#------------------------------------------------------------------------------
#$Date: 2022-01-15 04:38:01 +0200 (Sat, 15 Jan 2022) $
#$Revision: 272054 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/25/2022514.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2022514
loop_
_publ_author_name
'Patel, R. N.'
'Patel, S. K.'
'Patel, A. K.'
'Patel, N.'
'Butcher, Ray J.'
_publ_section_title
;
 A tetranuclear nickel(II) complex,
 [Ni4(L)4](ClO4)4·C2H3N·2H2O, with an asymmetric Ni4O4
 open-cubane-like core
;
_journal_coeditor_code           YY2002
_journal_issue                   2
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi               10.1107/S2056989021012408
_journal_volume                  78
_journal_year                    2022
_chemical_absolute_configuration unk
_chemical_formula_iupac
'[Ni4 (C13 H12 N3 O2)4] (Cl O4)4, C2 H3 N, 2H2 O'
_chemical_formula_moiety
;
C52 H48 N12 Ni4 O8, 4(Cl O4), C2 H3 N, 2(H2 O)
;
_chemical_formula_sum            'C54 H55 Cl4 N13 Ni4 O26'
_chemical_formula_weight         1678.75
_chemical_name_systematic
;cyclo-Tetrakis(μ-2-methoxy-6-{[2-(pyridin-2-yl)hydrazin-1-ylidene]methyl}phenolato)tetranickel(II) tetrakis(perchlorate) acetonitrile
monosolvate dihydrate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.5976(6)
_cell_length_b                   11.8723(3)
_cell_length_c                   22.2989(6)
_cell_measurement_reflns_used    9461
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.31
_cell_measurement_theta_min      2.43
_cell_volume                     6247.2(3)
_computing_cell_refinement
;
SAINT (Bruker, 2002)
;
_computing_data_collection
;
APEX2 (Bruker, 2005)
;
_computing_data_reduction
;
SAINT (Bruker, 2002)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick 2008)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0684
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            86241
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         1.920
_exptl_absorpt_coefficient_mu    1.456
_exptl_absorpt_correction_T_max  0.765
_exptl_absorpt_correction_T_min  0.554
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al.,  2015)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.785
_exptl_crystal_description       needle
_exptl_crystal_F_000             3432
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.837
_refine_diff_density_min         -1.299
_refine_ls_abs_structure_details
;
Flack x determined using 4529 quotients
[(I⁺)-(I⁻)]/[(I⁺)+(I⁻)]
(Parsons et al.,  2013)
;
_refine_ls_abs_structure_Flack   0.024(5)
_refine_ls_extinction_coef       0.00135(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2018/3 (Sheldrick 2018)
;
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1051
_refine_ls_number_reflns         14617
_refine_ls_number_restraints     320
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0571P)²+9.1783P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1250
_reflns_number_gt                11629
_reflns_number_total             14617
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            yy2002sup1.cif
_cod_data_source_block           I
_cod_database_code               2022514
_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+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni1 0.73671(3) 0.62167(6) 0.50776(4) 0.01973(18) Uani d 1 . .
Ni Ni2 0.65087(3) 0.46794(6) 0.42646(4) 0.01955(17) Uani d 1 . .
Ni Ni3 0.58915(3) 0.60905(7) 0.53570(4) 0.02116(18) Uani d 1 . .
Ni Ni4 0.64341(3) 0.75702(6) 0.42586(4) 0.02228(18) Uani d 1 . .
O O1A 0.6789(2) 0.7401(4) 0.5065(2) 0.0261(10) Uani d 1 . .
O O2A 0.6144(2) 0.9102(4) 0.4796(3) 0.0319(12) Uani d 1 . .
N N1A 0.7519(2) 0.6456(5) 0.5919(3) 0.0282(13) Uani d 1 . .
N N2A 0.7897(3) 0.5687(5) 0.6153(3) 0.0315(13) Uani d 1 . .
H H2AA 0.797624 0.565969 0.653817 0.06(3) Uiso calc 1 . .
N N3A 0.7945(2) 0.5026(5) 0.5191(3) 0.0251(12) Uani d 1 . .
C C1A 0.6699(3) 0.8175(6) 0.5507(3) 0.0259(15) Uani d 1 . .
C C2A 0.6349(3) 0.9109(5) 0.5375(4) 0.0284(15) Uani d 1 . .
C C3A 0.6212(4) 0.9884(6) 0.5812(4) 0.0383(19) Uani d 1 . .
H H3AA 0.597016 1.049895 0.571891 0.046 Uiso calc 1 . .
C C4A 0.6423(4) 0.9769(7) 0.6381(4) 0.045(2) Uani d 1 . .
H H4AA 0.632679 1.030502 0.668040 0.054 Uiso calc 1 . .
C C5A 0.6775(4) 0.8881(7) 0.6523(4) 0.0406(19) Uani d 1 . .
H H5AA 0.692022 0.881058 0.691864 0.049 Uiso calc 1 . .
C C6A 0.6920(3) 0.8081(6) 0.6086(3) 0.0302(16) Uani d 1 . .
C C7A 0.5891(4) 1.0134(6) 0.4589(4) 0.044(2) Uani d 1 . .
H H7AA 0.612658 1.077293 0.471255 0.066 Uiso calc 1 . .
H H7AB 0.551164 1.021250 0.476297 0.066 Uiso calc 1 . .
H H7AC 0.586234 1.011904 0.415072 0.066 Uiso calc 1 . .
C C8A 0.7308(3) 0.7216(6) 0.6278(3) 0.0311(16) Uani d 1 . .
H H8AA 0.741612 0.719868 0.668851 0.037 Uiso calc 1 . .
C C9A 0.8139(3) 0.4970(6) 0.5750(3) 0.0265(15) Uani d 1 . .
C C10A 0.8565(3) 0.4202(7) 0.5921(4) 0.0326(17) Uani d 1 . .
H H10A 0.869548 0.417446 0.632430 0.039 Uiso calc 1 . .
C C11A 0.8782(3) 0.3517(7) 0.5509(4) 0.0363(18) Uani d 1 . .
H H11A 0.906120 0.298033 0.562076 0.044 Uiso calc 1 . .
C C12A 0.8601(3) 0.3578(6) 0.4908(4) 0.0342(17) Uani d 1 . .
H H12A 0.876312 0.310984 0.460768 0.041 Uiso calc 1 . .
C C13A 0.8179(3) 0.4346(6) 0.4770(4) 0.0298(15) Uani d 1 . .
H H13A 0.804979 0.439766 0.436785 0.036 Uiso calc 1 . .
O O1B 0.71137(17) 0.5813(3) 0.4250(2) 0.0231(9) Uani d 1 . .
O O2B 0.80171(19) 0.7036(4) 0.4463(2) 0.0256(10) Uani d 1 . .
N N1B 0.6495(2) 0.4613(5) 0.3398(3) 0.0254(13) Uani d 1 . .
N N2B 0.6028(3) 0.4046(5) 0.3185(3) 0.0301(13) Uani d 1 . .
H H2BA 0.594259 0.403529 0.280135 0.07(4) Uiso calc 1 . .
N N3B 0.5861(2) 0.3646(4) 0.4175(3) 0.0252(12) Uani d 1 . .
C C1B 0.7471(3) 0.6010(5) 0.3779(3) 0.0239(14) Uani d 1 . .
C C2B 0.7959(3) 0.6656(5) 0.3881(3) 0.0240(14) Uani d 1 . .
C C3B 0.8342(3) 0.6893(6) 0.3426(3) 0.0272(15) Uani d 1 . .
H H3BA 0.867365 0.732216 0.350462 0.033 Uiso calc 1 . .
C C4B 0.8230(3) 0.6488(6) 0.2849(3) 0.0302(15) Uani d 1 . .
H H4BA 0.849159 0.663339 0.253437 0.036 Uiso calc 1 . .
C C5B 0.7750(3) 0.5886(6) 0.2734(3) 0.0282(15) Uani d 1 . .
H H5BA 0.767612 0.563818 0.233670 0.034 Uiso calc 1 . .
C C6B 0.7361(3) 0.5626(6) 0.3195(3) 0.0252(14) Uani d 1 . .
C C7B 0.8561(3) 0.7453(7) 0.4645(4) 0.0367(18) Uani d 1 . .
H H7BA 0.865425 0.812932 0.441373 0.055 Uiso calc 1 . .
H H7BB 0.884944 0.687402 0.457407 0.055 Uiso calc 1 . .
H H7BC 0.855123 0.763956 0.507341 0.055 Uiso calc 1 . .
C C8B 0.6866(3) 0.4975(6) 0.3018(3) 0.0260(14) Uani d 1 . .
H H8BA 0.681397 0.480901 0.260520 0.031 Uiso calc 1 . .
C C9B 0.5706(3) 0.3504(6) 0.3597(4) 0.0282(15) Uani d 1 . .
C C10B 0.5229(3) 0.2854(6) 0.3442(4) 0.0352(17) Uani d 1 . .
H H10B 0.511292 0.278466 0.303583 0.042 Uiso calc 1 . .
C C11B 0.4938(3) 0.2330(6) 0.3886(4) 0.0369(19) Uani d 1 . .
H H11B 0.461388 0.188949 0.379192 0.044 Uiso calc 1 . .
C C12B 0.5115(3) 0.2435(6) 0.4488(4) 0.0316(16) Uani d 1 . .
H H12B 0.492177 0.204730 0.479900 0.038 Uiso calc 1 . .
C C13B 0.5568(3) 0.3103(5) 0.4614(4) 0.0298(16) Uani d 1 . .
H H13B 0.568312 0.319200 0.501973 0.036 Uiso calc 1 . .
O O1C 0.64418(19) 0.4911(4) 0.5149(2) 0.0252(10) Uani d 1 . .
O O2C 0.7018(2) 0.3254(4) 0.4662(2) 0.0303(11) Uani d 1 . .
N N1C 0.6018(2) 0.5844(5) 0.6203(3) 0.0281(13) Uani d 1 . .
N N2C 0.5735(3) 0.6611(5) 0.6559(3) 0.0327(14) Uani d 1 . .
H H2CA 0.575273 0.658689 0.695341 0.14(6) Uiso calc 1 . .
N N3C 0.5404(2) 0.7317(5) 0.5660(3) 0.0270(12) Uani d 1 . .
C C1C 0.6662(3) 0.4124(6) 0.5522(3) 0.0253(15) Uani d 1 . .
C C2C 0.6976(3) 0.3228(6) 0.5273(4) 0.0299(16) Uani d 1 . .
C C3C 0.7222(3) 0.2412(6) 0.5633(4) 0.0367(18) Uani d 1 . .
H H3CA 0.742965 0.181040 0.545793 0.044 Uiso calc 1 . .
C C4C 0.7164(3) 0.2480(7) 0.6254(4) 0.0385(19) Uani d 1 . .
H H4CA 0.733433 0.192783 0.650417 0.046 Uiso calc 1 . .
C C5C 0.6862(3) 0.3341(7) 0.6501(4) 0.0364(18) Uani d 1 . .
H H5CA 0.682536 0.337817 0.692492 0.044 Uiso calc 1 . .
C C6C 0.6602(3) 0.4172(6) 0.6149(4) 0.0290(15) Uani d 1 . .
C C7C 0.7241(3) 0.2280(6) 0.4358(4) 0.041(2) Uani d 1 . .
H H7CA 0.764599 0.220712 0.444534 0.062 Uiso calc 1 . .
H H7CB 0.718647 0.236542 0.392429 0.062 Uiso calc 1 . .
H H7CC 0.704131 0.160439 0.449638 0.062 Uiso calc 1 . .
C C8C 0.6291(3) 0.5033(6) 0.6458(4) 0.0329(17) Uani d 1 . .
H H8CA 0.628574 0.500392 0.688326 0.040 Uiso calc 1 . .
C C9C 0.5425(3) 0.7411(6) 0.6262(4) 0.0315(16) Uani d 1 . .
C C10C 0.5134(3) 0.8263(7) 0.6577(4) 0.0387(18) Uani d 1 . .
H H10C 0.516037 0.832498 0.700031 0.046 Uiso calc 1 . .
C C11C 0.4814(4) 0.8989(7) 0.6252(5) 0.047(2) Uani d 1 . .
H H11C 0.461404 0.957613 0.644892 0.056 Uiso calc 1 . .
C C12C 0.4776(4) 0.8880(7) 0.5629(4) 0.0383(18) Uani d 1 . .
H H12C 0.454778 0.938126 0.540173 0.046 Uiso calc 1 . .
C C13C 0.5076(3) 0.8034(6) 0.5351(4) 0.0314(15) Uani d 1 . .
H H13C 0.504959 0.795620 0.492831 0.038 Uiso calc 1 . .
O O1D 0.5854(2) 0.6484(4) 0.4489(2) 0.0273(11) Uani d 1 . .
O O2D 0.5083(2) 0.5253(4) 0.5041(3) 0.0335(11) Uani d 1 . .
N N1D 0.6176(3) 0.7490(5) 0.3430(3) 0.0319(14) Uani d 1 . .
N N2D 0.6544(3) 0.7994(6) 0.3044(3) 0.0354(15) Uani d 1 . .
H H2DA 0.650230 0.794969 0.265219 0.06(3) Uiso calc 1 . .
N N3D 0.7016(3) 0.8547(5) 0.3897(3) 0.0287(13) Uani d 1 . .
C C1D 0.5384(3) 0.6181(5) 0.4174(4) 0.0278(15) Uani d 1 . .
C C2D 0.4963(3) 0.5530(5) 0.4450(3) 0.0276(15) Uani d 1 . .
C C3D 0.4487(3) 0.5165(6) 0.4145(4) 0.0330(17) Uani d 1 . .
H H3DA 0.420861 0.472560 0.434478 0.040 Uiso calc 1 . .
C C4D 0.4418(3) 0.5441(7) 0.3551(4) 0.0381(18) Uani d 1 . .
H H4DA 0.408760 0.520128 0.334346 0.046 Uiso calc 1 . .
C C5D 0.4820(3) 0.6059(6) 0.3257(4) 0.0365(18) Uani d 1 . .
H H5DA 0.477119 0.623155 0.284384 0.044 Uiso calc 1 . .
C C6D 0.5309(3) 0.6444(6) 0.3562(4) 0.0319(16) Uani d 1 . .
C C7D 0.4621(4) 0.4883(7) 0.5406(4) 0.045(2) Uani d 1 . .
H H7DA 0.451192 0.411766 0.528798 0.067 Uiso calc 1 . .
H H7DB 0.429829 0.539144 0.535135 0.067 Uiso calc 1 . .
H H7DC 0.473691 0.488523 0.582776 0.067 Uiso calc 1 . .
C C8D 0.5718(3) 0.7045(6) 0.3210(4) 0.0324(16) Uani d 1 . .
H H8DA 0.564968 0.712128 0.279187 0.039 Uiso calc 1 . .
C C9D 0.6979(3) 0.8568(6) 0.3297(4) 0.0333(17) Uani d 1 . .
C C10D 0.7367(4) 0.9166(7) 0.2944(4) 0.0397(19) Uani d 1 . .
H H10D 0.734936 0.914895 0.251865 0.048 Uiso calc 1 . .
C C11D 0.7779(4) 0.9786(7) 0.3244(5) 0.046(2) Uani d 1 . .
H H11D 0.804852 1.020685 0.302010 0.056 Uiso calc 1 . .
C C12D 0.7801(3) 0.9795(6) 0.3863(5) 0.042(2) Uani d 1 . .
H H12D 0.807932 1.023129 0.406559 0.050 Uiso calc 1 . .
C C13D 0.7415(3) 0.9164(6) 0.4182(4) 0.0342(17) Uani d 1 . .
H H13D 0.742885 0.916202 0.460822 0.041 Uiso calc 1 . .
Cl Cl1 0.52002(8) 0.25270(17) 0.65520(9) 0.0359(4) Uani d 1 . .
O O11 0.4683(2) 0.1969(6) 0.6705(3) 0.0526(16) Uani d 1 . .
O O12 0.5136(3) 0.3696(5) 0.6678(3) 0.0580(18) Uani d 1 . .
O O13 0.5308(4) 0.2377(7) 0.5934(3) 0.071(2) Uani d 1 . .
O O14 0.5644(3) 0.2096(7) 0.6908(3) 0.072(2) Uani d 1 . .
Cl Cl2 0.64516(10) 0.75422(18) 0.80261(10) 0.0462(5) Uani d 1 . .
O O21 0.6408(13) 0.711(2) 0.8612(9) 0.044(6) Uani d 0.57(6) A 1
O O22 0.6361(18) 0.6641(19) 0.7612(13) 0.072(8) Uani d 0.57(6) A 1
O O23 0.6043(10) 0.8369(17) 0.7913(11) 0.056(6) Uani d 0.57(6) A 1
O O24 0.7018(7) 0.797(3) 0.7964(16) 0.097(9) Uani d 0.57(6) A 1
O O21A 0.6366(17) 0.693(3) 0.8554(11) 0.053(11) Uani d 0.43(6) A 2
O O22A 0.6610(18) 0.677(2) 0.7558(11) 0.053(8) Uani d 0.43(6) A 2
O O23A 0.5915(12) 0.800(5) 0.7822(16) 0.081(11) Uani d 0.43(6) A 2
O O24A 0.685(2) 0.838(3) 0.8092(13) 0.093(12) Uani d 0.43(6) A 2
Cl Cl3 0.86202(15) 0.6242(4) 0.76039(17) 0.0898(11) Uani d 1 . .
O O31 0.9121(5) 0.6848(11) 0.7412(6) 0.144(5) Uani d 1 . .
O O32 0.8498(7) 0.5395(12) 0.7231(6) 0.064(4) Uani d 0.512(13) B 1
O O33 0.8143(6) 0.7097(13) 0.7581(8) 0.074(4) Uani d 0.512(13) B 1
O O34 0.8732(11) 0.598(2) 0.8193(7) 0.076(5) Uani d 0.512(13) B 1
O O32A 0.8836(6) 0.4985(11) 0.7347(6) 0.057(4) Uani d 0.488(13) B 2
O O33A 0.8224(7) 0.6441(15) 0.7248(7) 0.079(4) Uani d 0.488(13) B 2
O O34A 0.8626(12) 0.610(2) 0.8193(7) 0.068(5) Uani d 0.488(13) B 2
Cl Cl4 0.32147(12) 0.5162(3) 0.59552(15) 0.0719(8) Uani d 1 . .
O O41 0.3017(5) 0.4882(10) 0.6510(4) 0.076(3) Uani d 0.806(12) C 1
O O42 0.3541(5) 0.6162(7) 0.6010(5) 0.063(3) Uani d 0.806(12) C 1
O O43 0.3553(5) 0.4174(9) 0.5809(6) 0.092(4) Uani d 0.806(12) C 1
O O44 0.2846(5) 0.5263(11) 0.5485(4) 0.087(4) Uani d 0.806(12) C 1
O O41A 0.2808(14) 0.491(4) 0.6390(16) 0.099(14) Uani d 0.194(12) C 2
O O42A 0.3754(9) 0.486(4) 0.6243(13) 0.106(9) Uani d 0.194(12) C 2
O O43A 0.3244(17) 0.6325(18) 0.5851(18) 0.061(8) Uani d 0.194(12) C 2
O O44A 0.3147(16) 0.457(3) 0.5430(13) 0.072(9) Uani d 0.194(12) C 2
N N1S 0.4678(4) 0.9156(9) 0.4038(4) 0.075(3) Uani d 1 . .
C C11S 0.4759(4) 0.9363(7) 0.3557(5) 0.051(2) Uani d 1 . .
C C12S 0.4883(6) 0.9668(10) 0.2935(5) 0.071(3) Uani d 1 . .
H H12E 0.529373 0.972979 0.288126 0.106 Uiso calc 1 . .
H H12F 0.470415 1.039174 0.284150 0.106 Uiso calc 1 . .
H H12G 0.473352 0.908563 0.266681 0.106 Uiso calc 1 . .
O O1W 0.5643(5) 0.4311(10) 0.2040(5) 0.040(4) Uani d 0.51(2) D 1
H H1W1 0.538(4) 0.468(11) 0.2161(18) 0.060 Uiso d 0.51(2) D 1
H H1W2 0.587(6) 0.474(11) 0.189(9) 0.060 Uiso d 0.51(2) D 1
O O1WA 0.5995(10) 0.3463(16) 0.1981(8) 0.096(9) Uani d 0.49(2) D 2
H H1W3 0.602(13) 0.411(14) 0.19(2) 0.144 Uiso d 0.49(2) D 2
H H1W4 0.565(3) 0.33(2) 0.199(5) 0.144 Uiso d 0.49(2) D 2
O O2W 0.6389(3) 0.7126(6) 0.1929(3) 0.0547(17) Uani d 1 . .
H H2W1 0.6042(15) 0.712(10) 0.185(5) 0.082 Uiso d 1 . .
H H2W2 0.651(4) 0.670(9) 0.167(4) 0.082 Uiso d 1 . .
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1A Ni1 O1A . . 92.2(2) y
N1A Ni1 N3A . . 81.6(2) y
O1A Ni1 N3A . . 173.5(2) y
N1A Ni1 O1B . . 171.2(2) y
O1A Ni1 O1B . . 87.1(2) y
N3A Ni1 O1B . . 98.8(2) y
N1A Ni1 O2B . . 113.4(2) y
O1A Ni1 O2B . . 98.83(19) y
N3A Ni1 O2B . . 85.3(2) y
O1B Ni1 O2B . . 75.39(17) y
N1B Ni2 O1B . . 91.3(2) y
N1B Ni2 N3B . . 82.0(2) y
O1B Ni2 N3B . . 171.8(2) y
N1B Ni2 O1C . . 172.1(2) y
O1B Ni2 O1C . . 88.8(2) y
N3B Ni2 O1C . . 97.1(2) y
N1B Ni2 O2C . . 111.7(2) y
O1B Ni2 O2C . . 97.69(18) y
N3B Ni2 O2C . . 89.2(2) y
O1C Ni2 O2C . . 76.02(19) y
N1C Ni3 O1C . . 91.2(2) y
N1C Ni3 N3C . . 82.4(3) y
O1C Ni3 N3C . . 172.3(2) y
N1C Ni3 O1D . . 172.1(2) y
O1C Ni3 O1D . . 88.1(2) y
N3C Ni3 O1D . . 97.7(2) y
N1C Ni3 O2D . . 111.5(2) y
O1C Ni3 O2D . . 99.81(19) y
N3C Ni3 O2D . . 86.5(2) y
O1D Ni3 O2D . . 76.3(2) y
N1D Ni4 O1D . . 89.9(2) y
N1D Ni4 N3D . . 81.9(3) y
O1D Ni4 N3D . . 170.6(2) y
N1D Ni4 O1A . . 169.1(2) y
O1D Ni4 O1A . . 89.5(2) y
N3D Ni4 O1A . . 97.8(2) y
N1D Ni4 O2A . . 116.3(2) y
O1D Ni4 O2A . . 100.3(2) y
N3D Ni4 O2A . . 87.4(2) y
O1A Ni4 O2A . . 74.5(2) y
C1A O1A Ni1 . . 125.5(4) ?
C1A O1A Ni4 . . 121.3(4) ?
Ni1 O1A Ni4 . . 112.2(2) ?
C2A O2A C7A . . 116.2(6) ?
C2A O2A Ni4 . . 113.0(4) ?
C7A O2A Ni4 . . 129.4(5) ?
C8A N1A N2A . . 118.3(7) ?
C8A N1A Ni1 . . 128.8(5) ?
N2A N1A Ni1 . . 112.9(5) ?
C9A N2A N1A . . 115.8(6) ?
C9A N2A H2AA . . 122.1 ?
N1A N2A H2AA . . 122.1 ?
C9A N3A C13A . . 118.5(6) ?
C9A N3A Ni1 . . 113.1(5) ?
C13A N3A Ni1 . . 128.2(5) ?
O1A C1A C6A . . 123.8(6) ?
O1A C1A C2A . . 117.9(7) ?
C6A C1A C2A . . 118.3(6) ?
O2A C2A C3A . . 125.7(7) ?
O2A C2A C1A . . 113.3(6) ?
C3A C2A C1A . . 120.8(8) ?
C4A C3A C2A . . 120.2(8) ?
C4A C3A H3AA . . 119.9 ?
C2A C3A H3AA . . 119.9 ?
C3A C4A C5A . . 120.5(8) ?
C3A C4A H4AA . . 119.7 ?
C5A C4A H4AA . . 119.7 ?
C4A C5A C6A . . 120.3(9) ?
C4A C5A H5AA . . 119.8 ?
C6A C5A H5AA . . 119.8 ?
C1A C6A C5A . . 119.8(7) ?
C1A C6A C8A . . 124.7(6) ?
C5A C6A C8A . . 115.5(7) ?
O2A C7A H7AA . . 109.5 ?
O2A C7A H7AB . . 109.5 ?
H7AA C7A H7AB . . 109.5 ?
O2A C7A H7AC . . 109.5 ?
H7AA C7A H7AC . . 109.5 ?
H7AB C7A H7AC . . 109.5 ?
N1A C8A C6A . . 123.6(7) ?
N1A C8A H8AA . . 118.2 ?
C6A C8A H8AA . . 118.2 ?
N3A C9A N2A . . 116.2(6) ?
N3A C9A C10A . . 122.2(7) ?
N2A C9A C10A . . 121.6(7) ?
C11A C10A C9A . . 118.8(8) ?
C11A C10A H10A . . 120.6 ?
C9A C10A H10A . . 120.6 ?
C10A C11A C12A . . 120.7(7) ?
C10A C11A H11A . . 119.6 ?
C12A C11A H11A . . 119.6 ?
C13A C12A C11A . . 117.5(7) ?
C13A C12A H12A . . 121.2 ?
C11A C12A H12A . . 121.2 ?
N3A C13A C12A . . 122.2(7) ?
N3A C13A H13A . . 118.9 ?
C12A C13A H13A . . 118.9 ?
C1B O1B Ni2 . . 125.4(4) ?
C1B O1B Ni1 . . 118.9(4) ?
Ni2 O1B Ni1 . . 111.5(2) ?
C2B O2B C7B . . 117.9(5) ?
C2B O2B Ni1 . . 111.1(4) ?
C7B O2B Ni1 . . 125.4(4) ?
C8B N1B N2B . . 118.7(6) ?
C8B N1B Ni2 . . 129.1(5) ?
N2B N1B Ni2 . . 112.1(4) ?
C9B N2B N1B . . 116.7(6) ?
C9B N2B H2BA . . 121.7 ?
N1B N2B H2BA . . 121.7 ?
C9B N3B C13B . . 119.4(6) ?
C9B N3B Ni2 . . 112.6(5) ?
C13B N3B Ni2 . . 128.0(5) ?
O1B C1B C2B . . 118.5(6) ?
O1B C1B C6B . . 122.7(6) ?
C2B C1B C6B . . 118.8(6) ?
O2B C2B C3B . . 123.8(6) ?
O2B C2B C1B . . 114.3(6) ?
C3B C2B C1B . . 121.8(7) ?
C2B C3B C4B . . 118.7(7) ?
C2B C3B H3BA . . 120.6 ?
C4B C3B H3BA . . 120.6 ?
C5B C4B C3B . . 120.7(7) ?
C5B C4B H4BA . . 119.7 ?
C3B C4B H4BA . . 119.7 ?
C4B C5B C6B . . 121.2(7) ?
C4B C5B H5BA . . 119.4 ?
C6B C5B H5BA . . 119.4 ?
C1B C6B C5B . . 118.8(6) ?
C1B C6B C8B . . 125.1(6) ?
C5B C6B C8B . . 116.1(6) ?
O2B C7B H7BA . . 109.5 ?
O2B C7B H7BB . . 109.5 ?
H7BA C7B H7BB . . 109.5 ?
O2B C7B H7BC . . 109.5 ?
H7BA C7B H7BC . . 109.5 ?
H7BB C7B H7BC . . 109.5 ?
N1B C8B C6B . . 122.9(7) ?
N1B C8B H8BA . . 118.6 ?
C6B C8B H8BA . . 118.6 ?
N3B C9B N2B . . 115.9(6) ?
N3B C9B C10B . . 121.2(7) ?
N2B C9B C10B . . 122.9(7) ?
C11B C10B C9B . . 118.5(8) ?
C11B C10B H10B . . 120.7 ?
C9B C10B H10B . . 120.7 ?
C10B C11B C12B . . 120.2(7) ?
C10B C11B H11B . . 119.9 ?
C12B C11B H11B . . 119.9 ?
C13B C12B C11B . . 118.8(7) ?
C13B C12B H12B . . 120.6 ?
C11B C12B H12B . . 120.6 ?
C12B C13B N3B . . 121.7(8) ?
C12B C13B H13B . . 119.1 ?
N3B C13B H13B . . 119.1 ?
C1C O1C Ni3 . . 126.9(5) ?
C1C O1C Ni2 . . 118.8(4) ?
Ni3 O1C Ni2 . . 112.6(2) ?
C2C O2C C7C . . 118.5(6) ?
C2C O2C Ni2 . . 111.7(4) ?
C7C O2C Ni2 . . 127.8(5) ?
C8C N1C N2C . . 118.7(7) ?
C8C N1C Ni3 . . 128.3(6) ?
N2C N1C Ni3 . . 112.8(5) ?
C9C N2C N1C . . 115.9(7) ?
C9C N2C H2CA . . 122.1 ?
N1C N2C H2CA . . 122.1 ?
C13C N3C C9C . . 118.6(6) ?
C13C N3C Ni3 . . 129.0(5) ?
C9C N3C Ni3 . . 112.4(5) ?
O1C C1C C6C . . 123.0(6) ?
O1C C1C C2C . . 118.7(7) ?
C6C C1C C2C . . 118.3(6) ?
O2C C2C C3C . . 124.2(7) ?
O2C C2C C1C . . 114.4(6) ?
C3C C2C C1C . . 121.3(8) ?
C2C C3C C4C . . 119.6(7) ?
C2C C3C H3CA . . 120.2 ?
C4C C3C H3CA . . 120.2 ?
C5C C4C C3C . . 119.8(7) ?
C5C C4C H4CA . . 120.1 ?
C3C C4C H4CA . . 120.1 ?
C4C C5C C6C . . 122.0(8) ?
C4C C5C H5CA . . 119.0 ?
C6C C5C H5CA . . 119.0 ?
C5C C6C C1C . . 119.0(7) ?
C5C C6C C8C . . 117.2(8) ?
C1C C6C C8C . . 123.8(7) ?
O2C C7C H7CA . . 109.5 ?
O2C C7C H7CB . . 109.5 ?
H7CA C7C H7CB . . 109.5 ?
O2C C7C H7CC . . 109.5 ?
H7CA C7C H7CC . . 109.5 ?
H7CB C7C H7CC . . 109.5 ?
N1C C8C C6C . . 125.2(7) ?
N1C C8C H8CA . . 117.4 ?
C6C C8C H8CA . . 117.4 ?
N3C C9C N2C . . 116.4(7) ?
N3C C9C C10C . . 122.5(7) ?
N2C C9C C10C . . 121.1(7) ?
C11C C10C C9C . . 117.5(8) ?
C11C C10C H10C . . 121.3 ?
C9C C10C H10C . . 121.3 ?
C10C C11C C12C . . 120.5(8) ?
C10C C11C H11C . . 119.7 ?
C12C C11C H11C . . 119.7 ?
C13C C12C C11C . . 118.8(8) ?
C13C C12C H12C . . 120.6 ?
C11C C12C H12C . . 120.6 ?
N3C C13C C12C . . 122.0(8) ?
N3C C13C H13C . . 119.0 ?
C12C C13C H13C . . 119.0 ?
C1D O1D Ni4 . . 127.6(5) ?
C1D O1D Ni3 . . 118.5(4) ?
Ni4 O1D Ni3 . . 112.3(2) ?
C2D O2D C7D . . 117.2(6) ?
C2D O2D Ni3 . . 111.3(4) ?
C7D O2D Ni3 . . 126.9(5) ?
C8D N1D N2D . . 118.1(7) ?
C8D N1D Ni4 . . 129.7(5) ?
N2D N1D Ni4 . . 112.2(5) ?
C9D N2D N1D . . 116.1(7) ?
C9D N2D H2DA . . 121.9 ?
N1D N2D H2DA . . 121.9 ?
C9D N3D C13D . . 120.3(7) ?
C9D N3D Ni4 . . 112.0(5) ?
C13D N3D Ni4 . . 127.7(6) ?
O1D C1D C2D . . 119.7(7) ?
O1D C1D C6D . . 122.9(6) ?
C2D C1D C6D . . 117.2(7) ?
C3D C2D O2D . . 124.0(6) ?
C3D C2D C1D . . 122.2(7) ?
O2D C2D C1D . . 113.8(6) ?
C4D C3D C2D . . 119.8(7) ?
C4D C3D H3DA . . 120.1 ?
C2D C3D H3DA . . 120.1 ?
C5D C4D C3D . . 120.5(7) ?
C5D C4D H4DA . . 119.7 ?
C3D C4D H4DA . . 119.7 ?
C4D C5D C6D . . 120.5(8) ?
C4D C5D H5DA . . 119.7 ?
C6D C5D H5DA . . 119.7 ?
C1D C6D C5D . . 119.8(7) ?
C1D C6D C8D . . 123.8(7) ?
C5D C6D C8D . . 116.4(7) ?
O2D C7D H7DA . . 109.5 ?
O2D C7D H7DB . . 109.5 ?
H7DA C7D H7DB . . 109.5 ?
O2D C7D H7DC . . 109.5 ?
H7DA C7D H7DC . . 109.5 ?
H7DB C7D H7DC . . 109.5 ?
N1D C8D C6D . . 123.7(7) ?
N1D C8D H8DA . . 118.2 ?
C6D C8D H8DA . . 118.2 ?
N3D C9D N2D . . 117.1(7) ?
N3D C9D C10D . . 121.9(8) ?
N2D C9D C10D . . 121.0(8) ?
C11D C10D C9D . . 117.1(8) ?
C11D C10D H10D . . 121.5 ?
C9D C10D H10D . . 121.5 ?
C12D C11D C10D . . 120.7(8) ?
C12D C11D H11D . . 119.6 ?
C10D C11D H11D . . 119.6 ?
C13D C12D C11D . . 119.1(8) ?
C13D C12D H12D . . 120.4 ?
C11D C12D H12D . . 120.4 ?
N3D C13D C12D . . 120.8(9) ?
N3D C13D H13D . . 119.6 ?
C12D C13D H13D . . 119.6 ?
O14 Cl1 O13 . . 111.7(5) ?
O14 Cl1 O12 . . 108.8(5) ?
O13 Cl1 O12 . . 109.5(4) ?
O14 Cl1 O11 . . 109.3(4) ?
O13 Cl1 O11 . . 109.1(5) ?
O12 Cl1 O11 . . 108.3(4) ?
O24A Cl2 O21A . . 112.5(17) ?
O23 Cl2 O21 . . 111.8(11) ?
O23 Cl2 O22 . . 107.8(11) ?
O21 Cl2 O22 . . 108.6(13) ?
O24A Cl2 O22A . . 111.1(14) ?
O21A Cl2 O22A . . 108.6(16) ?
O23 Cl2 O24 . . 112.1(12) ?
O21 Cl2 O24 . . 106.6(13) ?
O22 Cl2 O24 . . 109.9(12) ?
O24A Cl2 O23A . . 111.2(15) ?
O21A Cl2 O23A . . 109.4(17) ?
O22A Cl2 O23A . . 103.7(15) ?
O33A Cl3 O34A . . 131.5(15) ?
O32 Cl3 O34 . . 117.6(13) ?
O33A Cl3 O31 . . 109.2(10) ?
O34A Cl3 O31 . . 110.4(13) ?
O32 Cl3 O31 . . 111.5(9) ?
O34 Cl3 O31 . . 103.8(12) ?
O32 Cl3 O33 . . 108.8(9) ?
O34 Cl3 O33 . . 109.1(13) ?
O31 Cl3 O33 . . 105.3(8) ?
O33A Cl3 O32A . . 100.3(10) ?
O34A Cl3 O32A . . 102.7(13) ?
O31 Cl3 O32A . . 95.4(7) ?
O41 Cl4 O44 . . 120.0(7) ?
O44A Cl4 O41A . . 114(2) ?
O44A Cl4 O43A . . 111.8(18) ?
O41A Cl4 O43A . . 111(2) ?
O41 Cl4 O42 . . 108.1(7) ?
O44 Cl4 O42 . . 109.7(7) ?
O41 Cl4 O43 . . 101.2(7) ?
O44 Cl4 O43 . . 104.3(8) ?
O42 Cl4 O43 . . 113.3(7) ?
O44A Cl4 O42A . . 110.2(17) ?
O41A Cl4 O42A . . 104.0(18) ?
O43A Cl4 O42A . . 105.6(18) ?
N1S C11S C12S . . 177.7(12) ?
C11S C12S H12E . . 109.5 ?
C11S C12S H12F . . 109.5 ?
H12E C12S H12F . . 109.5 ?
C11S C12S H12G . . 109.5 ?
H12E C12S H12G . . 109.5 ?
H12F C12S H12G . . 109.5 ?
H1W1 O1W H1W2 . . 107(5) ?
H1W3 O1WA H1W4 . . 108(5) ?
H2W1 O2W H2W2 . . 102(4) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 N1A . 1.932(7) y
Ni1 O1A . 1.960(5) y
Ni1 N3A . 1.980(6) y
Ni1 O1B . 1.998(5) y
Ni1 O2B . 2.276(4) y
Ni2 N1B . 1.935(6) y
Ni2 O1B . 1.962(4) y
Ni2 N3B . 1.971(6) y
Ni2 O1C . 1.997(5) y
Ni2 O2C . 2.257(5) y
Ni3 N1C . 1.932(7) y
Ni3 O1C . 1.965(5) y
Ni3 N3C . 1.975(6) y
Ni3 O1D . 1.993(5) y
Ni3 O2D . 2.264(5) y
Ni4 N1D . 1.948(7) y
Ni4 O1D . 1.950(5) y
Ni4 N3D . 1.969(6) y
Ni4 O1A . 1.993(5) y
Ni4 O2A . 2.283(5) y
O1A C1A . 1.365(8) ?
O2A C2A . 1.378(10) ?
O2A C7A . 1.439(8) ?
N1A C8A . 1.305(9) ?
N1A N2A . 1.377(9) ?
N2A C9A . 1.364(10) ?
N2A H2AA . 0.8800 ?
N3A C9A . 1.330(9) ?
N3A C13A . 1.356(9) ?
C1A C6A . 1.396(11) ?
C1A C2A . 1.414(10) ?
C2A C3A . 1.379(10) ?
C3A C4A . 1.370(13) ?
C3A H3AA . 0.9500 ?
C4A C5A . 1.378(13) ?
C4A H4AA . 0.9500 ?
C5A C6A . 1.403(10) ?
C5A H5AA . 0.9500 ?
C6A C8A . 1.441(11) ?
C7A H7AA . 0.9800 ?
C7A H7AB . 0.9800 ?
C7A H7AC . 0.9800 ?
C8A H8AA . 0.9500 ?
C9A C10A . 1.411(10) ?
C10A C11A . 1.330(12) ?
C10A H10A . 0.9500 ?
C11A C12A . 1.408(12) ?
C11A H11A . 0.9500 ?
C12A C13A . 1.384(10) ?
C12A H12A . 0.9500 ?
C13A H13A . 0.9500 ?
O1B C1B . 1.367(8) ?
O2B C2B . 1.380(8) ?
O2B C7B . 1.435(8) ?
N1B C8B . 1.292(9) ?
N1B N2B . 1.377(8) ?
N2B C9B . 1.353(10) ?
N2B H2BA . 0.8800 ?
N3B C9B . 1.351(10) ?
N3B C13B . 1.360(9) ?
C1B C2B . 1.402(9) ?
C1B C6B . 1.404(10) ?
C2B C3B . 1.387(10) ?
C3B C4B . 1.398(10) ?
C3B H3BA . 0.9500 ?
C4B C5B . 1.364(10) ?
C4B H4BA . 0.9500 ?
C5B C6B . 1.414(10) ?
C5B H5BA . 0.9500 ?
C6B C8B . 1.453(10) ?
C7B H7BA . 0.9800 ?
C7B H7BB . 0.9800 ?
C7B H7BC . 0.9800 ?
C8B H8BA . 0.9500 ?
C9B C10B . 1.408(10) ?
C10B C11B . 1.356(12) ?
C10B H10B . 0.9500 ?
C11B C12B . 1.411(12) ?
C11B H11B . 0.9500 ?
C12B C13B . 1.360(10) ?
C12B H12B . 0.9500 ?
C13B H13B . 0.9500 ?
O1C C1C . 1.355(8) ?
O2C C2C . 1.368(9) ?
O2C C7C . 1.439(9) ?
N1C C8C . 1.290(9) ?
N1C N2C . 1.381(9) ?
N2C C9C . 1.371(10) ?
N2C H2CA . 0.8800 ?
N3C C13C . 1.341(9) ?
N3C C9C . 1.347(10) ?
C1C C6C . 1.406(11) ?
C1C C2C . 1.410(10) ?
C2C C3C . 1.386(10) ?
C3C C4C . 1.393(12) ?
C3C H3CA . 0.9500 ?
C4C C5C . 1.363(12) ?
C4C H4CA . 0.9500 ?
C5C C6C . 1.401(10) ?
C5C H5CA . 0.9500 ?
C6C C8C . 1.434(11) ?
C7C H7CA . 0.9800 ?
C7C H7CB . 0.9800 ?
C7C H7CC . 0.9800 ?
C8C H8CA . 0.9500 ?
C9C C10C . 1.409(11) ?
C10C C11C . 1.355(13) ?
C10C H10C . 0.9500 ?
C11C C12C . 1.397(13) ?
C11C H11C . 0.9500 ?
C12C C13C . 1.375(10) ?
C12C H12C . 0.9500 ?
C13C H13C . 0.9500 ?
O1D C1D . 1.360(9) ?
O2D C2D . 1.387(9) ?
O2D C7D . 1.429(9) ?
N1D C8D . 1.300(10) ?
N1D N2D . 1.362(9) ?
N2D C9D . 1.355(11) ?
N2D H2DA . 0.8800 ?
N3D C9D . 1.341(10) ?
N3D C13D . 1.351(10) ?
C1D C2D . 1.403(10) ?
C1D C6D . 1.410(11) ?
C2D C3D . 1.383(10) ?
C3D C4D . 1.373(12) ?
C3D H3DA . 0.9500 ?
C4D C5D . 1.368(12) ?
C4D H4DA . 0.9500 ?
C5D C6D . 1.416(11) ?
C5D H5DA . 0.9500 ?
C6D C8D . 1.433(11) ?
C7D H7DA . 0.9800 ?
C7D H7DB . 0.9800 ?
C7D H7DC . 0.9800 ?
C8D H8DA . 0.9500 ?
C9D C10D . 1.401(11) ?
C10D C11D . 1.390(13) ?
C10D H10D . 0.9500 ?
C11D C12D . 1.381(14) ?
C11D H11D . 0.9500 ?
C12D C13D . 1.380(11) ?
C12D H12D . 0.9500 ?
C13D H13D . 0.9500 ?
Cl1 O14 . 1.409(6) ?
Cl1 O13 . 1.413(7) ?
Cl1 O12 . 1.424(6) ?
Cl1 O11 . 1.429(6) ?
Cl2 O24A . 1.378(18) ?
Cl2 O21A . 1.397(18) ?
Cl2 O23 . 1.399(14) ?
Cl2 O21 . 1.405(15) ?
Cl2 O22 . 1.430(14) ?
Cl2 O22A . 1.437(17) ?
Cl2 O24 . 1.438(14) ?
Cl2 O23A . 1.449(17) ?
Cl3 O33A . 1.248(12) ?
Cl3 O34A . 1.326(15) ?
Cl3 O32 . 1.336(12) ?
Cl3 O34 . 1.377(15) ?
Cl3 O31 . 1.448(9) ?
Cl3 O33 . 1.517(12) ?
Cl3 O32A . 1.677(14) ?
Cl4 O41 . 1.363(9) ?
Cl4 O44 . 1.368(9) ?
Cl4 O44A . 1.38(2) ?
Cl4 O41A . 1.40(2) ?
Cl4 O43A . 1.40(2) ?
Cl4 O42 . 1.420(9) ?
Cl4 O43 . 1.457(10) ?
Cl4 O42A . 1.47(2) ?
N1S C11S . 1.117(13) ?
C11S C12S . 1.462(15) ?
C12S H12E . 0.9800 ?
C12S H12F . 0.9800 ?
C12S H12G . 0.9800 ?
O1W H1W1 . 0.80(3) ?
O1W H1W2 . 0.82(3) ?
O1WA H1W3 . 0.82(3) ?
O1WA H1W4 . 0.82(3) ?
O2W H2W1 . 0.84(3) ?
O2W H2W2 . 0.83(3) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C7B H7BB N1S 3_565 0.98 2.60 3.523(11) 156.8 yes
C13B H13B O13 . 0.95 2.42 3.126(9) 130.7 yes
C13C H13C N1S . 0.95 2.59 3.348(11) 136.8 yes
N2D H2DA O2W . 0.88 1.91 2.720(9) 151.5 yes
C7D H7DC O12 . 0.98 2.56 3.389(10) 141.8 yes
C12S H12G O14 2_664 0.98 2.37 3.335(12) 167.5 yes
O2W H2W1 O11 2_664 0.84(3) 2.12(7) 2.795(8) 138(9) yes
O2W H2W2 Cl4 2_664 0.83(3) 2.78(3) 3.599(6) 170(9) yes
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C8A N1A N2A C9A . . . . -174.9(6) ?
Ni1 N1A N2A C9A . . . . 6.2(7) ?
Ni1 O1A C1A C6A . . . . -14.8(9) ?
Ni4 O1A C1A C6A . . . . 177.7(5) ?
Ni1 O1A C1A C2A . . . . 167.0(4) ?
Ni4 O1A C1A C2A . . . . -0.5(8) ?
C7A O2A C2A C3A . . . . 17.2(10) ?
Ni4 O2A C2A C3A . . . . -175.2(6) ?
C7A O2A C2A C1A . . . . -166.9(6) ?
Ni4 O2A C2A C1A . . . . 0.8(7) ?
O1A C1A C2A O2A . . . . -0.2(8) ?
C6A C1A C2A O2A . . . . -178.6(6) ?
O1A C1A C2A C3A . . . . 175.9(6) ?
C6A C1A C2A C3A . . . . -2.4(10) ?
O2A C2A C3A C4A . . . . 176.9(7) ?
C1A C2A C3A C4A . . . . 1.2(11) ?
C2A C3A C4A C5A . . . . 0.1(12) ?
C3A C4A C5A C6A . . . . -0.2(12) ?
O1A C1A C6A C5A . . . . -175.9(6) ?
C2A C1A C6A C5A . . . . 2.3(10) ?
O1A C1A C6A C8A . . . . 5.5(11) ?
C2A C1A C6A C8A . . . . -176.2(6) ?
C4A C5A C6A C1A . . . . -1.1(11) ?
C4A C5A C6A C8A . . . . 177.6(7) ?
N2A N1A C8A C6A . . . . 178.6(6) ?
Ni1 N1A C8A C6A . . . . -2.7(11) ?
C1A C6A C8A N1A . . . . 3.8(11) ?
C5A C6A C8A N1A . . . . -174.8(7) ?
C13A N3A C9A N2A . . . . 178.7(6) ?
Ni1 N3A C9A N2A . . . . 2.9(7) ?
C13A N3A C9A C10A . . . . -2.2(10) ?
Ni1 N3A C9A C10A . . . . -178.0(5) ?
N1A N2A C9A N3A . . . . -6.0(9) ?
N1A N2A C9A C10A . . . . 174.9(6) ?
N3A C9A C10A C11A . . . . 0.4(11) ?
N2A C9A C10A C11A . . . . 179.4(7) ?
C9A C10A C11A C12A . . . . 1.9(11) ?
C10A C11A C12A C13A . . . . -2.2(11) ?
C9A N3A C13A C12A . . . . 1.8(10) ?
Ni1 N3A C13A C12A . . . . 176.9(5) ?
C11A C12A C13A N3A . . . . 0.4(11) ?
C8B N1B N2B C9B . . . . 168.2(6) ?
Ni2 N1B N2B C9B . . . . -8.9(7) ?
Ni2 O1B C1B C2B . . . . -165.5(4) ?
Ni1 O1B C1B C2B . . . . -10.6(7) ?
Ni2 O1B C1B C6B . . . . 16.7(9) ?
Ni1 O1B C1B C6B . . . . 171.7(5) ?
C7B O2B C2B C3B . . . . -16.1(10) ?
Ni1 O2B C2B C3B . . . . -171.2(5) ?
C7B O2B C2B C1B . . . . 164.7(6) ?
Ni1 O2B C2B C1B . . . . 9.6(7) ?
O1B C1B C2B O2B . . . . -0.7(9) ?
C6B C1B C2B O2B . . . . 177.2(6) ?
O1B C1B C2B C3B . . . . -179.9(6) ?
C6B C1B C2B C3B . . . . -2.1(10) ?
O2B C2B C3B C4B . . . . -178.2(6) ?
C1B C2B C3B C4B . . . . 1.0(10) ?
C2B C3B C4B C5B . . . . 1.0(11) ?
C3B C4B C5B C6B . . . . -1.9(11) ?
O1B C1B C6B C5B . . . . 178.9(6) ?
C2B C1B C6B C5B . . . . 1.1(10) ?
O1B C1B C6B C8B . . . . -0.5(10) ?
C2B C1B C6B C8B . . . . -178.3(6) ?
C4B C5B C6B C1B . . . . 0.8(11) ?
C4B C5B C6B C8B . . . . -179.7(7) ?
N2B N1B C8B C6B . . . . 177.2(6) ?
Ni2 N1B C8B C6B . . . . -6.3(10) ?
C1B C6B C8B N1B . . . . -5.2(11) ?
C5B C6B C8B N1B . . . . 175.3(6) ?
C13B N3B C9B N2B . . . . -178.2(6) ?
Ni2 N3B C9B N2B . . . . 2.5(7) ?
C13B N3B C9B C10B . . . . 3.5(10) ?
Ni2 N3B C9B C10B . . . . -175.8(5) ?
N1B N2B C9B N3B . . . . 4.2(9) ?
N1B N2B C9B C10B . . . . -177.5(6) ?
N3B C9B C10B C11B . . . . -2.8(11) ?
N2B C9B C10B C11B . . . . 179.1(7) ?
C9B C10B C11B C12B . . . . -0.2(11) ?
C10B C11B C12B C13B . . . . 2.4(11) ?
C11B C12B C13B N3B . . . . -1.6(10) ?
C9B N3B C13B C12B . . . . -1.3(9) ?
Ni2 N3B C13B C12B . . . . 177.9(5) ?
C8C N1C N2C C9C . . . . -176.2(6) ?
Ni3 N1C N2C C9C . . . . -0.8(7) ?
Ni3 O1C C1C C6C . . . . -12.1(9) ?
Ni2 O1C C1C C6C . . . . -175.5(5) ?
Ni3 O1C C1C C2C . . . . 169.2(5) ?
Ni2 O1C C1C C2C . . . . 5.8(8) ?
C7C O2C C2C C3C . . . . 11.8(10) ?
Ni2 O2C C2C C3C . . . . 176.9(6) ?
C7C O2C C2C C1C . . . . -169.2(6) ?
Ni2 O2C C2C C1C . . . . -4.1(7) ?
O1C C1C C2C O2C . . . . -0.5(9) ?
C6C C1C C2C O2C . . . . -179.3(6) ?
O1C C1C C2C C3C . . . . 178.5(6) ?
C6C C1C C2C C3C . . . . -0.3(10) ?
O2C C2C C3C C4C . . . . 178.5(7) ?
C1C C2C C3C C4C . . . . -0.5(11) ?
C2C C3C C4C C5C . . . . 0.6(12) ?
C3C C4C C5C C6C . . . . 0.1(12) ?
C4C C5C C6C C1C . . . . -0.8(11) ?
C4C C5C C6C C8C . . . . 179.5(7) ?
O1C C1C C6C C5C . . . . -177.8(6) ?
C2C C1C C6C C5C . . . . 0.9(10) ?
O1C C1C C6C C8C . . . . 1.8(10) ?
C2C C1C C6C C8C . . . . -179.5(6) ?
N2C N1C C8C C6C . . . . 179.8(6) ?
Ni3 N1C C8C C6C . . . . 5.2(10) ?
C5C C6C C8C N1C . . . . -178.4(7) ?
C1C C6C C8C N1C . . . . 1.9(11) ?
C13C N3C C9C N2C . . . . 175.7(6) ?
Ni3 N3C C9C N2C . . . . -4.9(8) ?
C13C N3C C9C C10C . . . . -2.6(10) ?
Ni3 N3C C9C C10C . . . . 176.8(6) ?
N1C N2C C9C N3C . . . . 3.9(9) ?
N1C N2C C9C C10C . . . . -177.8(7) ?
N3C C9C C10C C11C . . . . 1.4(12) ?
N2C C9C C10C C11C . . . . -176.8(7) ?
C9C C10C C11C C12C . . . . 0.4(13) ?
C10C C11C C12C C13C . . . . -1.0(13) ?
C9C N3C C13C C12C . . . . 2.0(10) ?
Ni3 N3C C13C C12C . . . . -177.3(6) ?
C11C C12C C13C N3C . . . . -0.3(12) ?
C8D N1D N2D C9D . . . . 172.1(6) ?
Ni4 N1D N2D C9D . . . . -7.5(8) ?
Ni4 O1D C1D C2D . . . . -169.2(4) ?
Ni3 O1D C1D C2D . . . . -5.0(8) ?
Ni4 O1D C1D C6D . . . . 14.1(9) ?
Ni3 O1D C1D C6D . . . . 178.3(5) ?
C7D O2D C2D C3D . . . . -20.3(10) ?
Ni3 O2D C2D C3D . . . . -178.1(5) ?
C7D O2D C2D C1D . . . . 162.5(6) ?
Ni3 O2D C2D C1D . . . . 4.7(7) ?
O1D C1D C2D C3D . . . . -177.7(6) ?
C6D C1D C2D C3D . . . . -0.8(9) ?
O1D C1D C2D O2D . . . . -0.4(9) ?
C6D C1D C2D O2D . . . . 176.5(6) ?
O2D C2D C3D C4D . . . . -177.0(7) ?
C1D C2D C3D C4D . . . . 0.0(10) ?
C2D C3D C4D C5D . . . . 1.0(11) ?
C3D C4D C5D C6D . . . . -1.3(12) ?
O1D C1D C6D C5D . . . . 177.3(6) ?
C2D C1D C6D C5D . . . . 0.5(10) ?
O1D C1D C6D C8D . . . . 0.6(11) ?
C2D C1D C6D C8D . . . . -176.2(6) ?
C4D C5D C6D C1D . . . . 0.5(11) ?
C4D C5D C6D C8D . . . . 177.5(7) ?
N2D N1D C8D C6D . . . . 177.0(7) ?
Ni4 N1D C8D C6D . . . . -3.5(11) ?
C1D C6D C8D N1D . . . . -6.1(11) ?
C5D C6D C8D N1D . . . . 177.1(7) ?
C13D N3D C9D N2D . . . . -175.4(6) ?
Ni4 N3D C9D N2D . . . . 3.8(8) ?
C13D N3D C9D C10D . . . . 3.8(10) ?
Ni4 N3D C9D C10D . . . . -177.0(6) ?
N1D N2D C9D N3D . . . . 2.5(10) ?
N1D N2D C9D C10D . . . . -176.8(7) ?
N3D C9D C10D C11D . . . . -3.0(11) ?
N2D C9D C10D C11D . . . . 176.2(7) ?
C9D C10D C11D C12D . . . . 0.4(12) ?
C10D C11D C12D C13D . . . . 1.2(12) ?
C9D N3D C13D C12D . . . . -2.1(10) ?
Ni4 N3D C13D C12D . . . . 178.9(5) ?
C11D C12D C13D N3D . . . . -0.4(11) ?

_cod_database_fobs_code 2022514
