#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:23:43 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179479 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/76/4337616.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_4337616
loop_
_publ_author_name
'Esteban, Jordi'
'Font-Bardia, Mercè'
'Costa, José Sánchez'
'Teat, Simon J.'
'Escuer, Albert'
_publ_section_title
;
 New topologies in pentanuclear nickel/oximato clusters: structural and
 magnetic characterization.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3194
_journal_page_last               3203
_journal_paper_doi               10.1021/ic500057j
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety
'4(C44 H32 N20 Ni5 O11 S2), C O, 20(C2 H3 N), 16(H2 O)'
_chemical_formula_sum            'C217 H208 N100 Ni20 O62 S8'
_chemical_formula_weight         6639.51
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 101.395(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   32.3601(17)
_cell_length_b                   23.1876(12)
_cell_length_c                   23.2403(13)
_cell_measurement_reflns_used    1859
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.78
_cell_measurement_theta_min      2.51
_cell_volume                     17094.7(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0666
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            17445
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.09
_exptl_absorpt_coefficient_mu    1.196
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             6788
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.753
_refine_diff_density_min         -1.274
_refine_diff_density_rms         0.229
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1007
_refine_ls_number_reflns         17445
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.1002
_refine_ls_R_factor_gt           0.0521
_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)+(0.1127P)²+71.8872P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1787
_refine_ls_wR_factor_ref         0.2148
_reflns_number_gt                10876
_reflns_number_total             17445
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500057j_si_001.cif
_cod_data_source_block           af13fus13a
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4337616
loop_
_symmetry_equiv_pos_as_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'
'-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_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
Ni1 Ni 0.20398(2) 0.35669(3) 0.12653(3) 0.02128(17) Uani 1 1 d .
Ni2 Ni 0.22862(2) 0.35932(3) 0.28064(3) 0.02308(18) Uani 1 1 d .
Ni3 Ni 0.20068(2) 0.50268(3) 0.12384(3) 0.01905(17) Uani 1 1 d .
Ni4 Ni 0.22106(2) 0.50803(3) 0.27550(3) 0.01958(17) Uani 1 1 d .
Ni5 Ni 0.11037(2) 0.42470(3) 0.08601(3) 0.02651(19) Uani 1 1 d .
O1 O 0.16938(11) 0.42810(14) 0.13612(16) 0.0213(8) Uani 1 1 d D
H1O H 0.1666(15) 0.4467(14) 0.1685(4) 0.026 Uiso 1 1 d D
O2 O 0.24198(11) 0.48708(14) 0.20153(16) 0.0216(8) Uani 1 1 d D
H2OA H 0.2681(6) 0.5020(15) 0.2119(16) 0.026 Uiso 1 1 d D
H2OB H 0.2455(13) 0.4475(3) 0.205(2) 0.026 Uiso 1 1 d D
O3 O 0.24620(11) 0.38190(15) 0.20152(16) 0.0241(8) Uani 1 1 d D
H3O H 0.2705(5) 0.3667(17) 0.196(2) 0.029 Uiso 1 1 d D
S1 S 0.33323(5) 0.21270(7) 0.28183(9) 0.0452(4) Uani 1 1 d .
C1 C 0.29587(19) 0.2592(2) 0.2851(3) 0.0309(13) Uani 1 1 d .
N1 N 0.26989(15) 0.2932(2) 0.2878(2) 0.0323(11) Uani 1 1 d .
S2 S 0.09965(7) 0.43139(10) 0.27544(11) 0.0637(6) Uani 1 1 d .
C2 C 0.1487(3) 0.4313(3) 0.2740(3) 0.0493(18) Uani 1 1 d .
N2 N 0.18653(14) 0.43040(17) 0.2674(2) 0.0228(10) Uani 1 1 d D
O4 O 0.12615(12) 0.36113(16) 0.03299(17) 0.0287(9) Uani 1 1 d .
O5 O 0.16804(12) 0.30875(15) 0.17592(16) 0.0267(9) Uani 1 1 d .
O6 O 0.23759(12) 0.40011(15) 0.07309(17) 0.0273(9) Uani 1 1 d .
O7 O 0.15899(12) 0.52354(16) 0.04843(16) 0.0268(9) Uani 1 1 d .
O8 O 0.16349(11) 0.55320(15) 0.16663(16) 0.0226(8) Uani 1 1 d .
O9 O 0.27236(12) 0.40944(15) 0.33589(17) 0.0277(9) Uani 1 1 d .
O10 O 0.09026(13) 0.48683(18) 0.1404(2) 0.0392(10) Uani 1 1 d D
H10O H 0.0671(13) 0.4676(18) 0.150(3) 0.047 Uiso 1 1 d D
H10D H 0.0916(14) 0.5232(10) 0.154(3) 0.047 Uiso 1 1 d D
O11 O 0.09100(13) 0.35821(18) 0.13433(19) 0.0392(10) Uani 1 1 d D
H11O H 0.0686(12) 0.3772(19) 0.144(2) 0.047 Uiso 1 1 d D
H11A H 0.0984(10) 0.3276(15) 0.159(2) 0.047 Uiso 1 1 d D
N3 N 0.23122(14) 0.28092(18) 0.1023(2) 0.0252(10) Uani 1 1 d .
N4 N 0.1183(3) 0.2440(3) -0.0599(4) 0.084(2) Uani 1 1 d .
N5 N 0.15992(14) 0.33262(18) 0.0551(2) 0.0234(10) Uani 1 1 d .
N6 N 0.20151(15) 0.32814(19) 0.3476(2) 0.0272(11) Uani 1 1 d .
N7 N 0.0873(2) 0.2355(3) 0.2197(3) 0.072(2) Uani 1 1 d D
N8 N 0.17931(14) 0.31167(18) 0.2337(2) 0.0255(10) Uani 1 1 d .
N9 N 0.23777(14) 0.56785(18) 0.1008(2) 0.0231(10) Uani 1 1 d .
N10 N 0.3116(2) 0.4396(2) -0.0072(3) 0.0487(15) Uani 1 1 d .
N11 N 0.23863(13) 0.45639(18) 0.07996(19) 0.0214(10) Uani 1 1 d .
N12 N 0.18761(14) 0.53794(18) 0.33861(19) 0.0219(10) Uani 1 1 d .
N13 N 0.07880(16) 0.6246(2) 0.1953(2) 0.0364(12) Uani 1 1 d D
N14 N 0.17216(13) 0.55162(18) 0.22391(19) 0.0200(9) Uani 1 1 d .
N15 N 0.26373(14) 0.57511(18) 0.2976(2) 0.0230(10) Uani 1 1 d .
N16 N 0.3639(2) 0.4589(3) 0.4277(3) 0.0601(18) Uani 1 1 d .
N17 N 0.26975(14) 0.46525(18) 0.32711(19) 0.0227(10) Uani 1 1 d .
N18 N 0.05564(16) 0.4299(2) 0.0235(2) 0.0362(12) Uani 1 1 d .
N19 N 0.1016(2) 0.5933(3) -0.0729(3) 0.0648(19) Uani 1 1 d .
N20 N 0.12407(14) 0.49263(19) 0.0366(2) 0.0253(10) Uani 1 1 d .
C3 C 0.26758(19) 0.2572(2) 0.1270(3) 0.0312(13) Uani 1 1 d .
H3 H 0.2843 0.2755 0.1589 0.037 Uiso 1 1 calc R
C4 C 0.2819(2) 0.2053(3) 0.1065(3) 0.0405(16) Uani 1 1 d .
H4 H 0.3075 0.1894 0.1248 0.049 Uiso 1 1 calc R
C5 C 0.2572(2) 0.1783(3) 0.0588(3) 0.0453(17) Uani 1 1 d .
H5 H 0.2663 0.1444 0.0439 0.054 Uiso 1 1 calc R
C6 C 0.2188(2) 0.2025(3) 0.0335(3) 0.0395(15) Uani 1 1 d .
H6 H 0.2010 0.1846 0.0023 0.047 Uiso 1 1 calc R
C7 C 0.20736(18) 0.2547(2) 0.0562(3) 0.0289(13) Uani 1 1 d .
C8 C 0.16817(18) 0.2844(2) 0.0303(2) 0.0268(12) Uani 1 1 d .
C9 C 0.1405(2) 0.2624(3) -0.0189(3) 0.0479(18) Uani 1 1 d .
C10 C 0.2152(2) 0.3353(3) 0.4049(3) 0.0386(15) Uani 1 1 d .
H10 H 0.2397 0.3563 0.4179 0.046 Uiso 1 1 calc R
C11 C 0.1939(2) 0.3121(3) 0.4464(3) 0.0451(17) Uani 1 1 d .
H11 H 0.2037 0.3189 0.4861 0.054 Uiso 1 1 calc R
C12 C 0.1590(2) 0.2799(3) 0.4283(3) 0.0415(16) Uani 1 1 d .
H12 H 0.1446 0.2642 0.4555 0.050 Uiso 1 1 calc R
C13 C 0.1448(2) 0.2702(3) 0.3683(3) 0.0346(14) Uani 1 1 d .
H13 H 0.1211 0.2479 0.3544 0.042 Uiso 1 1 calc R
C14 C 0.16752(19) 0.2952(2) 0.3302(3) 0.0296(13) Uani 1 1 d .
C15 C 0.15555(19) 0.2885(2) 0.2650(3) 0.0309(13) Uani 1 1 d .
C16 C 0.1180(2) 0.2586(3) 0.2401(3) 0.0429(16) Uani 1 1 d .
C17 C 0.23741(18) 0.6237(2) 0.1146(3) 0.0293(13) Uani 1 1 d .
H17 H 0.2192 0.6363 0.1384 0.035 Uiso 1 1 calc R
C18 C 0.2634(2) 0.6637(3) 0.0947(3) 0.0382(15) Uani 1 1 d .
H18 H 0.2626 0.7024 0.1049 0.046 Uiso 1 1 calc R
C19 C 0.2904(2) 0.6452(3) 0.0597(3) 0.0424(16) Uani 1 1 d .
H19 H 0.3084 0.6711 0.0463 0.051 Uiso 1 1 calc R
C20 C 0.2903(2) 0.5871(3) 0.0445(3) 0.0353(14) Uani 1 1 d .
H20 H 0.3076 0.5739 0.0197 0.042 Uiso 1 1 calc R
C21 C 0.26448(17) 0.5492(2) 0.0666(2) 0.0259(12) Uani 1 1 d .
C22 C 0.26307(18) 0.4872(2) 0.0551(2) 0.0274(12) Uani 1 1 d .
C23 C 0.2909(2) 0.4603(2) 0.0210(3) 0.0330(14) Uani 1 1 d .
C24 C 0.19712(18) 0.5311(2) 0.3969(2) 0.0282(13) Uani 1 1 d .
H24 H 0.2205 0.5089 0.4128 0.034 Uiso 1 1 calc R
C25 C 0.17425(19) 0.5551(3) 0.4341(3) 0.0343(14) Uani 1 1 d .
H25 H 0.1818 0.5490 0.4743 0.041 Uiso 1 1 calc R
C26 C 0.13963(19) 0.5889(3) 0.4109(3) 0.0319(13) Uani 1 1 d .
H26 H 0.1235 0.6060 0.4351 0.038 Uiso 1 1 calc R
C27 C 0.12958(18) 0.5965(2) 0.3498(3) 0.0292(13) Uani 1 1 d .
H27 H 0.1065 0.6188 0.3329 0.035 Uiso 1 1 calc R
C28 C 0.15410(16) 0.5709(2) 0.3155(2) 0.0214(11) Uani 1 1 d .
C29 C 0.14510(16) 0.5753(2) 0.2517(2) 0.0200(11) Uani 1 1 d .
C30 C 0.10828(17) 0.6034(2) 0.2208(2) 0.0234(12) Uani 1 1 d .
C31 C 0.25996(18) 0.6295(2) 0.2790(2) 0.0261(12) Uani 1 1 d .
H31 H 0.2360 0.6402 0.2520 0.031 Uiso 1 1 calc R
C32 C 0.29036(19) 0.6709(3) 0.2984(3) 0.0344(14) Uani 1 1 d .
H32 H 0.2872 0.7083 0.2840 0.041 Uiso 1 1 calc R
C33 C 0.3256(2) 0.6554(3) 0.3397(3) 0.0367(15) Uani 1 1 d .
H33 H 0.3463 0.6826 0.3537 0.044 Uiso 1 1 calc R
C34 C 0.32983(18) 0.5990(2) 0.3599(3) 0.0308(13) Uani 1 1 d .
H34 H 0.3535 0.5881 0.3874 0.037 Uiso 1 1 calc R
C35 C 0.29873(17) 0.5590(2) 0.3390(2) 0.0247(12) Uani 1 1 d .
C36 C 0.30069(17) 0.4981(2) 0.3533(2) 0.0237(12) Uani 1 1 d .
C37 C 0.33550(19) 0.4756(3) 0.3934(3) 0.0346(14) Uani 1 1 d .
C38 C 0.0217(2) 0.3946(3) 0.0180(4) 0.0510(19) Uani 1 1 d .
H38 H 0.0202 0.3670 0.0465 0.061 Uiso 1 1 calc R
C39 C -0.0107(2) 0.3999(4) -0.0308(4) 0.062(2) Uani 1 1 d .
H39 H -0.0337 0.3751 -0.0353 0.074 Uiso 1 1 calc R
C40 C -0.0092(3) 0.4402(4) -0.0714(4) 0.069(3) Uani 1 1 d .
H40 H -0.0316 0.4438 -0.1031 0.083 Uiso 1 1 calc R
C41 C 0.0252(2) 0.4769(3) -0.0671(3) 0.0499(18) Uani 1 1 d .
H41 H 0.0270 0.5041 -0.0960 0.060 Uiso 1 1 calc R
C42 C 0.0570(2) 0.4706(3) -0.0168(3) 0.0386(15) Uani 1 1 d .
C43 C 0.09547(19) 0.5059(2) -0.0070(3) 0.0310(13) Uani 1 1 d .
C44 C 0.0991(2) 0.5546(3) -0.0438(3) 0.0435(16) Uani 1 1 d .
N1A N -0.0124(3) 0.5926(5) -0.1663(6) 0.0593(9) Uani 0.50 1 d PD
C1A C 0.0098(4) 0.6324(5) -0.1666(5) 0.054(4) Uani 0.50 1 d PD
C2A C 0.0400(4) 0.6800(5) -0.1625(6) 0.047(3) Uani 0.50 1 d PD
H2A1 H 0.0252 0.7153 -0.1742 0.070 Uiso 0.50 1 calc PR
H2A2 H 0.0596 0.6725 -0.1877 0.070 Uiso 0.50 1 calc PR
H2A3 H 0.0551 0.6835 -0.1227 0.070 Uiso 0.50 1 calc PR
N2A N 0.0615(4) 0.1333(5) 0.1094(6) 0.0593(9) Uani 0.50 1 d PD
C3A C 0.0577(4) 0.1768(5) 0.0813(6) 0.049(3) Uani 0.50 1 d PD
C4A C 0.0408(4) 0.2351(4) 0.0658(6) 0.049(3) Uani 0.50 1 d PD
H4A1 H 0.0542 0.2512 0.0361 0.074 Uiso 0.50 1 calc PR
H4A2 H 0.0463 0.2593 0.1001 0.074 Uiso 0.50 1 calc PR
H4A3 H 0.0110 0.2328 0.0513 0.074 Uiso 0.50 1 calc PR
N3A N 0.32303(18) 0.5369(3) 0.2034(3) 0.0593(9) Uani 1 1 d D
C5A C 0.3538(2) 0.5638(4) 0.2097(4) 0.071(3) Uani 1 1 d D
C6A C 0.3956(3) 0.5910(5) 0.2243(6) 0.108(4) Uani 1 1 d D
N4A N -0.06769(19) 0.2714(3) -0.0142(3) 0.0593(9) Uani 1 1 d D
C7A C -0.0953(2) 0.3003(4) -0.0386(4) 0.078(3) Uani 1 1 d D
C8A C -0.1291(2) 0.3389(4) -0.0662(4) 0.066(2) Uani 1 1 d D
N5A N 0.3330(4) 0.3689(6) 0.2038(7) 0.0593(9) Uani 0.50 1 d PD
C9A C 0.3570(5) 0.3769(7) 0.1737(7) 0.118(11) Uani 0.50 1 d PD
C10A C 0.3804(6) 0.4053(8) 0.1317(9) 0.087(6) Uani 0.50 1 d PD
H10A H 0.3770 0.3830 0.0963 0.131 Uiso 0.50 1 calc PR
H10B H 0.4098 0.4077 0.1493 0.131 Uiso 0.50 1 calc PR
H10C H 0.3694 0.4434 0.1227 0.131 Uiso 0.50 1 calc PR
N6A N -0.0661(4) 0.1817(5) 0.1150(5) 0.0593(9) Uani 0.50 1 d PD
C11A C -0.0701(4) 0.1506(5) 0.0743(5) 0.045(3) Uani 0.50 1 d PD
C12A C -0.0588(4) 0.1192(6) 0.0246(5) 0.050(4) Uani 0.50 1 d PD
H12A H -0.0830 0.0986 0.0040 0.075 Uiso 0.50 1 calc PR
H12B H -0.0365 0.0924 0.0389 0.075 Uiso 0.50 1 calc PR
H12C H -0.0495 0.1461 -0.0016 0.075 Uiso 0.50 1 calc PR
N7A N 0.3280(4) 0.3024(6) 0.4452(5) 0.0593(9) Uani 0.50 1 d PD
C13A C 0.3478(3) 0.3183(4) 0.4128(4) 0.0247(17) Uani 0.50 1 d PD
C14A C 0.3706(3) 0.3361(4) 0.3667(4) 0.0247(17) Uani 0.50 1 d PD
N8A N 0.5137(4) 0.2396(5) 0.1345(6) 0.0593(9) Uani 0.50 1 d PD
C15A C 0.4839(4) 0.2097(6) 0.1382(8) 0.082(6) Uani 0.50 1 d PD
C16A C 0.4640(4) 0.1635(7) 0.1671(8) 0.070(5) Uani 0.50 1 d PD
O1W O 0.0000 0.1512(9) 0.2500 0.054(5) Uani 0.50 2 d SP
C1W C 0.0106(11) 0.1734(15) 0.283(2) 0.061(11) Uani 0.25 1 d P
O2W O 0.4586(4) 0.2936(6) 0.2211(6) 0.085(4) Uani 0.50 1 d P
O2W' O 0.4191(5) 0.2602(9) 0.2173(7) 0.128(6) Uani 0.50 1 d P
O3W O 0.0000 0.5340(9) 0.2500 0.186(7) Uani 1 2 d S
O4W O 0.4216(4) 0.4280(6) 0.0253(6) 0.092(4) Uani 0.50 1 d P
O5W O 0.4582(4) 0.4922(6) 0.3835(7) 0.090(4) Uani 0.50 1 d P
O6W O 0.0139(7) -0.0097(15) 0.264(3) 0.31(2) Uani 0.50 1 d P
O7W O 0.4384(5) 0.4350(7) 0.3065(7) 0.105(5) Uani 0.50 1 d P
O8W O 0.5035(4) 0.3439(7) 0.0775(6) 0.094(4) Uani 0.50 1 d 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'
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'
S S 0.1246 0.1234 '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
O1 Ni1 N5 90.02(16) . .
O1 Ni1 O6 92.04(14) . .
N5 Ni1 O6 90.61(16) . .
O1 Ni1 O3 87.94(14) . .
N5 Ni1 O3 176.95(16) . .
O6 Ni1 O3 91.73(15) . .
O1 Ni1 N3 169.32(17) . .
N5 Ni1 N3 79.36(18) . .
O6 Ni1 N3 87.00(16) . .
O3 Ni1 N3 102.72(16) . .
O1 Ni1 O5 89.70(14) . .
N5 Ni1 O5 85.78(16) . .
O6 Ni1 O5 176.00(15) . .
O3 Ni1 O5 91.94(15) . .
N3 Ni1 O5 90.63(16) . .
N1 Ni2 N6 92.55(19) . .
N1 Ni2 N8 93.85(18) . .
N6 Ni2 N8 79.12(19) . .
N1 Ni2 O9 90.84(17) . .
N6 Ni2 O9 93.98(17) . .
N8 Ni2 O9 171.81(17) . .
N1 Ni2 O3 88.42(17) . .
N6 Ni2 O3 168.32(17) . .
N8 Ni2 O3 89.20(16) . .
O9 Ni2 O3 97.65(15) . .
N1 Ni2 N2 175.91(19) . .
N6 Ni2 N2 91.45(18) . .
N8 Ni2 N2 86.10(17) . .
O9 Ni2 N2 89.70(15) . .
O3 Ni2 N2 87.49(16) . .
O7 Ni3 N11 93.22(16) . .
O7 Ni3 O1 93.35(15) . .
N11 Ni3 O1 89.35(15) . .
O7 Ni3 O2 176.24(14) . .
N11 Ni3 O2 89.73(16) . .
O1 Ni3 O2 89.01(14) . .
O7 Ni3 N9 85.60(16) . .
N11 Ni3 N9 79.50(17) . .
O1 Ni3 N9 168.72(16) . .
O2 Ni3 N9 92.66(16) . .
O7 Ni3 O8 86.00(14) . .
N11 Ni3 O8 177.12(16) . .
O1 Ni3 O8 93.46(14) . .
O2 Ni3 O8 90.94(14) . .
N9 Ni3 O8 97.67(16) . .
O2 Ni4 N17 91.92(16) . .
O2 Ni4 N14 88.32(16) . .
N17 Ni4 N14 179.59(19) . .
O2 Ni4 N15 94.12(16) . .
N17 Ni4 N15 79.64(17) . .
N14 Ni4 N15 100.01(17) . .
O2 Ni4 N12 166.82(16) . .
N17 Ni4 N12 101.21(17) . .
N14 Ni4 N12 78.56(17) . .
N15 Ni4 N12 89.40(17) . .
O2 Ni4 N2 88.81(16) . .
N17 Ni4 N2 88.37(17) . .
N14 Ni4 N2 91.96(17) . .
N15 Ni4 N2 167.74(17) . .
N12 Ni4 N2 90.42(17) . .
O1 Ni5 N20 90.48(16) . .
O1 Ni5 O4 93.15(14) . .
N20 Ni5 O4 96.25(17) . .
O1 Ni5 N18 168.85(19) . .
N20 Ni5 N18 79.07(19) . .
O4 Ni5 N18 84.25(18) . .
O1 Ni5 O11 93.94(16) . .
N20 Ni5 O11 174.97(18) . .
O4 Ni5 O11 85.92(16) . .
N18 Ni5 O11 96.68(19) . .
O1 Ni5 O10 89.79(15) . .
N20 Ni5 O10 86.39(18) . .
O4 Ni5 O10 176.03(16) . .
N18 Ni5 O10 93.37(19) . .
O11 Ni5 O10 91.22(18) . .
Ni5 O1 Ni1 112.37(16) . .
Ni5 O1 Ni3 112.75(16) . .
Ni1 O1 Ni3 111.89(17) . .
Ni5 O1 H1O 105(3) . .
Ni1 O1 H1O 129.6(14) . .
Ni3 O1 H1O 81(3) . .
Ni4 O2 Ni3 115.77(17) . .
Ni4 O2 H2OA 98(2) . .
Ni3 O2 H2OA 126(2) . .
Ni4 O2 H2OB 103(3) . .
Ni3 O2 H2OB 108(3) . .
H2OA O2 H2OB 105.2(15) . .
Ni1 O3 Ni2 114.76(17) . .
Ni1 O3 H3O 102(3) . .
Ni2 O3 H3O 116(4) . .
N1 C1 S1 178.5(6) . .
C1 N1 Ni2 169.6(5) . .
N2 C2 S2 174.3(6) . .
C2 N2 Ni4 118.9(4) . .
C2 N2 Ni2 127.2(4) . .
Ni4 N2 Ni2 109.7(2) . .
N5 O4 Ni5 114.8(3) . .
N8 O5 Ni1 117.1(3) . .
N11 O6 Ni1 114.5(3) . .
N20 O7 Ni3 116.2(3) . .
N14 O8 Ni3 116.5(3) . .
N17 O9 Ni2 116.3(3) . .
Ni5 O10 H10O 100(3) . .
Ni5 O10 H10D 149(3) . .
H10O O10 H10D 110.0(15) . .
Ni5 O11 H11O 96(3) . .
Ni5 O11 H11A 148(2) . .
H11O O11 H11A 110.0(15) . .
C3 N3 C7 118.8(5) . .
C3 N3 Ni1 128.2(4) . .
C7 N3 Ni1 113.0(4) . .
O4 N5 C8 119.4(5) . .
O4 N5 Ni1 125.7(3) . .
C8 N5 Ni1 114.9(4) . .
C10 N6 C14 117.8(5) . .
C10 N6 Ni2 127.3(4) . .
C14 N6 Ni2 114.8(4) . .
C15 N8 O5 118.7(5) . .
C15 N8 Ni2 114.5(4) . .
O5 N8 Ni2 126.3(3) . .
C17 N9 C21 119.2(5) . .
C17 N9 Ni3 127.9(4) . .
C21 N9 Ni3 112.9(3) . .
C22 N11 O6 120.1(4) . .
C22 N11 Ni3 114.6(4) . .
O6 N11 Ni3 125.2(3) . .
C24 N12 C28 118.4(5) . .
C24 N12 Ni4 128.3(4) . .
C28 N12 Ni4 113.2(3) . .
O8 N14 C29 117.5(4) . .
O8 N14 Ni4 126.5(3) . .
C29 N14 Ni4 115.6(3) . .
C31 N15 C35 119.4(5) . .
C31 N15 Ni4 128.0(4) . .
C35 N15 Ni4 112.5(3) . .
C36 N17 O9 118.9(4) . .
C36 N17 Ni4 114.9(3) . .
O9 N17 Ni4 126.2(3) . .
C42 N18 C38 120.0(6) . .
C42 N18 Ni5 113.2(4) . .
C38 N18 Ni5 126.7(5) . .
C43 N20 O7 119.6(5) . .
C43 N20 Ni5 115.5(4) . .
O7 N20 Ni5 124.9(3) . .
N3 C3 C4 122.3(6) . .
N3 C3 H3 118.9 . .
C4 C3 H3 118.9 . .
C5 C4 C3 118.8(6) . .
C5 C4 H4 120.6 . .
C3 C4 H4 120.6 . .
C4 C5 C6 119.0(6) . .
C4 C5 H5 120.5 . .
C6 C5 H5 120.5 . .
C5 C6 C7 118.2(6) . .
C5 C6 H6 120.9 . .
C7 C6 H6 120.9 . .
N3 C7 C6 122.9(5) . .
N3 C7 C8 115.6(5) . .
C6 C7 C8 121.5(5) . .
N5 C8 C9 121.1(5) . .
N5 C8 C7 117.1(5) . .
C9 C8 C7 121.8(5) . .
N4 C9 C8 178.7(9) . .
N6 C10 C11 122.1(6) . .
N6 C10 H10 118.9 . .
C11 C10 H10 118.9 . .
C12 C11 C10 119.7(7) . .
C12 C11 H11 120.2 . .
C10 C11 H11 120.2 . .
C11 C12 C13 119.1(6) . .
C11 C12 H12 120.4 . .
C13 C12 H12 120.4 . .
C14 C13 C12 117.5(6) . .
C14 C13 H13 121.3 . .
C12 C13 H13 121.3 . .
N6 C14 C13 123.7(6) . .
N6 C14 C15 113.5(5) . .
C13 C14 C15 122.7(5) . .
N8 C15 C16 122.6(6) . .
N8 C15 C14 117.9(5) . .
C16 C15 C14 119.5(5) . .
N7 C16 C15 178.7(9) . .
N9 C17 C18 122.0(6) . .
N9 C17 H17 119.0 . .
C18 C17 H17 119.0 . .
C19 C18 C17 119.2(6) . .
C19 C18 H18 120.4 . .
C17 C18 H18 120.4 . .
C18 C19 C20 118.8(6) . .
C18 C19 H19 120.6 . .
C20 C19 H19 120.6 . .
C21 C20 C19 119.5(6) . .
C21 C20 H20 120.2 . .
C19 C20 H20 120.2 . .
N9 C21 C20 121.3(5) . .
N9 C21 C22 114.8(5) . .
C20 C21 C22 123.9(5) . .
N11 C22 C23 120.6(5) . .
N11 C22 C21 117.7(5) . .
C23 C22 C21 121.5(5) . .
N10 C23 C22 177.7(7) . .
N12 C24 C25 123.3(5) . .
N12 C24 H24 118.4 . .
C25 C24 H24 118.4 . .
C24 C25 C26 118.8(6) . .
C24 C25 H25 120.6 . .
C26 C25 H25 120.6 . .
C25 C26 C27 118.2(6) . .
C25 C26 H26 120.9 . .
C27 C26 H26 120.9 . .
C28 C27 C26 119.3(5) . .
C28 C27 H27 120.3 . .
C26 C27 H27 120.3 . .
N12 C28 C27 121.9(5) . .
N12 C28 C29 115.3(5) . .
C27 C28 C29 122.8(5) . .
N14 C29 C30 121.3(5) . .
N14 C29 C28 117.1(5) . .
C30 C29 C28 121.6(5) . .
N13 C30 C29 178.3(6) . .
N15 C31 C32 122.5(5) . .
N15 C31 H31 118.7 . .
C32 C31 H31 118.7 . .
C31 C32 C33 118.9(5) . .
C31 C32 H32 120.6 . .
C33 C32 H32 120.6 . .
C32 C33 C34 119.3(6) . .
C32 C33 H33 120.3 . .
C34 C33 H33 120.3 . .
C35 C34 C33 119.8(6) . .
C35 C34 H34 120.1 . .
C33 C34 H34 120.1 . .
C34 C35 N15 120.1(5) . .
C34 C35 C36 125.2(5) . .
N15 C35 C36 114.5(5) . .
N17 C36 C37 121.9(5) . .
N17 C36 C35 117.8(5) . .
C37 C36 C35 120.3(5) . .
N16 C37 C36 177.4(7) . .
N18 C38 C39 119.3(7) . .
N18 C38 H38 120.4 . .
C39 C38 H38 120.4 . .
C40 C39 C38 120.8(8) . .
C40 C39 H39 119.6 . .
C38 C39 H39 119.6 . .
C39 C40 C41 121.3(8) . .
C39 C40 H40 119.3 . .
C41 C40 H40 119.3 . .
C40 C41 C42 116.1(8) . .
C40 C41 H41 121.9 . .
C42 C41 H41 121.9 . .
N18 C42 C41 122.4(6) . .
N18 C42 C43 115.4(6) . .
C41 C42 C43 122.0(6) . .
N20 C43 C44 122.4(6) . .
N20 C43 C42 116.8(5) . .
C44 C43 C42 120.8(5) . .
N19 C44 C43 179.4(9) . .
N1A C1A C2A 175.0(15) . .
C1A C2A H2A1 109.5 . .
C1A C2A H2A2 109.5 . .
H2A1 C2A H2A2 109.5 . .
C1A C2A H2A3 109.5 . .
H2A1 C2A H2A3 109.5 . .
H2A2 C2A H2A3 109.5 . .
N2A C3A C4A 154.2(15) . .
C3A C4A H4A1 109.5 . .
C3A C4A H4A2 109.5 . .
H4A1 C4A H4A2 109.5 . .
C3A C4A H4A3 109.5 . .
H4A1 C4A H4A3 109.5 . .
H4A2 C4A H4A3 109.5 . .
N3A C5A C6A 171.2(12) . .
N4A C7A C8A 176.6(12) . .
N5A C9A C10A 161.4(19) . .
C9A C10A H10A 109.5 . .
C9A C10A H10B 109.5 . .
H10A C10A H10B 109.5 . .
C9A C10A H10C 109.5 . .
H10A C10A H10C 109.5 . .
H10B C10A H10C 109.5 . .
N6A C11A C12A 158.4(14) . .
C11A C12A H12A 109.5 . .
C11A C12A H12B 109.5 . .
H12A C12A H12B 109.5 . .
C11A C12A H12C 109.5 . .
H12A C12A H12C 109.5 . .
H12B C12A H12C 109.5 . .
N7A C13A C14A 174.7(12) . .
N8A C15A C16A 151.2(15) . .
C1W O1W C1W 113(6) 2 .
O1W C1W C1W 33(3) . 2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O1 2.036(3) .
Ni1 N5 2.040(4) .
Ni1 O6 2.067(4) .
Ni1 O3 2.075(4) .
Ni1 N3 2.092(4) .
Ni1 O5 2.106(4) .
Ni2 N1 2.018(5) .
Ni2 N6 2.063(5) .
Ni2 N8 2.066(5) .
Ni2 O9 2.070(4) .
Ni2 O3 2.096(4) .
Ni2 N2 2.122(4) .
Ni3 O7 2.047(4) .
Ni3 N11 2.048(4) .
Ni3 O1 2.052(3) .
Ni3 O2 2.055(4) .
Ni3 N9 2.066(4) .
Ni3 O8 2.069(4) .
Ni4 O2 2.027(4) .
Ni4 N17 2.039(4) .
Ni4 N14 2.053(4) .
Ni4 N15 2.076(4) .
Ni4 N12 2.105(4) .
Ni4 N2 2.107(4) .
Ni5 O1 2.032(4) .
Ni5 N20 2.048(5) .
Ni5 O4 2.050(4) .
Ni5 N18 2.061(5) .
Ni5 O11 2.076(4) .
Ni5 O10 2.103(4) .
O1 H1O 0.887(10) .
O2 H2OA 0.900(10) .
O2 H2OB 0.927(8) .
O3 H3O 0.896(10) .
S1 C1 1.633(6) .
C1 N1 1.164(7) .
S2 C2 1.596(8) .
C2 N2 1.262(9) .
O4 N5 1.294(6) .
O5 N8 1.323(6) .
O6 N11 1.314(5) .
O7 N20 1.320(6) .
O8 N14 1.306(5) .
O9 N17 1.310(6) .
O10 H10O 0.939(9) .
O10 H10D 0.899(8) .
O11 H11O 0.911(9) .
O11 H11A 0.918(9) .
N3 C3 1.323(7) .
N3 C7 1.336(7) .
N4 C9 1.156(9) .
N5 C8 1.311(7) .
N6 C10 1.327(8) .
N6 C14 1.334(7) .
N7 C16 1.143(9) .
N8 C15 1.275(7) .
N9 C17 1.336(7) .
N9 C21 1.355(7) .
N10 C23 1.133(8) .
N11 C22 1.285(7) .
N12 C24 1.337(7) .
N12 C28 1.349(7) .
N13 C30 1.132(7) .
N14 C29 1.307(7) .
N15 C31 1.331(7) .
N15 C35 1.385(7) .
N16 C37 1.156(8) .
N17 C36 1.309(7) .
N18 C42 1.335(8) .
N18 C38 1.356(8) .
N19 C44 1.135(9) .
N20 C43 1.268(7) .
C3 C4 1.407(8) .
C3 H3 0.9300 .
C4 C5 1.381(9) .
C4 H4 0.9300 .
C5 C6 1.386(9) .
C5 H5 0.9300 .
C6 C7 1.397(8) .
C6 H6 0.9300 .
C7 C8 1.464(8) .
C8 C9 1.401(9) .
C10 C11 1.398(9) .
C10 H10 0.9300 .
C11 C12 1.350(10) .
C11 H11 0.9300 .
C12 C13 1.399(9) .
C12 H12 0.9300 .
C13 C14 1.383(8) .
C13 H13 0.9300 .
C14 C15 1.498(8) .
C15 C16 1.420(9) .
C17 C18 1.392(8) .
C17 H17 0.9300 .
C18 C19 1.373(9) .
C18 H18 0.9300 .
C19 C20 1.394(9) .
C19 H19 0.9300 .
C20 C21 1.379(8) .
C20 H20 0.9300 .
C21 C22 1.462(7) .
C22 C23 1.451(9) .
C24 C25 1.364(8) .
C24 H24 0.9300 .
C25 C26 1.385(9) .
C25 H25 0.9300 .
C26 C27 1.403(8) .
C26 H26 0.9300 .
C27 C28 1.367(8) .
C27 H27 0.9300 .
C28 C29 1.458(8) .
C29 C30 1.421(7) .
C31 C32 1.383(8) .
C31 H31 0.9300 .
C32 C33 1.385(9) .
C32 H32 0.9300 .
C33 C34 1.388(8) .
C33 H33 0.9300 .
C34 C35 1.384(8) .
C34 H34 0.9300 .
C35 C36 1.448(7) .
C36 C37 1.414(8) .
C38 C39 1.390(10) .
C38 H38 0.9300 .
C39 C40 1.334(12) .
C39 H39 0.9300 .
C40 C41 1.387(11) .
C40 H40 0.9300 .
C41 C42 1.406(9) .
C41 H41 0.9300 .
C42 C43 1.470(9) .
C43 C44 1.434(9) .
N1A C1A 1.168(8) .
C1A C2A 1.467(8) .
C2A H2A1 0.9600 .
C2A H2A2 0.9600 .
C2A H2A3 0.9600 .
N2A C3A 1.195(8) .
C3A C4A 1.475(8) .
C4A H4A1 0.9600 .
C4A H4A2 0.9600 .
C4A H4A3 0.9600 .
N3A C5A 1.158(6) .
C5A C6A 1.471(7) .
N4A C7A 1.169(6) .
C7A C8A 1.461(7) .
N5A C9A 1.158(9) .
C9A C10A 1.500(8) .
C10A H10A 0.9600 .
C10A H10B 0.9600 .
C10A H10C 0.9600 .
N6A C11A 1.176(8) .
C11A C12A 1.472(8) .
C12A H12A 0.9600 .
C12A H12B 0.9600 .
C12A H12C 0.9600 .
N7A C13A 1.142(8) .
C13A C14A 1.476(8) .
N8A C15A 1.205(8) .
C15A C16A 1.478(9) .
O1W C1W 0.94(4) 2
O1W C1W 0.94(4) .
C1W C1W 1.56(9) 2
O2W O2W' 1.481(19) .
O6W O6W 1.00(5) 2
