 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/66/4316627.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_4316627
loop_
_publ_author_name
'Anandalok Audhya'
'Manoranjan Maity'
'Kisholoy Bhattacharya'
'Rodolphe Clérac'
'Muktimoy Chaudhury'
_publ_section_title
;
 Tri- and Tetranuclear Nickel(II) Inverse Metallacrown Complexes Involving
 Oximato Oxygen Linkers: Role of the Guest Anion (Oxo versus Alkoxo) in
 Controlling the Size of the Ring Topology
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9026
_journal_page_last               9035
_journal_paper_doi               10.1021/ic101273y
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C32 H61 Cl2 N8 Ni4 O26'
_chemical_formula_weight         1279.63
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 119.455(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.844(4)
_cell_length_b                   12.601(2)
_cell_length_c                   22.061(4)
_cell_measurement_temperature    150(2)
_cell_volume                     5287.5(16)
_computing_cell_refinement       'BRUKER APEX II'
_computing_data_collection       'BRUKER APEX II'
_computing_data_reduction        'BRUKER APEX II'
_computing_molecular_graphics    'MERCURY 2.2, PLATON-97'
_computing_publication_material  'MERCURY 2.2, PLATON-97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 0.3
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'CCD AREA DETECTOR'
_diffrn_measurement_method       OMEGA-SCAN
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_sigmaI/netI    0.0658
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            25749
_diffrn_reflns_theta_full        25.65
_diffrn_reflns_theta_max         25.65
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    1.592
_exptl_absorpt_correction_T_max  0.8319
_exptl_absorpt_correction_T_min  0.6466
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            RED
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2652
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.606
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     682
_refine_ls_number_reflns         9810
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0888
_refine_ls_R_factor_gt           0.0568
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.1679P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1588
_refine_ls_wR_factor_ref         0.1817
_reflns_number_gt                6616
_reflns_number_total             9810
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101273y_si_002_2.cif
_cod_data_source_block           compound3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'MONOCLINIC' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'MULTI-SCAN'
changed to 'multi-scan' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        5287.4(15)
_cod_database_code               4316627
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.16642(3) 0.41195(5) -0.00314(3) 0.02200(18) Uani 1 1 d . . .
Ni2 Ni 0.27362(3) 0.21273(5) 0.00029(3) 0.02618(19) Uani 1 1 d . . .
Ni4 Ni 0.25445(3) 0.41383(5) 0.17618(3) 0.02654(19) Uani 1 1 d . . .
Ni3 Ni 0.36401(3) 0.21813(5) 0.17715(3) 0.02636(19) Uani 1 1 d . . .
C2 C 0.1572(3) 0.5744(4) -0.0933(3) 0.0258(11) Uani 1 1 d . . .
C3 C 0.2014(3) 0.4937(4) -0.1028(3) 0.0272(11) Uani 1 1 d . . .
C1 C 0.1299(3) 0.6653(4) -0.1419(3) 0.0378(13) Uani 1 1 d . . .
H1A H 0.1025 0.7118 -0.1285 0.057 Uiso 1 1 calc R . .
H1B H 0.0997 0.6392 -0.1893 0.057 Uiso 1 1 calc R . .
H1C H 0.1693 0.7052 -0.1400 0.057 Uiso 1 1 calc R . .
C4 C 0.2257(3) 0.5016(5) -0.1538(3) 0.0441(15) Uani 1 1 d . . .
H4A H 0.2771 0.5043 -0.1294 0.066 Uiso 1 1 calc R . .
H4B H 0.2066 0.5662 -0.1815 0.066 Uiso 1 1 calc R . .
H4C H 0.2095 0.4395 -0.1845 0.066 Uiso 1 1 calc R . .
O15 O 0.26474(17) 0.4461(2) 0.08862(16) 0.0241(7) Uani 1 1 d . . .
O11 O 0.26158(17) 0.2517(3) 0.15410(16) 0.0270(8) Uani 1 1 d . . .
O3 O 0.19300(17) 0.2558(3) 0.02655(17) 0.0242(8) Uani 1 1 d . . .
O7 O 0.34058(18) 0.3046(3) 0.08541(18) 0.0255(8) Uani 1 1 d . . .
O2 O 0.24826(18) 0.3315(3) -0.06880(17) 0.0301(8) Uani 1 1 d . . .
O6 O 0.33797(18) 0.0772(3) 0.12642(17) 0.0327(9) Uani 1 1 d . . .
O10 O 0.35875(19) 0.4171(3) 0.24655(18) 0.0335(9) Uani 1 1 d . . .
O14 O 0.11328(18) 0.4335(3) 0.04863(17) 0.0319(8) Uani 1 1 d . . .
O9 O 0.47048(19) 0.2091(3) 0.21155(19) 0.0379(9) Uani 1 1 d . . .
O1 O 0.14184(17) 0.5629(3) -0.04624(17) 0.0281(8) Uani 1 1 d . . .
O5 O 0.2111(2) 0.1032(3) -0.07321(18) 0.0376(9) Uani 1 1 d . . .
O13 O 0.2227(2) 0.3795(3) 0.24898(17) 0.0367(9) Uani 1 1 d . . .
Cl1 Cl 0.37549(9) 0.71801(16) 0.98651(9) 0.0617(5) Uani 1 1 d . . .
Cl2 Cl 0.03918(14) 0.46765(17) 0.65139(11) 0.0898(7) Uani 1 1 d . . .
N7 N 0.1489(2) 0.4113(3) 0.1168(2) 0.0281(10) Uani 1 1 d . . .
N1 N 0.2128(2) 0.4119(3) -0.0625(2) 0.0245(9) Uani 1 1 d . . .
N3 N 0.2931(2) 0.0814(3) 0.0587(2) 0.0275(10) Uani 1 1 d . . .
N2 N 0.0720(2) 0.3441(3) -0.0825(2) 0.0289(10) Uani 1 1 d . . .
N5 N 0.3996(2) 0.3501(3) 0.2358(2) 0.0287(10) Uani 1 1 d . . .
N4 N 0.3619(3) 0.1957(4) -0.0125(3) 0.0383(12) Uani 1 1 d . . .
N6 N 0.3681(2) 0.1235(4) 0.2569(2) 0.0367(11) Uani 1 1 d . . .
N8 N 0.2647(3) 0.5789(4) 0.1893(3) 0.0587(16) Uani 1 1 d . . .
C5 C 0.0798(3) 0.2280(4) -0.0747(3) 0.0334(13) Uani 1 1 d . . .
H7A H 0.1001 0.2005 -0.1031 0.040 Uiso 1 1 calc R . .
H7B H 0.0330 0.1949 -0.0918 0.040 Uiso 1 1 calc R . .
C27 C 0.1121(3) 0.3878(4) 0.1477(3) 0.0270(11) Uani 1 1 d . . .
C18 C 0.5043(3) 0.2814(5) 0.2539(3) 0.0390(14) Uani 1 1 d . . .
C7 C 0.0454(3) 0.3763(4) -0.1569(2) 0.0320(12) Uani 1 1 d . . .
H6A H 0.0798 0.3524 -0.1709 0.038 Uiso 1 1 calc R . .
H6B H 0.0438 0.4547 -0.1593 0.038 Uiso 1 1 calc R . .
C6 C 0.1271(3) 0.1988(4) 0.0008(3) 0.0294(12) Uani 1 1 d . . .
H5A H 0.1043 0.2181 0.0285 0.035 Uiso 1 1 calc R . .
H5B H 0.1359 0.1214 0.0052 0.035 Uiso 1 1 calc R . .
C19 C 0.4672(3) 0.3642(4) 0.2703(3) 0.0338(13) Uani 1 1 d . . .
C30 C 0.2936(3) 0.5516(4) 0.0976(3) 0.0304(12) Uani 1 1 d . . .
H8A H 0.2877 0.5783 0.0529 0.036 Uiso 1 1 calc R . .
H8B H 0.3444 0.5506 0.1320 0.036 Uiso 1 1 calc R . .
C29 C 0.2555(3) 0.6221(4) 0.1227(3) 0.0383(14) Uani 1 1 d . . .
H9A H 0.2747 0.6951 0.1299 0.046 Uiso 1 1 calc R . .
H9B H 0.2049 0.6248 0.0876 0.046 Uiso 1 1 calc R . .
C20 C 0.5037(3) 0.4506(5) 0.3218(3) 0.0456(15) Uani 1 1 d . . .
H18A H 0.4703 0.5081 0.3139 0.068 Uiso 1 1 calc R . .
H18B H 0.5427 0.4779 0.3163 0.068 Uiso 1 1 calc R . .
H18C H 0.5219 0.4226 0.3690 0.068 Uiso 1 1 calc R . .
C10 C 0.2141(3) 0.0135(4) -0.0485(3) 0.0358(13) Uani 1 1 d . . .
C28 C 0.0340(3) 0.3799(5) 0.1106(3) 0.0432(14) Uani 1 1 d . . .
H22A H 0.0135 0.4448 0.0837 0.065 Uiso 1 1 calc R . .
H22B H 0.0178 0.3708 0.1446 0.065 Uiso 1 1 calc R . .
H22C H 0.0191 0.3188 0.0791 0.065 Uiso 1 1 calc R . .
C25 C 0.1259(3) 0.3343(5) 0.2653(3) 0.0515(17) Uani 1 1 d . . .
H20A H 0.1627 0.3104 0.3112 0.077 Uiso 1 1 calc R . .
H20B H 0.0931 0.2759 0.2417 0.077 Uiso 1 1 calc R . .
H20C H 0.1005 0.3942 0.2709 0.077 Uiso 1 1 calc R . .
C22 C 0.2427(3) 0.1667(4) 0.1861(3) 0.0326(12) Uani 1 1 d . . .
H24A H 0.2331 0.1010 0.1582 0.039 Uiso 1 1 calc R . .
H24B H 0.1997 0.1859 0.1878 0.039 Uiso 1 1 calc R . .
C21 C 0.3029(3) 0.1479(5) 0.2592(3) 0.0418(14) Uani 1 1 d . . .
H23A H 0.3102 0.2120 0.2880 0.050 Uiso 1 1 calc R . .
H23B H 0.2912 0.0881 0.2808 0.050 Uiso 1 1 calc R . .
C8 C -0.0261(3) 0.3343(5) -0.2094(3) 0.0429(15) Uani 1 1 d . . .
H19A H -0.0334 0.3456 -0.2570 0.051 Uiso 1 1 calc R . .
H19B H -0.0278 0.2570 -0.2025 0.051 Uiso 1 1 calc R . .
C26 C 0.1588(3) 0.3683(4) 0.2230(3) 0.0352(13) Uani 1 1 d . . .
C12 C 0.2632(3) -0.1077(4) 0.0615(3) 0.0470(16) Uani 1 1 d . . .
H16A H 0.2972 -0.1539 0.0576 0.070 Uiso 1 1 calc R . .
H16B H 0.2169 -0.1418 0.0390 0.070 Uiso 1 1 calc R . .
H16C H 0.2784 -0.0955 0.1108 0.070 Uiso 1 1 calc R . .
C15 C 0.3787(4) 0.0893(5) -0.0292(4) 0.062(2) Uani 1 1 d . . .
H15A H 0.4002 0.0461 0.0138 0.074 Uiso 1 1 calc R . .
H15B H 0.3342 0.0544 -0.0629 0.074 Uiso 1 1 calc R . .
C9 C 0.1753(4) -0.0753(5) -0.0948(3) 0.058(2) Uani 1 1 d . . .
H13A H 0.1554 -0.0527 -0.1434 0.087 Uiso 1 1 calc R . .
H13B H 0.1373 -0.0974 -0.0861 0.087 Uiso 1 1 calc R . .
H13C H 0.2074 -0.1350 -0.0858 0.087 Uiso 1 1 calc R . .
C17 C 0.5821(3) 0.2821(6) 0.2857(4) 0.070(2) Uani 1 1 d . . .
H17A H 0.5971 0.2203 0.2694 0.105 Uiso 1 1 calc R . .
H17B H 0.6036 0.2794 0.3365 0.105 Uiso 1 1 calc R . .
H17C H 0.5969 0.3472 0.2722 0.105 Uiso 1 1 calc R . .
C14 C 0.3952(3) 0.3409(4) 0.0724(3) 0.0361(13) Uani 1 1 d . . .
H26A H 0.4344 0.3714 0.1153 0.043 Uiso 1 1 calc R . .
H26B H 0.3769 0.3965 0.0360 0.043 Uiso 1 1 calc R . .
C13 C 0.4212(3) 0.2460(5) 0.0483(3) 0.0449(15) Uani 1 1 d . . .
H25A H 0.4568 0.2698 0.0359 0.054 Uiso 1 1 calc R . .
H25B H 0.4437 0.1938 0.0867 0.054 Uiso 1 1 calc R . .
C11 C 0.2589(3) -0.0035(4) 0.0266(3) 0.0329(12) Uani 1 1 d . . .
O4 O -0.0809(2) 0.3847(4) -0.2036(2) 0.0611(13) Uani 1 1 d . . .
H4'' H -0.0732 0.3793 -0.1624 0.092 Uiso 1 1 calc R . .
C23 C 0.4314(3) 0.1181(5) 0.3267(3) 0.0470(16) Uani 1 1 d . . .
H29A H 0.4390 0.1888 0.3488 0.056 Uiso 1 1 calc R . .
H29B H 0.4725 0.1023 0.3209 0.056 Uiso 1 1 calc R . .
C24 C 0.4285(4) 0.0369(7) 0.3754(4) 0.075(2) Uani 1 1 d . . .
C16 C 0.4261(5) 0.0895(6) -0.0584(4) 0.075(2) Uani 1 1 d . . .
H32A H 0.4730 0.1153 -0.0231 0.090 Uiso 1 1 calc R . .
H32B H 0.4313 0.0163 -0.0716 0.090 Uiso 1 1 calc R . .
O8 O 0.3989(3) 0.1551(4) -0.1169(2) 0.0700(15) Uani 1 1 d . . .
H8' H 0.3919 0.1193 -0.1518 0.105 Uiso 1 1 calc R . .
O19 O 0.3032(3) 0.7126(6) 0.9559(3) 0.108(2) Uani 1 1 d . . .
O22 O -0.0110(4) 0.4850(5) 0.5838(3) 0.137(3) Uani 1 1 d . . .
O24 O 0.0223(4) 0.5243(5) 0.6961(3) 0.126(3) Uani 1 1 d . . .
O18 O 0.4078(4) 0.7350(10) 1.0549(4) 0.194(5) Uani 1 1 d . . .
O23 O 0.0825(6) 0.3929(9) 0.6765(7) 0.238(6) Uani 1 1 d . . .
O27 O 0.0658(2) 0.6400(4) 0.0710(2) 0.0530(11) Uani 1 1 d . . .
O26 O 0.0855(5) 0.8401(6) 0.0331(4) 0.103(3) Uani 1 1 d . . .
O17 O 0.4104(4) 0.6905(10) 0.9532(5) 0.193(5) Uani 1 1 d . . .
O12A O 0.4123(4) -0.0560(7) 0.3497(5) 0.059(2) Uiso 0.60 1 d P . .
O12B O 0.4228(6) -0.0751(10) 0.3261(7) 0.057(3) Uiso 0.40 1 d P . .
C31A C 0.2381(5) 0.6403(7) 0.2251(5) 0.056(2) Uiso 0.73 1 d P . .
C31B C 0.2894(12) 0.6315(17) 0.2463(11) 0.040(5) Uiso 0.27 1 d P . .
C32A C 0.2714(7) 0.6301(11) 0.2966(7) 0.066(4) Uiso 0.56 1 d P . .
C32B C 0.2725(9) 0.7431(13) 0.2568(9) 0.065(4) Uiso 0.44 1 d P . .
O16A O 0.3478(8) 0.6770(12) 0.3240(8) 0.153(5) Uiso 0.58 1 d P . .
O16B O 0.2044(13) 0.7289(19) 0.2622(13) 0.182(9) Uiso 0.42 1 d P . .
O20A O 0.3813(8) 0.8255(13) 0.9732(8) 0.134(5) Uiso 0.54 1 d P . .
O20B O 0.3823(9) 0.5951(14) 0.9920(9) 0.133(6) Uiso 0.46 1 d P . .
O25A O -0.0013(9) 0.3577(13) 0.6517(9) 0.123(5) Uiso 0.45 1 d P . .
O25B O 0.0990(7) 0.5482(11) 0.6569(7) 0.120(4) Uiso 0.55 1 d P . .
H2' H 0.044(3) 0.359(4) -0.072(3) 0.019(15) Uiso 1 1 d . . .
H6' H 0.362(3) 0.053(5) 0.242(3) 0.052 Uiso 1 1 d . . .
H4' H 0.351(3) 0.243(5) -0.050(3) 0.056(19) Uiso 1 1 d . . .
H3' H 0.216(3) 0.251(4) 0.072(3) 0.035 Uiso 1 1 d . . .
H7' H 0.322(3) 0.350(5) 0.090(3) 0.039 Uiso 1 1 d . . .
H27D H 0.076(4) 0.712(6) 0.056(4) 0.081 Uiso 1 1 d . . .
H27E H 0.079(4) 0.577(6) 0.046(4) 0.081 Uiso 1 1 d . . .
H26D H 0.042(6) 0.878(9) 0.009(6) 0.150 Uiso 1 1 d . . .
H26E H 0.098(8) 0.813(11) 0.015(8) 0.150 Uiso 1 1 d . . .
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'
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
O14 Ni1 N1 171.04(15) . . ?
O14 Ni1 O3 95.70(14) . . ?
N1 Ni1 O3 93.04(14) . . ?
O14 Ni1 O1 92.59(14) . . ?
N1 Ni1 O1 78.57(15) . . ?
O3 Ni1 O1 170.97(14) . . ?
O14 Ni1 N2 85.65(17) . . ?
N1 Ni1 N2 93.41(18) . . ?
O3 Ni1 N2 83.42(15) . . ?
O1 Ni1 N2 93.65(15) . . ?
O14 Ni1 O15 91.53(13) . . ?
N1 Ni1 O15 91.33(14) . . ?
O3 Ni1 O15 84.09(12) . . ?
O1 Ni1 O15 99.31(12) . . ?
N2 Ni1 O15 166.86(14) . . ?
O2 Ni2 N3 172.60(15) . . ?
O2 Ni2 O5 94.21(14) . . ?
N3 Ni2 O5 78.57(16) . . ?
O2 Ni2 O7 94.57(14) . . ?
N3 Ni2 O7 92.66(15) . . ?
O5 Ni2 O7 171.22(14) . . ?
O2 Ni2 N4 84.42(16) . . ?
N3 Ni2 N4 94.81(18) . . ?
O5 Ni2 N4 97.14(18) . . ?
O7 Ni2 N4 83.85(17) . . ?
O2 Ni2 O3 93.38(13) . . ?
N3 Ni2 O3 88.74(15) . . ?
O5 Ni2 O3 93.80(14) . . ?
O7 Ni2 O3 85.55(13) . . ?
N4 Ni2 O3 168.96(16) . . ?
N7 Ni4 O10 172.69(16) . . ?
N7 Ni4 O13 77.85(16) . . ?
O10 Ni4 O13 95.07(15) . . ?
N7 Ni4 O15 90.66(15) . . ?
O10 Ni4 O15 96.45(14) . . ?
O13 Ni4 O15 168.47(14) . . ?
N7 Ni4 N8 96.7(2) . . ?
O10 Ni4 N8 82.5(2) . . ?
O13 Ni4 N8 98.84(18) . . ?
O15 Ni4 N8 83.20(16) . . ?
N7 Ni4 O11 91.46(14) . . ?
O10 Ni4 O11 90.79(13) . . ?
O13 Ni4 O11 93.82(14) . . ?
O15 Ni4 O11 85.51(12) . . ?
N8 Ni4 O11 166.15(19) . . ?
N5 Ni3 O6 173.60(16) . . ?
N5 Ni3 O9 78.47(16) . . ?
O6 Ni3 O9 96.57(15) . . ?
N5 Ni3 O11 91.03(15) . . ?
O6 Ni3 O11 93.85(14) . . ?
O9 Ni3 O11 169.48(14) . . ?
N5 Ni3 N6 94.99(18) . . ?
O6 Ni3 N6 81.32(17) . . ?
O9 Ni3 N6 94.90(17) . . ?
O11 Ni3 N6 85.24(16) . . ?
N5 Ni3 O7 91.41(15) . . ?
O6 Ni3 O7 93.03(13) . . ?
O9 Ni3 O7 94.50(14) . . ?
O11 Ni3 O7 86.36(13) . . ?
N6 Ni3 O7 169.53(16) . . ?
O1 C2 C1 121.0(5) . . ?
O1 C2 C3 119.8(4) . . ?
C1 C2 C3 119.1(4) . . ?
N1 C3 C4 123.9(5) . . ?
N1 C3 C2 111.5(4) . . ?
C4 C3 C2 124.6(4) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C30 O15 Ni4 106.8(3) . . ?
C30 O15 Ni1 118.7(3) . . ?
Ni4 O15 Ni1 108.64(14) . . ?
C22 O11 Ni3 105.0(3) . . ?
C22 O11 Ni4 122.0(3) . . ?
Ni3 O11 Ni4 109.33(14) . . ?
C6 O3 Ni1 106.1(3) . . ?
C6 O3 Ni2 123.3(3) . . ?
Ni1 O3 Ni2 106.93(15) . . ?
C6 O3 H3' 108(4) . . ?
Ni1 O3 H3' 110(3) . . ?
Ni2 O3 H3' 102(4) . . ?
C14 O7 Ni2 106.4(3) . . ?
C14 O7 Ni3 121.3(3) . . ?
Ni2 O7 Ni3 107.92(15) . . ?
C14 O7 H7' 110(5) . . ?
Ni2 O7 H7' 111(5) . . ?
Ni3 O7 H7' 100(5) . . ?
N1 O2 Ni2 116.6(3) . . ?
N3 O6 Ni3 116.0(3) . . ?
N5 O10 Ni4 116.6(3) . . ?
N7 O14 Ni1 115.6(3) . . ?
C18 O9 Ni3 112.3(4) . . ?
C2 O1 Ni1 111.9(3) . . ?
C10 O5 Ni2 113.2(3) . . ?
C26 O13 Ni4 113.3(3) . . ?
O18 Cl1 O17 122.3(5) . . ?
O18 Cl1 O19 113.9(5) . . ?
O17 Cl1 O19 122.8(5) . . ?
O18 Cl1 O20A 91.7(8) . . ?
O17 Cl1 O20A 90.0(8) . . ?
O19 Cl1 O20A 98.3(7) . . ?
O18 Cl1 O20B 95.4(9) . . ?
O17 Cl1 O20B 74.1(8) . . ?
O19 Cl1 O20B 91.8(7) . . ?
O20A Cl1 O20B 164.0(9) . . ?
O23 Cl2 O22 128.9(7) . . ?
O23 Cl2 O24 118.2(7) . . ?
O22 Cl2 O24 109.7(5) . . ?
O23 Cl2 O25B 91.8(8) . . ?
O22 Cl2 O25B 99.6(6) . . ?
O24 Cl2 O25B 96.3(6) . . ?
O23 Cl2 O25A 69.9(8) . . ?
O22 Cl2 O25A 89.7(7) . . ?
O24 Cl2 O25A 95.6(7) . . ?
O25B Cl2 O25A 161.3(8) . . ?
C27 N7 O14 117.6(4) . . ?
C27 N7 Ni4 117.5(3) . . ?
O14 N7 Ni4 124.9(3) . . ?
C3 N1 O2 117.4(4) . . ?
C3 N1 Ni1 117.0(3) . . ?
O2 N1 Ni1 125.2(3) . . ?
C11 N3 O6 119.4(4) . . ?
C11 N3 Ni2 116.4(3) . . ?
O6 N3 Ni2 124.2(3) . . ?
C5 N2 C7 110.8(4) . . ?
C5 N2 Ni1 107.1(3) . . ?
C7 N2 Ni1 119.3(3) . . ?
C5 N2 H2' 106(4) . . ?
C7 N2 H2' 109(4) . . ?
Ni1 N2 H2' 104(4) . . ?
C19 N5 O10 118.5(4) . . ?
C19 N5 Ni3 117.3(4) . . ?
O10 N5 Ni3 123.9(3) . . ?
C13 N4 C15 113.6(5) . . ?
C13 N4 Ni2 106.8(3) . . ?
C15 N4 Ni2 118.9(4) . . ?
C13 N4 H4' 104(4) . . ?
C15 N4 H4' 110(4) . . ?
Ni2 N4 H4' 102(4) . . ?
C21 N6 C23 113.3(5) . . ?
C21 N6 Ni3 105.4(3) . . ?
C23 N6 Ni3 122.2(4) . . ?
C21 N6 H6' 104(4) . . ?
C23 N6 H6' 103(4) . . ?
Ni3 N6 H6' 108(4) . . ?
C31B N8 C31A 42.4(10) . . ?
C31B N8 C29 124.6(10) . . ?
C31A N8 C29 117.2(6) . . ?
C31B N8 Ni4 127.8(10) . . ?
C31A N8 Ni4 124.9(5) . . ?
C29 N8 Ni4 105.9(3) . . ?
N2 C5 C6 110.3(4) . . ?
N2 C5 H7A 109.6 . . ?
C6 C5 H7A 109.6 . . ?
N2 C5 H7B 109.6 . . ?
C6 C5 H7B 109.6 . . ?
H7A C5 H7B 108.1 . . ?
N7 C27 C26 111.0(4) . . ?
N7 C27 C28 123.8(5) . . ?
C26 C27 C28 125.1(5) . . ?
O9 C18 C19 120.4(5) . . ?
O9 C18 C17 118.3(6) . . ?
C19 C18 C17 121.3(5) . . ?
N2 C7 C8 116.3(5) . . ?
N2 C7 H6A 108.2 . . ?
C8 C7 H6A 108.2 . . ?
N2 C7 H6B 108.2 . . ?
C8 C7 H6B 108.2 . . ?
H6A C7 H6B 107.4 . . ?
O3 C6 C5 108.6(4) . . ?
O3 C6 H5A 110.0 . . ?
C5 C6 H5A 110.0 . . ?
O3 C6 H5B 110.0 . . ?
C5 C6 H5B 110.0 . . ?
H5A C6 H5B 108.3 . . ?
N5 C19 C18 111.3(5) . . ?
N5 C19 C20 125.0(5) . . ?
C18 C19 C20 123.6(5) . . ?
O15 C30 C29 108.3(4) . . ?
O15 C30 H8A 110.0 . . ?
C29 C30 H8A 110.0 . . ?
O15 C30 H8B 110.0 . . ?
C29 C30 H8B 110.0 . . ?
H8A C30 H8B 108.4 . . ?
N8 C29 C30 108.5(4) . . ?
N8 C29 H9A 110.0 . . ?
C30 C29 H9A 110.0 . . ?
N8 C29 H9B 110.0 . . ?
C30 C29 H9B 110.0 . . ?
H9A C29 H9B 108.4 . . ?
C19 C20 H18A 109.5 . . ?
C19 C20 H18B 109.5 . . ?
H18A C20 H18B 109.5 . . ?
C19 C20 H18C 109.5 . . ?
H18A C20 H18C 109.5 . . ?
H18B C20 H18C 109.5 . . ?
O5 C10 C11 119.4(5) . . ?
O5 C10 C9 119.9(5) . . ?
C11 C10 C9 120.6(5) . . ?
C27 C28 H22A 109.5 . . ?
C27 C28 H22B 109.5 . . ?
H22A C28 H22B 109.5 . . ?
C27 C28 H22C 109.5 . . ?
H22A C28 H22C 109.5 . . ?
H22B C28 H22C 109.5 . . ?
C26 C25 H20A 109.5 . . ?
C26 C25 H20B 109.5 . . ?
H20A C25 H20B 109.5 . . ?
C26 C25 H20C 109.5 . . ?
H20A C25 H20C 109.5 . . ?
H20B C25 H20C 109.5 . . ?
O11 C22 C21 109.1(4) . . ?
O11 C22 H24A 109.9 . . ?
C21 C22 H24A 109.9 . . ?
O11 C22 H24B 109.9 . . ?
C21 C22 H24B 109.9 . . ?
H24A C22 H24B 108.3 . . ?
N6 C21 C22 109.9(4) . . ?
N6 C21 H23A 109.7 . . ?
C22 C21 H23A 109.7 . . ?
N6 C21 H23B 109.7 . . ?
C22 C21 H23B 109.7 . . ?
H23A C21 H23B 108.2 . . ?
O4 C8 C7 111.9(5) . . ?
O4 C8 H19A 109.2 . . ?
C7 C8 H19A 109.2 . . ?
O4 C8 H19B 109.2 . . ?
C7 C8 H19B 109.2 . . ?
H19A C8 H19B 107.9 . . ?
O13 C26 C27 120.1(5) . . ?
O13 C26 C25 121.7(5) . . ?
C27 C26 C25 118.2(5) . . ?
C11 C12 H16A 109.5 . . ?
C11 C12 H16B 109.5 . . ?
H16A C12 H16B 109.5 . . ?
C11 C12 H16C 109.5 . . ?
H16A C12 H16C 109.5 . . ?
H16B C12 H16C 109.5 . . ?
C16 C15 N4 115.1(6) . . ?
C16 C15 H15A 108.5 . . ?
N4 C15 H15A 108.5 . . ?
C16 C15 H15B 108.5 . . ?
N4 C15 H15B 108.5 . . ?
H15A C15 H15B 107.5 . . ?
C10 C9 H13A 109.5 . . ?
C10 C9 H13B 109.5 . . ?
H13A C9 H13B 109.5 . . ?
C10 C9 H13C 109.5 . . ?
H13A C9 H13C 109.5 . . ?
H13B C9 H13C 109.5 . . ?
C18 C17 H17A 109.5 . . ?
C18 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C18 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O7 C14 C13 108.0(4) . . ?
O7 C14 H26A 110.1 . . ?
C13 C14 H26A 110.1 . . ?
O7 C14 H26B 110.1 . . ?
C13 C14 H26B 110.1 . . ?
H26A C14 H26B 108.4 . . ?
N4 C13 C14 110.0(5) . . ?
N4 C13 H25A 109.7 . . ?
C14 C13 H25A 109.7 . . ?
N4 C13 H25B 109.7 . . ?
C14 C13 H25B 109.7 . . ?
H25A C13 H25B 108.2 . . ?
N3 C11 C10 112.4(4) . . ?
N3 C11 C12 124.5(5) . . ?
C10 C11 C12 123.1(5) . . ?
C8 O4 H4'' 109.5 . . ?
N6 C23 C24 115.3(5) . . ?
N6 C23 H29A 108.4 . . ?
C24 C23 H29A 108.4 . . ?
N6 C23 H29B 108.4 . . ?
C24 C23 H29B 108.4 . . ?
H29A C23 H29B 107.5 . . ?
O12A C24 C23 114.0(8) . . ?
O12A C24 O12B 20.2(6) . . ?
C23 C24 O12B 96.8(7) . . ?
O8 C16 C15 109.6(6) . . ?
O8 C16 H32A 109.7 . . ?
C15 C16 H32A 109.7 . . ?
O8 C16 H32B 109.7 . . ?
C15 C16 H32B 109.7 . . ?
H32A C16 H32B 108.2 . . ?
C16 O8 H8' 109.5 . . ?
H27D O27 H27E 110(6) . . ?
H26D O26 H26E 120(10) . . ?
O12B O12A C24 121.3(17) . . ?
O12A O12B C24 38.5(12) . . ?
C31B C31A C32A 67.0(15) . . ?
C31B C31A N8 61.4(14) . . ?
C32A C31A N8 117.1(9) . . ?
C31B C31A C32B 71.4(15) . . ?
C32A C31A C32B 71.5(10) . . ?
N8 C31A C32B 119.1(10) . . ?
C31B C31A O16B 119.4(17) . . ?
C32A C31A O16B 68.3(10) . . ?
N8 C31A O16B 172.8(11) . . ?
C32B C31A O16B 57.0(10) . . ?
C31A C31B N8 76.1(15) . . ?
C31A C31B C32A 70.7(16) . . ?
N8 C31B C32A 130.5(18) . . ?
C31A C31B C32B 70.1(15) . . ?
N8 C31B C32B 128.2(17) . . ?
C32A C31B C32B 72.1(14) . . ?
C31A C31B O16A 125(2) . . ?
N8 C31B O16A 158.8(19) . . ?
C32A C31B O16A 62.6(11) . . ?
C32B C31B O16A 68.8(12) . . ?
C31B C32A C31A 42.4(10) . . ?
C31B C32A O16A 68.3(12) . . ?
C31A C32A O16A 105.4(11) . . ?
C31B C32A O16B 98.7(15) . . ?
C31A C32A O16B 65.7(10) . . ?
O16A C32A O16B 113.1(13) . . ?
C31A C32B C31B 38.5(9) . . ?
C31A C32B O16B 69.9(12) . . ?
C31B C32B O16B 102.8(16) . . ?
C31A C32B O16A 91.7(10) . . ?
C31B C32B O16A 59.7(11) . . ?
O16B C32B O16A 114.0(15) . . ?
C32A O16A C31B 49.1(10) . . ?
C32A O16A C32B 59.4(9) . . ?
C31B O16A C32B 51.5(10) . . ?
C32B O16B C31A 53.1(11) . . ?
C32B O16B C32A 59.8(12) . . ?
C31A O16B C32A 46.0(8) . . ?
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 O14 2.007(3) . ?
Ni1 N1 2.012(4) . ?
Ni1 O3 2.065(3) . ?
Ni1 O1 2.075(3) . ?
Ni1 N2 2.121(4) . ?
Ni1 O15 2.149(3) . ?
Ni2 O2 2.009(3) . ?
Ni2 N3 2.010(4) . ?
Ni2 O5 2.055(4) . ?
Ni2 O7 2.075(4) . ?
Ni2 N4 2.093(5) . ?
Ni2 O3 2.176(3) . ?
Ni4 N7 2.016(4) . ?
Ni4 O10 2.031(4) . ?
Ni4 O13 2.084(4) . ?
Ni4 O15 2.092(3) . ?
Ni4 N8 2.096(5) . ?
Ni4 O11 2.124(3) . ?
Ni3 N5 2.013(4) . ?
Ni3 O6 2.026(3) . ?
Ni3 O9 2.064(4) . ?
Ni3 O11 2.080(3) . ?
Ni3 N6 2.092(4) . ?
Ni3 O7 2.128(3) . ?
C2 O1 1.247(6) . ?
C2 C1 1.479(7) . ?
C2 C3 1.486(7) . ?
C3 N1 1.302(6) . ?
C3 C4 1.464(7) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
O15 C30 1.442(5) . ?
O11 C22 1.449(6) . ?
O3 C6 1.451(5) . ?
O3 H3' 0.88(6) . ?
O7 C14 1.433(6) . ?
O7 H7' 0.73(6) . ?
O2 N1 1.323(5) . ?
O6 N3 1.325(5) . ?
O10 N5 1.332(5) . ?
O14 N7 1.340(5) . ?
O9 C18 1.252(6) . ?
O5 C10 1.242(6) . ?
O13 C26 1.230(6) . ?
Cl1 O18 1.331(7) . ?
Cl1 O17 1.340(7) . ?
Cl1 O19 1.379(6) . ?
Cl1 O20A 1.404(16) . ?
Cl1 O20B 1.555(17) . ?
Cl2 O23 1.255(8) . ?
Cl2 O22 1.365(6) . ?
Cl2 O24 1.406(7) . ?
Cl2 O25B 1.611(14) . ?
Cl2 O25A 1.645(17) . ?
N7 C27 1.317(6) . ?
N3 C11 1.298(6) . ?
N2 C5 1.474(6) . ?
N2 C7 1.503(6) . ?
N2 H2' 0.79(5) . ?
N5 C19 1.300(6) . ?
N4 C13 1.473(8) . ?
N4 C15 1.484(7) . ?
N4 H4' 0.95(6) . ?
N6 C21 1.482(7) . ?
N6 C23 1.482(7) . ?
N6 H6' 0.94(6) . ?
N8 C31B 1.28(2) . ?
N8 C31A 1.419(11) . ?
N8 C29 1.484(7) . ?
C5 C6 1.513(7) . ?
C5 H7A 0.9900 . ?
C5 H7B 0.9900 . ?
C27 C26 1.481(7) . ?
C27 C28 1.490(7) . ?
C18 C19 1.471(8) . ?
C18 C17 1.486(8) . ?
C7 C8 1.510(7) . ?
C7 H6A 0.9900 . ?
C7 H6B 0.9900 . ?
C6 H5A 0.9900 . ?
C6 H5B 0.9900 . ?
C19 C20 1.489(7) . ?
C30 C29 1.497(7) . ?
C30 H8A 0.9900 . ?
C30 H8B 0.9900 . ?
C29 H9A 0.9900 . ?
C29 H9B 0.9900 . ?
C20 H18A 0.9800 . ?
C20 H18B 0.9800 . ?
C20 H18C 0.9800 . ?
C10 C11 1.467(7) . ?
C10 C9 1.471(7) . ?
C28 H22A 0.9800 . ?
C28 H22B 0.9800 . ?
C28 H22C 0.9800 . ?
C25 C26 1.493(8) . ?
C25 H20A 0.9800 . ?
C25 H20B 0.9800 . ?
C25 H20C 0.9800 . ?
C22 C21 1.517(7) . ?
C22 H24A 0.9900 . ?
C22 H24B 0.9900 . ?
C21 H23A 0.9900 . ?
C21 H23B 0.9900 . ?
C8 O4 1.416(7) . ?
C8 H19A 0.9900 . ?
C8 H19B 0.9900 . ?
C12 C11 1.502(7) . ?
C12 H16A 0.9800 . ?
C12 H16B 0.9800 . ?
C12 H16C 0.9800 . ?
C15 C16 1.462(10) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C9 H13A 0.9800 . ?
C9 H13B 0.9800 . ?
C9 H13C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C14 C13 1.526(8) . ?
C14 H26A 0.9900 . ?
C14 H26B 0.9900 . ?
C13 H25A 0.9900 . ?
C13 H25B 0.9900 . ?
O4 H4'' 0.8400 . ?
C23 C24 1.506(8) . ?
C23 H29A 0.9900 . ?
C23 H29B 0.9900 . ?
C24 O12A 1.274(11) . ?
C24 O12B 1.749(16) . ?
C16 O8 1.395(8) . ?
C16 H32A 0.9900 . ?
C16 H32B 0.9900 . ?
O8 H8' 0.8400 . ?
O27 H27D 1.03(8) . ?
O27 H27E 1.07(8) . ?
O26 H26D 0.95(11) . ?
O26 H26E 0.67(13) . ?
O12A O12B 0.708(13) . ?
C31A C31B 0.99(2) . ?
C31A C32A 1.381(16) . ?
C31A C32B 1.488(18) . ?
C31A O16B 1.75(3) . ?
C31B C32A 1.35(2) . ?
C31B C32B 1.50(3) . ?
C31B O16A 1.65(2) . ?
C32A O16A 1.582(19) . ?
C32A O16B 1.78(3) . ?
C32B O16B 1.56(3) . ?
C32B O16A 1.79(2) . ?
