#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/92/4329228.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_4329228
loop_
_publ_author_name
'Jordi Esteban'
'Laura Alcázar'
'Maria Torres-Molina'
'Montserrat Monfort'
'Mercè Font-Bardia'
'Albert Escuer'
_publ_section_title
;
 High Nuclearity in Azido/Oximate Chemistry: Ni14 and Ni13 Clusters with S
 = 6 and 9 Ground States
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5503
_journal_page_last               5505
_journal_paper_doi               10.1021/ic3004036
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety
'C88 H96 Cl2 N48 Ni14 O24, 7(C H4 O), 5.50(H2 O), 2(Cl)'
_chemical_formula_sum            'C95 H135 Cl4 N48 Ni14 O36.5'
_chemical_formula_weight         3497.25
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                108.409(5)
_cell_angle_beta                 92.219(5)
_cell_angle_gamma                115.014(4)
_cell_formula_units_Z            1
_cell_length_a                   16.2274(14)
_cell_length_b                   16.7091(16)
_cell_length_c                   19.2008(18)
_cell_measurement_reflns_used    9787
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.71
_cell_measurement_theta_min      2.28
_cell_volume                     4385.7(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP (Brueggermann and Smith, 1990)'
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(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         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            17249
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    1.596
_exptl_absorpt_correction_T_max  0.70
_exptl_absorpt_correction_T_min  0.53
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       prism
_exptl_crystal_F_000             1793
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.100
_refine_diff_density_min         -1.490
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1013
_refine_ls_number_reflns         17249
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0791P)²+8.5287P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1380
_refine_ls_wR_factor_ref         0.1601
_reflns_number_gt                12562
_reflns_number_total             17249
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3004036_si_002.cif
_cod_data_source_block           af40mtm1na
_cod_original_formula_sum        'C95 H135 Cl4 N48 Ni14 O36.50'
_cod_database_code               4329228
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ni4 Ni 0.02591(4) 0.14423(4) 0.45022(3) 0.01903(13) Uani 1 1 d .
Ni1 Ni -0.00229(4) 0.06484(4) 0.58559(3) 0.01999(14) Uani 1 1 d U
Ni3 Ni -0.13982(4) 0.21507(4) 0.45733(3) 0.02180(14) Uani 1 1 d .
Ni2 Ni -0.11909(4) 0.10014(4) 0.29681(3) 0.02312(14) Uani 1 1 d .
Ni5 Ni 0.21772(4) 0.31300(4) 0.42382(3) 0.02228(14) Uani 1 1 d .
Ni6 Ni -0.21839(4) -0.11844(4) 0.59253(3) 0.02319(14) Uani 1 1 d U
Ni7 Ni 0.07903(4) 0.26570(4) 0.25068(3) 0.02678(15) Uani 1 1 d .
Cl1 Cl -0.10318(9) 0.03856(9) 0.66996(7) 0.0352(3) Uani 1 1 d U
O1 O 0.07509(19) 0.0746(2) 0.49961(16) 0.0191(6) Uani 1 1 d .
O2 O -0.0414(2) 0.1958(2) 0.40093(17) 0.0220(7) Uani 1 1 d .
O3 O 0.1286(2) 0.1716(2) 0.39085(17) 0.0225(7) Uani 1 1 d .
O4 O 0.0845(2) 0.2038(2) 0.64916(18) 0.0288(7) Uani 1 1 d .
O5 O -0.06347(19) 0.1104(2) 0.51996(16) 0.0204(6) Uani 1 1 d .
O6 O -0.1215(2) 0.2089(2) 0.27028(18) 0.0290(7) Uani 1 1 d .
O7 O 0.0971(2) 0.2719(2) 0.53728(17) 0.0233(7) Uani 1 1 d .
O8 O -0.0528(2) 0.0073(2) 0.37869(16) 0.0209(6) Uani 1 1 d .
O9 O 0.2631(2) 0.2887(2) 0.32353(18) 0.0296(7) Uani 1 1 d .
O10 O -0.2779(2) -0.1379(3) 0.6814(2) 0.0346(8) Uani 1 1 d .
O11 O -0.1502(2) 0.2962(2) 0.39829(18) 0.0280(7) Uani 1 1 d .
O12 O -0.0267(2) 0.3373(2) 0.53715(18) 0.0264(7) Uani 1 1 d .
N1 N -0.2407(3) 0.2203(3) 0.5253(2) 0.0267(9) Uani 1 1 d .
N2 N -0.1238(2) 0.1463(2) 0.5246(2) 0.0200(8) Uani 1 1 d .
N3 N 0.1092(3) 0.3947(3) 0.2295(2) 0.0340(10) Uani 1 1 d .
N4 N -0.0450(3) 0.2703(3) 0.2550(2) 0.0298(9) Uani 1 1 d .
N5 N 0.3206(3) 0.4602(3) 0.4918(2) 0.0254(8) Uani 1 1 d .
N6 N 0.1747(2) 0.3356(3) 0.5236(2) 0.0225(8) Uani 1 1 d .
N7 N -0.2129(3) -0.0233(3) 0.1998(2) 0.0295(9) Uani 1 1 d .
N8 N -0.1067(2) -0.0076(3) 0.3159(2) 0.0222(8) Uani 1 1 d .
N9 N 0.0785(3) 0.1965(3) 0.1351(2) 0.0348(10) Uani 1 1 d .
N10 N 0.2025(3) 0.2589(3) 0.2599(2) 0.0288(9) Uani 1 1 d .
N11 N -0.3175(3) -0.0876(3) 0.5392(2) 0.0258(9) Uani 1 1 d .
N12 N -0.1663(2) -0.0956(2) 0.5035(2) 0.0191(8) Uani 1 1 d .
N13 N -0.2275(3) 0.0965(3) 0.3591(2) 0.0251(8) Uani 1 1 d U
N14 N -0.3048(3) 0.0693(3) 0.3382(2) 0.0336(9) Uani 1 1 d U
N15 N -0.3849(3) 0.0400(4) 0.3178(3) 0.0495(12) Uani 1 1 d .
N16 N -0.3083(3) -0.2667(3) 0.5332(2) 0.0245(8) Uani 1 1 d U
N17 N -0.3370(3) -0.2933(3) 0.4693(3) 0.0294(9) Uani 1 1 d U
N18 N -0.3671(3) -0.3198(3) 0.4065(3) 0.0419(11) Uani 1 1 d .
N19 N 0.1208(3) 0.3397(3) 0.3697(2) 0.0260(9) Uani 1 1 d .
N20 N 0.1415(3) 0.4238(3) 0.3905(2) 0.0252(9) Uani 1 1 d .
N21 N 0.1614(3) 0.5031(3) 0.4100(2) 0.0356(10) Uani 1 1 d .
N22 N 0.0037(3) 0.1270(3) 0.2533(2) 0.0269(9) Uani 1 1 d .
N23 N 0.0131(3) 0.0621(3) 0.2118(2) 0.0290(9) Uani 1 1 d .
N24 N 0.0225(3) -0.0003(3) 0.1721(3) 0.0395(11) Uani 1 1 d .
C1 C -0.2992(3) 0.2588(3) 0.5268(3) 0.0311(11) Uani 1 1 d .
C2 C -0.3422(3) 0.2745(4) 0.5880(3) 0.0342(12) Uani 1 1 d .
H2 H -0.3813 0.3023 0.5887 0.041 Uiso 1 1 calc R
C3 C -0.3275(4) 0.2492(4) 0.6472(3) 0.0363(12) Uani 1 1 d .
H3 H -0.3541 0.2618 0.6887 0.044 Uiso 1 1 calc R
C4 C -0.2724(3) 0.2048(4) 0.6434(3) 0.0323(11) Uani 1 1 d .
H4 H -0.2641 0.1833 0.6809 0.039 Uiso 1 1 calc R
C5 C -0.2293(3) 0.1926(3) 0.5825(3) 0.0276(10) Uani 1 1 d .
C6 C -0.1674(3) 0.1498(3) 0.5792(3) 0.0252(10) Uani 1 1 d .
H6 H -0.1594 0.1259 0.6152 0.030 Uiso 1 1 calc R
C7 C -0.3207(4) 0.2814(4) 0.4610(3) 0.0335(11) Uani 1 1 d .
H7A H -0.2955 0.2555 0.4205 0.050 Uiso 1 1 calc R
H7B H -0.2936 0.3490 0.4748 0.050 Uiso 1 1 calc R
H7C H -0.3867 0.2542 0.4455 0.050 Uiso 1 1 calc R
C8 C 0.1846(4) 0.4577(4) 0.2147(3) 0.0435(14) Uani 1 1 d .
C9 C 0.1860(4) 0.5362(4) 0.2021(3) 0.0462(14) Uani 1 1 d .
H9 H 0.2394 0.5788 0.1925 0.055 Uiso 1 1 calc R
C10 C 0.1094(4) 0.5507(4) 0.2038(3) 0.0488(15) Uani 1 1 d .
H10 H 0.1100 0.6025 0.1949 0.059 Uiso 1 1 calc R
C11 C 0.0313(4) 0.4878(4) 0.2187(3) 0.0410(13) Uani 1 1 d .
H11 H -0.0217 0.4965 0.2203 0.049 Uiso 1 1 calc R
C12 C 0.0327(4) 0.4109(4) 0.2313(3) 0.0345(12) Uani 1 1 d .
C13 C -0.0485(4) 0.3423(4) 0.2472(3) 0.0316(11) Uani 1 1 d .
H13 H -0.1016 0.3504 0.2515 0.038 Uiso 1 1 calc R
C14 C 0.2678(4) 0.4408(5) 0.2123(4) 0.0529(16) Uani 1 1 d .
H14A H 0.2677 0.4062 0.2438 0.079 Uiso 1 1 calc R
H14B H 0.3230 0.5007 0.2298 0.079 Uiso 1 1 calc R
H14C H 0.2663 0.4048 0.1617 0.079 Uiso 1 1 calc R
C15 C 0.3971(3) 0.5210(3) 0.4766(3) 0.0293(11) Uani 1 1 d .
C16 C 0.4663(3) 0.6015(4) 0.5344(3) 0.0372(13) Uani 1 1 d .
H16 H 0.5200 0.6415 0.5232 0.045 Uiso 1 1 calc R
C17 C 0.4546(4) 0.6207(4) 0.6068(3) 0.0362(12) Uani 1 1 d .
H17 H 0.5000 0.6737 0.6451 0.043 Uiso 1 1 calc R
C18 C 0.3741(3) 0.5603(3) 0.6226(3) 0.0328(11) Uani 1 1 d .
H18 H 0.3638 0.5728 0.6713 0.039 Uiso 1 1 calc R
C19 C 0.3095(3) 0.4808(3) 0.5638(3) 0.0262(10) Uani 1 1 d .
C20 C 0.2254(3) 0.4135(3) 0.5783(3) 0.0243(10) Uani 1 1 d .
H20 H 0.2094 0.4267 0.6252 0.029 Uiso 1 1 calc R
C21 C 0.4055(4) 0.5029(4) 0.3976(3) 0.0408(13) Uani 1 1 d .
H21A H 0.3522 0.4458 0.3660 0.061 Uiso 1 1 calc R
H21B H 0.4606 0.4959 0.3904 0.061 Uiso 1 1 calc R
H21C H 0.4091 0.5553 0.3849 0.061 Uiso 1 1 calc R
C22 C -0.2737(4) -0.0356(4) 0.1426(3) 0.0356(12) Uani 1 1 d .
C23 C -0.3242(4) -0.1222(4) 0.0841(3) 0.0437(14) Uani 1 1 d .
H23 H -0.3645 -0.1275 0.0453 0.052 Uiso 1 1 calc R
C25 C -0.2548(4) -0.1897(4) 0.1427(3) 0.0401(13) Uani 1 1 d .
H25 H -0.2476 -0.2417 0.1438 0.048 Uiso 1 1 calc R
C24 C -0.3147(4) -0.1985(4) 0.0837(3) 0.0469(14) Uani 1 1 d .
H24 H -0.3477 -0.2566 0.0443 0.056 Uiso 1 1 calc R
C26 C -0.2061(3) -0.1018(4) 0.1998(3) 0.0320(11) Uani 1 1 d .
C27 C -0.1450(3) -0.0899(3) 0.2647(3) 0.0263(10) Uani 1 1 d .
H27 H -0.1349 -0.1394 0.2681 0.032 Uiso 1 1 calc R
C28 C -0.2904(4) 0.0481(4) 0.1456(3) 0.0451(14) Uani 1 1 d .
H28A H -0.2479 0.1034 0.1873 0.068 Uiso 1 1 calc R
H28B H -0.3530 0.0341 0.1515 0.068 Uiso 1 1 calc R
H28C H -0.2810 0.0598 0.1000 0.068 Uiso 1 1 calc R
C29 C 0.0151(4) 0.1631(4) 0.0733(3) 0.0433(14) Uani 1 1 d .
C30 C 0.0288(4) 0.1192(5) 0.0022(3) 0.0500(15) Uani 1 1 d .
H30 H -0.0164 0.0963 -0.0402 0.060 Uiso 1 1 calc R
C31 C 0.1082(4) 0.1103(5) -0.0048(4) 0.0537(16) Uani 1 1 d .
H31 H 0.1179 0.0815 -0.0516 0.064 Uiso 1 1 calc R
C32 C 0.1748(4) 0.1460(4) 0.0604(3) 0.0489(15) Uani 1 1 d .
H32 H 0.2302 0.1423 0.0575 0.059 Uiso 1 1 calc R
C33 C 0.1572(4) 0.1863(4) 0.1286(3) 0.0338(12) Uani 1 1 d .
C34 C 0.2214(4) 0.2200(4) 0.1986(3) 0.0327(11) Uani 1 1 d .
H34 H 0.2754 0.2132 0.1984 0.039 Uiso 1 1 calc R
C35 C -0.0746(5) 0.1676(5) 0.0813(4) 0.0629(19) Uani 1 1 d .
H35A H -0.0929 0.1562 0.1256 0.094 Uiso 1 1 calc R
H35B H -0.1218 0.1202 0.0383 0.094 Uiso 1 1 calc R
H35C H -0.0665 0.2293 0.0852 0.094 Uiso 1 1 calc R
C36 C -0.3947(3) -0.0813(3) 0.5578(3) 0.0292(11) Uani 1 1 d .
C37 C -0.4567(3) -0.0801(4) 0.5064(3) 0.0350(12) Uani 1 1 d .
H37 H -0.5099 -0.0767 0.5199 0.042 Uiso 1 1 calc R
C38 C -0.4407(4) -0.0837(4) 0.4366(3) 0.0378(12) Uani 1 1 d .
H38 H -0.4827 -0.0834 0.4025 0.045 Uiso 1 1 calc R
C39 C -0.3617(3) -0.0879(3) 0.4176(3) 0.0292(11) Uani 1 1 d .
H39 H -0.3483 -0.0889 0.3708 0.035 Uiso 1 1 calc R
C40 C -0.3022(3) -0.0907(3) 0.4693(3) 0.0235(10) Uani 1 1 d .
C41 C -0.2143(3) -0.0881(3) 0.4537(3) 0.0238(10) Uani 1 1 d .
H41 H -0.1942 -0.0814 0.4103 0.029 Uiso 1 1 calc R
C42 C -0.4099(4) -0.0733(4) 0.6356(3) 0.0430(14) Uani 1 1 d .
H42A H -0.3608 -0.0761 0.6625 0.064 Uiso 1 1 calc R
H42B H -0.4683 -0.1246 0.6333 0.064 Uiso 1 1 calc R
H42C H -0.4103 -0.0139 0.6608 0.064 Uiso 1 1 calc R
C43 C -0.0997(4) 0.3984(4) 0.4236(3) 0.0356(12) Uani 1 1 d .
H43A H -0.1163 0.4194 0.3867 0.053 Uiso 1 1 calc R
H43B H -0.0342 0.4178 0.4310 0.053 Uiso 1 1 calc R
H43C H -0.1149 0.4261 0.4700 0.053 Uiso 1 1 calc R
C44 C -0.0276(3) 0.3849(3) 0.6139(3) 0.0289(11) Uani 1 1 d .
H44A H 0.0323 0.4381 0.6377 0.043 Uiso 1 1 calc R
H44B H -0.0420 0.3416 0.6399 0.043 Uiso 1 1 calc R
H44C H -0.0737 0.4069 0.6153 0.043 Uiso 1 1 calc R
Cl1W Cl 0.7822(2) 0.4453(2) 0.22913(17) 0.1180(9) Uani 1 1 d .
O2W O 0.0041(7) 0.2883(6) 0.7532(5) 0.054(2) Uani 0.50 1 d PD
C2W C 0.0678(11) 0.3399(13) 0.8245(7) 0.093(6) Uani 0.50 1 d PD
O3W O 0.4081(6) 0.3344(7) 0.1304(5) 0.064(3) Uani 0.50 1 d PD
C3W C 0.4674(8) 0.3978(9) 0.2047(6) 0.053(3) Uani 0.50 1 d PD
O4W O 0.6037(5) 0.2652(6) 0.2066(4) 0.0451(19) Uani 0.50 1 d PD
C4W C 0.6242(9) 0.2181(9) 0.2524(6) 0.049(3) Uani 0.50 1 d PD
O5W O 0.8012(13) 0.3102(16) 0.0792(7) 0.167(9) Uani 0.50 1 d P
O6W O 0.1987(4) 0.9877(4) 0.1846(3) 0.0224(13) Uani 0.50 1 d P
O7W O 0.1733(7) 0.8221(7) 0.2073(5) 0.062(2) Uani 0.50 1 d PD
C7W C 0.1874(16) 0.7606(13) 0.1393(9) 0.112(7) Uani 0.50 1 d PD
O8W O 0.4182(11) 0.6672(12) -0.0210(9) 0.124(5) Uani 0.50 1 d PD
C8W C 0.3600(19) 0.665(2) 0.0371(14) 0.169(12) Uani 0.50 1 d PD
O9W O 0.4142(9) 0.6996(10) 0.1869(7) 0.116(5) Uani 0.50 1 d PD
C9W C 0.4831(16) 0.666(2) 0.1969(15) 0.147(11) Uani 0.50 1 d PD
O10W O 0.3432(15) 0.7851(16) 0.1776(11) 0.077(6) Uani 0.25 1 d P
O11W O 0.4267(5) 0.1786(6) 0.1100(5) 0.051(2) Uani 0.50 1 d P
O12W O 0.2920(6) 0.0057(6) 0.0706(4) 0.049(2) Uani 0.50 1 d P
O13W O 0.6873(9) 0.6252(9) 0.2412(7) 0.110(4) Uani 0.50 1 d PD
C13W C 0.6945(12) 0.5614(13) 0.1716(8) 0.086(5) Uani 0.50 1 d PD
O14W O 0.249(3) 0.412(2) 1.0049(19) 0.071(12) Uani 0.13 1 d P
O15W O 0.408(3) 0.456(3) 1.0535(17) 0.063(11) Uani 0.13 1 d P
O16W O 0.4994(18) 0.0549(19) 0.0106(14) 0.032(6) Uani 0.13 1 d P
O17W O 0.130(3) 0.557(2) 1.0135(17) 0.053(9) Uani 0.13 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'
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
O2 Ni4 O3 94.00(12) . .
O2 Ni4 O5 96.04(12) . .
O3 Ni4 O5 169.89(12) . .
O2 Ni4 O8 93.92(12) . .
O3 Ni4 O8 94.77(12) . .
O5 Ni4 O8 85.71(12) . .
O2 Ni4 O7 92.02(12) . .
O3 Ni4 O7 93.61(12) . .
O5 Ni4 O7 84.89(12) . .
O8 Ni4 O7 169.36(12) . .
O2 Ni4 O1 171.16(12) . .
O3 Ni4 O1 92.69(11) . .
O5 Ni4 O1 77.44(11) . .
O8 Ni4 O1 79.77(12) . .
O7 Ni4 O1 93.31(12) . .
O8 Ni1 O4 103.70(13) 2_556 .
O8 Ni1 O5 163.84(12) 2_556 .
O4 Ni1 O5 88.66(12) . .
O8 Ni1 O1 93.57(11) 2_556 .
O4 Ni1 O1 90.27(12) . .
O5 Ni1 O1 75.74(11) . .
O8 Ni1 O1 78.36(12) 2_556 2_556
O4 Ni1 O1 167.16(12) . 2_556
O5 Ni1 O1 87.32(11) . 2_556
O1 Ni1 O1 76.92(12) . 2_556
O8 Ni1 Cl1 87.53(9) 2_556 .
O4 Ni1 Cl1 96.06(10) . .
O5 Ni1 Cl1 101.69(9) . .
O1 Ni1 Cl1 173.14(9) . .
O1 Ni1 Cl1 96.69(8) 2_556 .
O2 Ni3 N2 91.79(13) . .
O2 Ni3 O11 90.08(12) . .
N2 Ni3 O11 174.60(14) . .
O2 Ni3 O12 85.78(12) . .
N2 Ni3 O12 84.84(13) . .
O11 Ni3 O12 90.25(13) . .
O2 Ni3 N13 80.23(13) . .
N2 Ni3 N13 100.35(15) . .
O11 Ni3 N13 84.95(14) . .
O12 Ni3 N13 165.19(13) . .
O2 Ni3 N1 170.46(14) . .
N2 Ni3 N1 78.75(14) . .
O11 Ni3 N1 99.45(14) . .
O12 Ni3 N1 94.50(13) . .
N13 Ni3 N1 100.11(15) . .
N8 Ni2 O6 173.91(14) . .
N8 Ni2 O2 92.04(13) . .
O6 Ni2 O2 89.57(13) . .
N8 Ni2 N22 87.11(15) . .
O6 Ni2 N22 87.01(14) . .
O2 Ni2 N22 90.02(14) . .
N8 Ni2 N13 95.69(14) . .
O6 Ni2 N13 90.38(14) . .
O2 Ni2 N13 79.45(13) . .
N22 Ni2 N13 169.18(15) . .
N8 Ni2 N7 77.51(15) . .
O6 Ni2 N7 101.63(14) . .
O2 Ni2 N7 167.03(14) . .
N22 Ni2 N7 97.00(15) . .
N13 Ni2 N7 93.81(15) . .
N6 Ni5 O3 89.57(13) . .
N6 Ni5 O9 178.64(14) . .
O3 Ni5 O9 90.08(12) . .
N6 Ni5 N19 95.28(15) . .
O3 Ni5 N19 92.71(14) . .
O9 Ni5 N19 86.04(14) . .
N6 Ni5 N16 88.96(14) . 2_556
O3 Ni5 N16 80.66(13) . 2_556
O9 Ni5 N16 89.69(14) . 2_556
N19 Ni5 N16 172.13(15) . 2_556
N6 Ni5 N5 77.26(14) . .
O3 Ni5 N5 162.57(14) . .
O9 Ni5 N5 102.82(14) . .
N19 Ni5 N5 99.75(15) . .
N16 Ni5 N5 87.65(14) 2_556 .
N12 Ni6 O10 175.72(14) . .
N12 Ni6 O3 90.05(13) . 2_556
O10 Ni6 O3 94.22(13) . 2_556
N12 Ni6 N16 94.95(14) . .
O10 Ni6 N16 85.63(14) . .
O3 Ni6 N16 80.86(13) 2_556 .
N12 Ni6 N11 76.96(14) . .
O10 Ni6 N11 98.83(14) . .
O3 Ni6 N11 162.47(13) 2_556 .
N16 Ni6 N11 88.49(14) . .
N12 Ni6 Cl1 88.66(11) . .
O10 Ni6 Cl1 91.44(11) . .
O3 Ni6 Cl1 90.01(9) 2_556 .
N16 Ni6 Cl1 170.16(11) . .
N11 Ni6 Cl1 101.25(11) . .
N4 Ni7 N10 172.35(16) . .
N4 Ni7 N22 84.50(15) . .
N10 Ni7 N22 91.75(15) . .
N4 Ni7 N19 89.47(15) . .
N10 Ni7 N19 84.32(15) . .
N22 Ni7 N19 96.48(15) . .
N4 Ni7 N9 107.50(16) . .
N10 Ni7 N9 78.86(16) . .
N22 Ni7 N9 86.75(16) . .
N19 Ni7 N9 162.98(16) . .
N4 Ni7 N3 78.54(16) . .
N10 Ni7 N3 106.17(16) . .
N22 Ni7 N3 160.53(16) . .
N19 Ni7 N3 92.89(15) . .
N9 Ni7 N3 89.27(16) . .
Ni1 Cl1 Ni6 98.14(5) . .
N12 O1 Ni4 113.7(2) 2_556 .
N12 O1 Ni1 133.5(2) 2_556 .
Ni4 O1 Ni1 101.03(12) . .
N12 O1 Ni1 101.8(2) 2_556 2_556
Ni4 O1 Ni1 97.89(12) . 2_556
Ni1 O1 Ni1 103.08(12) . 2_556
Ni4 O2 Ni3 111.61(14) . .
Ni4 O2 Ni2 111.96(14) . .
Ni3 O2 Ni2 102.32(13) . .
Ni4 O3 Ni5 112.79(14) . .
Ni4 O3 Ni6 113.69(14) . 2_556
Ni5 O3 Ni6 101.20(13) . 2_556
N2 O5 Ni4 114.9(2) . .
N2 O5 Ni1 137.7(2) . .
Ni4 O5 Ni1 103.89(12) . .
N4 O6 Ni2 120.0(3) . .
N6 O7 Ni4 114.9(2) . .
N8 O8 Ni1 136.9(2) . 2_556
N8 O8 Ni4 117.6(2) . .
Ni1 O8 Ni4 103.15(13) 2_556 .
N10 O9 Ni5 118.2(3) . .
C43 O11 Ni3 125.0(3) . .
C44 O12 Ni3 126.3(3) . .
C1 N1 C5 117.9(4) . .
C1 N1 Ni3 131.3(3) . .
C5 N1 Ni3 109.8(3) . .
C6 N2 O5 120.1(4) . .
C6 N2 Ni3 115.4(3) . .
O5 N2 Ni3 123.9(3) . .
C8 N3 C12 116.8(5) . .
C8 N3 Ni7 133.2(4) . .
C12 N3 Ni7 110.0(3) . .
C13 N4 O6 116.3(4) . .
C13 N4 Ni7 116.7(3) . .
O6 N4 Ni7 126.9(3) . .
C15 N5 C19 118.2(4) . .
C15 N5 Ni5 131.0(3) . .
C19 N5 Ni5 109.6(3) . .
C20 N6 O7 117.0(4) . .
C20 N6 Ni5 118.3(3) . .
O7 N6 Ni5 124.6(3) . .
C22 N7 C26 116.8(4) . .
C22 N7 Ni2 133.0(4) . .
C26 N7 Ni2 110.2(3) . .
C27 N8 O8 119.1(4) . .
C27 N8 Ni2 118.8(3) . .
O8 N8 Ni2 121.8(3) . .
C29 N9 C33 118.8(5) . .
C29 N9 Ni7 130.7(4) . .
C33 N9 Ni7 110.5(3) . .
C34 N10 O9 117.4(4) . .
C34 N10 Ni7 115.5(3) . .
O9 N10 Ni7 127.0(3) . .
C36 N11 C40 117.6(4) . .
C36 N11 Ni6 132.2(3) . .
C40 N11 Ni6 109.3(3) . .
C41 N12 O1 119.0(3) . 2_556
C41 N12 Ni6 119.5(3) . .
O1 N12 Ni6 120.8(3) 2_556 .
N14 N13 Ni3 127.4(3) . .
N14 N13 Ni2 129.9(3) . .
Ni3 N13 Ni2 96.14(16) . .
N13 N14 N15 178.4(6) . .
N17 N16 Ni6 118.8(3) . .
N17 N16 Ni5 121.7(3) . 2_556
Ni6 N16 Ni5 94.60(15) . 2_556
N18 N17 N16 178.6(5) . .
N20 N19 Ni5 112.7(3) . .
N20 N19 Ni7 114.7(3) . .
Ni5 N19 Ni7 115.24(18) . .
N21 N20 N19 179.7(5) . .
N23 N22 Ni2 119.8(3) . .
N23 N22 Ni7 119.8(3) . .
Ni2 N22 Ni7 116.20(18) . .
N24 N23 N22 179.7(6) . .
N1 C1 C2 120.7(5) . .
N1 C1 C7 119.3(4) . .
C2 C1 C7 120.0(4) . .
C3 C2 C1 120.8(5) . .
C3 C2 H2 119.6 . .
C1 C2 H2 119.6 . .
C4 C3 C2 118.4(5) . .
C4 C3 H3 120.8 . .
C2 C3 H3 120.8 . .
C3 C4 C5 118.9(5) . .
C3 C4 H4 120.5 . .
C5 C4 H4 120.5 . .
N1 C5 C4 123.1(4) . .
N1 C5 C6 117.1(4) . .
C4 C5 C6 119.8(4) . .
N2 C6 C5 117.5(4) . .
N2 C6 H6 121.3 . .
C5 C6 H6 121.3 . .
C1 C7 H7A 109.5 . .
C1 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C1 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
N3 C8 C9 122.0(5) . .
N3 C8 C14 117.3(5) . .
C9 C8 C14 120.7(5) . .
C10 C9 C8 120.3(6) . .
C10 C9 H9 119.8 . .
C8 C9 H9 119.8 . .
C9 C10 C11 119.2(6) . .
C9 C10 H10 120.4 . .
C11 C10 H10 120.4 . .
C10 C11 C12 118.8(6) . .
C10 C11 H11 120.6 . .
C12 C11 H11 120.6 . .
N3 C12 C11 122.9(5) . .
N3 C12 C13 116.3(4) . .
C11 C12 C13 120.8(5) . .
N4 C13 C12 118.3(5) . .
N4 C13 H13 120.9 . .
C12 C13 H13 120.9 . .
C8 C14 H14A 109.5 . .
C8 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C8 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
N5 C15 C16 121.0(5) . .
N5 C15 C21 118.2(4) . .
C16 C15 C21 120.7(5) . .
C17 C16 C15 120.0(5) . .
C17 C16 H16 120.0 . .
C15 C16 H16 120.0 . .
C16 C17 C18 119.3(5) . .
C16 C17 H17 120.3 . .
C18 C17 H17 120.3 . .
C19 C18 C17 118.2(5) . .
C19 C18 H18 120.9 . .
C17 C18 H18 120.9 . .
N5 C19 C18 123.1(4) . .
N5 C19 C20 116.8(4) . .
C18 C19 C20 120.0(4) . .
N6 C20 C19 116.8(4) . .
N6 C20 H20 121.6 . .
C19 C20 H20 121.6 . .
C15 C21 H21A 109.5 . .
C15 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
C15 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
N7 C22 C23 122.6(5) . .
N7 C22 C28 117.8(5) . .
C23 C22 C28 119.5(5) . .
C24 C23 C22 120.0(5) . .
C24 C23 H23 120.0 . .
C22 C23 H23 120.0 . .
C26 C25 C24 118.5(5) . .
C26 C25 H25 120.7 . .
C24 C25 H25 120.7 . .
C23 C24 C25 119.3(6) . .
C23 C24 H24 120.4 . .
C25 C24 H24 120.4 . .
N7 C26 C25 122.7(5) . .
N7 C26 C27 116.7(4) . .
C25 C26 C27 120.5(5) . .
N8 C27 C26 116.0(4) . .
N8 C27 H27 122.0 . .
C26 C27 H27 122.0 . .
C22 C28 H28A 109.5 . .
C22 C28 H28B 109.5 . .
H28A C28 H28B 109.5 . .
C22 C28 H28C 109.5 . .
H28A C28 H28C 109.5 . .
H28B C28 H28C 109.5 . .
N9 C29 C30 121.3(5) . .
N9 C29 C35 118.5(5) . .
C30 C29 C35 120.1(5) . .
C31 C30 C29 120.2(6) . .
C31 C30 H30 119.9 . .
C29 C30 H30 119.9 . .
C30 C31 C32 118.3(6) . .
C30 C31 H31 120.9 . .
C32 C31 H31 120.9 . .
C33 C32 C31 119.2(6) . .
C33 C32 H32 120.4 . .
C31 C32 H32 120.4 . .
N9 C33 C32 122.1(5) . .
N9 C33 C34 116.0(4) . .
C32 C33 C34 121.8(5) . .
N10 C34 C33 119.0(5) . .
N10 C34 H34 120.5 . .
C33 C34 H34 120.5 . .
C29 C35 H35A 109.5 . .
C29 C35 H35B 109.5 . .
H35A C35 H35B 109.5 . .
C29 C35 H35C 109.5 . .
H35A C35 H35C 109.5 . .
H35B C35 H35C 109.5 . .
N11 C36 C37 120.6(5) . .
N11 C36 C42 118.0(4) . .
C37 C36 C42 121.4(4) . .
C38 C37 C36 121.1(5) . .
C38 C37 H37 119.4 . .
C36 C37 H37 119.4 . .
C37 C38 C39 118.9(5) . .
C37 C38 H38 120.6 . .
C39 C38 H38 120.6 . .
C38 C39 C40 118.8(5) . .
C38 C39 H39 120.6 . .
C40 C39 H39 120.6 . .
N11 C40 C39 123.1(4) . .
N11 C40 C41 116.0(4) . .
C39 C40 C41 120.7(4) . .
N12 C41 C40 115.9(4) . .
N12 C41 H41 122.0 . .
C40 C41 H41 122.0 . .
C36 C42 H42A 109.5 . .
C36 C42 H42B 109.5 . .
H42A C42 H42B 109.5 . .
C36 C42 H42C 109.5 . .
H42A C42 H42C 109.5 . .
H42B C42 H42C 109.5 . .
O11 C43 H43A 109.5 . .
O11 C43 H43B 109.5 . .
H43A C43 H43B 109.5 . .
O11 C43 H43C 109.5 . .
H43A C43 H43C 109.5 . .
H43B C43 H43C 109.5 . .
O12 C44 H44A 109.5 . .
O12 C44 H44B 109.5 . .
H44A C44 H44B 109.5 . .
O12 C44 H44C 109.5 . .
H44A C44 H44C 109.5 . .
H44B C44 H44C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni4 O2 2.015(3) .
Ni4 O3 2.030(3) .
Ni4 O5 2.037(3) .
Ni4 O8 2.040(3) .
Ni4 O7 2.048(3) .
Ni4 O1 2.077(3) .
Ni1 O8 2.027(3) 2_556
Ni1 O4 2.043(3) .
Ni1 O5 2.074(3) .
Ni1 O1 2.118(3) .
Ni1 O1 2.149(3) 2_556
Ni1 Cl1 2.3546(13) .
Ni3 O2 2.043(3) .
Ni3 N2 2.054(4) .
Ni3 O11 2.074(3) .
Ni3 O12 2.127(3) .
Ni3 N13 2.134(4) .
Ni3 N1 2.146(4) .
Ni2 N8 2.033(4) .
Ni2 O6 2.052(3) .
Ni2 O2 2.055(3) .
Ni2 N22 2.117(4) .
Ni2 N13 2.156(4) .
Ni2 N7 2.178(4) .
Ni5 N6 2.041(4) .
Ni5 O3 2.042(3) .
Ni5 O9 2.070(3) .
Ni5 N19 2.125(4) .
Ni5 N16 2.170(4) 2_556
Ni5 N5 2.207(4) .
Ni6 N12 2.009(3) .
Ni6 O10 2.040(3) .
Ni6 O3 2.061(3) 2_556
Ni6 N16 2.144(4) .
Ni6 N11 2.192(4) .
Ni6 Cl1 2.4003(14) .
Ni7 N4 2.050(4) .
Ni7 N10 2.058(4) .
Ni7 N22 2.134(4) .
Ni7 N19 2.144(4) .
Ni7 N9 2.152(4) .
Ni7 N3 2.175(4) .
O1 N12 1.378(4) 2_556
O1 Ni1 2.149(3) 2_556
O3 Ni6 2.061(3) 2_556
O5 N2 1.340(4) .
O6 N4 1.350(5) .
O7 N6 1.363(5) .
O8 N8 1.350(5) .
O8 Ni1 2.027(3) 2_556
O9 N10 1.347(5) .
O11 C43 1.445(6) .
O12 C44 1.441(5) .
N1 C1 1.351(6) .
N1 C5 1.354(6) .
N2 C6 1.288(6) .
N3 C8 1.346(7) .
N3 C12 1.377(7) .
N4 C13 1.282(6) .
N5 C15 1.345(6) .
N5 C19 1.354(6) .
N6 C20 1.281(6) .
N7 C22 1.351(6) .
N7 C26 1.361(7) .
N8 C27 1.273(6) .
N9 C29 1.334(7) .
N9 C33 1.364(6) .
N10 C34 1.271(6) .
N11 C36 1.354(6) .
N11 C40 1.362(6) .
N12 C41 1.278(6) .
N12 O1 1.378(4) 2_556
N13 N14 1.142(6) .
N14 N15 1.177(6) .
N16 N17 1.165(6) .
N16 Ni5 2.170(4) 2_556
N17 N18 1.150(6) .
N19 N20 1.218(5) .
N20 N21 1.146(6) .
N22 N23 1.199(6) .
N23 N24 1.154(6) .
C1 C2 1.399(7) .
C1 C7 1.496(7) .
C2 C3 1.377(8) .
C2 H2 0.9300 .
C3 C4 1.373(7) .
C3 H3 0.9300 .
C4 C5 1.389(7) .
C4 H4 0.9300 .
C5 C6 1.452(6) .
C6 H6 0.9300 .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C8 C9 1.398(8) .
C8 C14 1.491(8) .
C9 C10 1.362(8) .
C9 H9 0.9300 .
C10 C11 1.373(8) .
C10 H10 0.9300 .
C11 C12 1.390(8) .
C11 H11 0.9300 .
C12 C13 1.455(7) .
C13 H13 0.9300 .
C14 H14A 0.9600 .
C14 H14B 0.9600 .
C14 H14C 0.9600 .
C15 C16 1.408(7) .
C15 C21 1.475(7) .
C16 C17 1.364(8) .
C16 H16 0.9300 .
C17 C18 1.387(7) .
C17 H17 0.9300 .
C18 C19 1.386(7) .
C18 H18 0.9300 .
C19 C20 1.460(6) .
C20 H20 0.9300 .
C21 H21A 0.9600 .
C21 H21B 0.9600 .
C21 H21C 0.9600 .
C22 C23 1.388(8) .
C22 C28 1.518(8) .
C23 C24 1.345(8) .
C23 H23 0.9300 .
C25 C26 1.384(7) .
C25 C24 1.393(8) .
C25 H25 0.9300 .
C24 H24 0.9300 .
C26 C27 1.468(7) .
C27 H27 0.9300 .
C28 H28A 0.9600 .
C28 H28B 0.9600 .
C28 H28C 0.9600 .
C29 C30 1.407(8) .
C29 C35 1.500(8) .
C30 C31 1.364(8) .
C30 H30 0.9300 .
C31 C32 1.405(9) .
C31 H31 0.9300 .
C32 C33 1.373(8) .
C32 H32 0.9300 .
C33 C34 1.457(7) .
C34 H34 0.9300 .
C35 H35A 0.9600 .
C35 H35B 0.9600 .
C35 H35C 0.9600 .
C36 C37 1.394(7) .
C36 C42 1.495(7) .
C37 C38 1.361(8) .
C37 H37 0.9300 .
C38 C39 1.371(7) .
C38 H38 0.9300 .
C39 C40 1.383(7) .
C39 H39 0.9300 .
C40 C41 1.454(6) .
C41 H41 0.9300 .
C42 H42A 0.9600 .
C42 H42B 0.9600 .
C42 H42C 0.9600 .
C43 H43A 0.9600 .
C43 H43B 0.9600 .
C43 H43C 0.9600 .
C44 H44A 0.9600 .
C44 H44B 0.9600 .
C44 H44C 0.9600 .
O2W C2W 1.442(9) .
O3W C3W 1.470(9) .
O4W C4W 1.463(8) .
O7W C7W 1.478(10) .
O8W C8W 1.488(10) .
O9W C9W 1.485(10) .
O13W C13W 1.468(9) .
O16W O16W 1.76(6) 2_655
