#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:30:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179331 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/28/4322853.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_4322853
loop_
_publ_author_name
'Vasilis Tangoulis'
'Catherine P. Raptopoulou'
'Aris Terzis'
'Evangelos G. Bakalbassis'
'Eleanna Diamantopoulou'
'Spyros P. Perlepes'
_publ_section_title
;
 Polynuclear Nickel(II) Complexes: Preparation, Characterization, Magnetic
 Properties, and Quantum-Chemical Study of [Ni5(OH)(Rbta)5(acac)4(H2O)4]
 (RbtaH = Benzotriazole and 5,6-Dimethylbenzotriazole)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3142
_journal_page_last               3153
_journal_paper_doi               10.1021/ic9714091
_journal_volume                  37
_journal_year                    1998
_chemical_formula_analytical
'[Ni5(C6H4N3)5(C5H7O2)2(OH)(H2O)4].4(C3H6O).0.5(C6H14)'
_chemical_formula_structural
'[Ni(bta)5(acac)5(OH)(H2O)4].4(aceton).0.5(hexane)'
_chemical_formula_sum            'C65 H88 N15 Ni5 O17'
_chemical_formula_weight         1645.07
_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
_cell_angle_alpha                89.02(1)
_cell_angle_beta                 104.76(2)
_cell_angle_gamma                111.78(1)
_cell_formula_units_Z            2
_cell_length_a                   13.855(1)
_cell_length_b                   12.013(1)
_cell_length_c                   25.611(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      11.5
_cell_measurement_theta_min      5.5
_cell_volume                     3813.5(7)
_computing_cell_refinement
'Program LEAST (UCLA Crystallographic Package)'
_computing_data_collection
'Program COLLECT (UCLA Crystallographic Package)'
_computing_data_reduction
'Program REDUCE (UCLA Crystallographic Package)'
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  SHELXL-93
_computing_structure_solution    SHELXS-92
_diffrn_ambient_temperature      298
_diffrn_measurement_device       'P21 Nicolet'
_diffrn_measurement_method       theta-2theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0174
_diffrn_reflns_av_sigmaI/netI    0.0537
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            11263
_diffrn_reflns_theta_max         23.20
_diffrn_reflns_theta_min         1.63
_diffrn_standards_decay_%        -2.9
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.287
_exptl_absorpt_correction_T_max  1.28
_exptl_absorpt_correction_T_min  1.00
_exptl_absorpt_correction_type   'empirical psi-scan'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_meas      1.41
_exptl_crystal_density_method    'floating method'
_exptl_crystal_F_000             1718
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.779
_refine_diff_density_min         -0.986
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.542
_refine_ls_goodness_of_fit_obs   0.888
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1030
_refine_ls_number_reflns         10709
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.632
_refine_ls_restrained_S_obs      0.888
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_obs          0.0514
_refine_ls_shift/esd_max         0.098
_refine_ls_shift/esd_mean        0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0405P)²+37.0009P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2742
_refine_ls_wR_factor_obs         0.1297
_reflns_number_observed          7979
_reflns_number_total             10713
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9714091_1.cif
_cod_data_source_block           peed15
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+37.0009P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+37.0009P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3813.3(4)
_cod_database_code               4322853
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ni1 Ni 0.01595(10) 0.06474(11) 0.25738(5) 0.0268(7) Uani 1 d . .
Ni2 Ni 0.15902(11) 0.18482(12) 0.39731(6) 0.0322(7) Uani 1 d . .
Ni3 Ni 0.13483(11) 0.19256(12) 0.16473(6) 0.0307(7) Uani 1 d . .
Ni4 Ni -0.27201(11) -0.00018(13) 0.22704(6) 0.0364(7) Uani 1 d . .
Ni5 Ni 0.08527(11) -0.13808(12) 0.21102(6) 0.0336(8) Uani 1 d . .
O1 O 0.1682(6) 0.3336(7) 0.4375(3) 0.045(5) Uani 1 d . .
O2 O 0.3157(6) 0.2241(7) 0.4358(3) 0.044(4) Uani 1 d . .
O3 O 0.1761(7) 0.3380(7) 0.1238(3) 0.045(5) Uani 1 d . .
O4 O 0.2751(6) 0.1721(7) 0.1662(3) 0.044(4) Uani 1 d . .
O5 O -0.3851(6) -0.1018(8) 0.2636(3) 0.050(5) Uani 1 d . .
O6 O -0.3796(7) -0.0640(8) 0.1537(4) 0.053(5) Uani 1 d . .
O7 O 0.1037(7) -0.2951(7) 0.2190(4) 0.051(6) Uani 1 d . .
O8 O 0.0435(7) -0.1635(8) 0.1293(3) 0.050(6) Uani 1 d . .
O9 O -0.3298(7) 0.1440(8) 0.2312(4) 0.053(5) Uani 1 d . .
O10 O 0.1223(7) 0.0773(8) 0.4650(3) 0.048(5) Uani 1 d . .
O11 O 0.0662(7) 0.0773(8) 0.0891(3) 0.050(5) Uani 1 d . .
O12 O 0.2523(7) -0.0511(8) 0.2062(4) 0.053(5) Uani 1 d . .
N1 N -0.1630(7) 0.0669(8) 0.3044(4) 0.035(5) Uani 1 d . .
N2 N -0.0580(7) 0.0936(8) 0.3135(3) 0.029(5) Uani 1 d . .
N3 N -0.0044(7) 0.1399(8) 0.3651(4) 0.034(5) Uani 1 d . .
N11 N 0.1558(7) 0.0254(8) 0.3637(4) 0.034(5) Uani 1 d . .
N12 N 0.1103(7) -0.0087(7) 0.3110(4) 0.030(5) Uani 1 d . .
N13 N 0.1311(7) -0.0989(8) 0.2946(3) 0.031(5) Uani 1 d . .
N21 N -0.1688(7) 0.1227(8) 0.1862(4) 0.035(5) Uani 1 d . .
N22 N -0.0657(7) 0.1358(7) 0.1968(4) 0.031(5) Uani 1 d . .
N23 N -0.0163(7) 0.2000(8) 0.1621(4) 0.035(5) Uani 1 d . .
N31 N 0.1972(7) 0.2787(8) 0.2427(3) 0.030(5) Uani 1 d . .
N32 N 0.1464(7) 0.2260(7) 0.2803(3) 0.028(5) Uani 1 d . .
N33 N 0.1969(7) 0.2774(7) 0.3298(3) 0.030(5) Uani 1 d . .
N41 N -0.0771(7) -0.1906(8) 0.2144(4) 0.035(5) Uani 1 d . .
N42 N -0.1035(7) -0.1019(8) 0.2283(3) 0.030(5) Uani 1 d . .
N43 N -0.2085(7) -0.1340(8) 0.2229(3) 0.033(5) Uani 1 d . .
O O 0.0827(6) 0.0324(6) 0.1996(3) 0.037(5) Uani 1 d . .
C4 C -0.0711(11) 0.1868(12) 0.4410(5) 0.050(8) Uani 1 d . .
C5 C -0.1642(12) 0.1773(14) 0.4540(6) 0.062(10) Uani 1 d . .
C6 C -0.2649(12) 0.1275(15) 0.4153(6) 0.060(8) Uani 1 d . .
C7 C -0.2765(11) 0.0872(13) 0.3641(5) 0.052(7) Uani 1 d . .
C8 C -0.0807(9) 0.1451(10) 0.3888(4) 0.035(6) Uani 1 d . .
C9 C -0.1805(9) 0.0973(10) 0.3508(5) 0.040(7) Uani 1 d . .
C14 C 0.2370(11) -0.2182(12) 0.3447(6) 0.049(8) Uani 1 d . .
C15 C 0.2976(13) -0.2217(15) 0.3950(6) 0.062(10) Uani 1 d . .
C16 C 0.3148(12) -0.1421(14) 0.4385(6) 0.060(9) Uani 1 d . .
H16 H 0.3564(12) -0.1482(14) 0.4719(6) 0.071(44) Uiso 1 calc R .
C17 C 0.2719(10) -0.0551(13) 0.4334(6) 0.051(7) Uani 1 d . .
C18 C 0.1920(8) -0.1282(10) 0.3386(5) 0.038(6) Uani 1 d . .
C19 C 0.2097(8) -0.0491(10) 0.3830(4) 0.035(6) Uani 1 d . .
C24 C -0.0841(11) 0.3039(13) 0.0828(5) 0.051(8) Uani 1 d . .
C25 C -0.1763(14) 0.3188(16) 0.0554(6) 0.068(11) Uani 1 d . .
C26 C -0.2736(14) 0.2693(17) 0.0706(7) 0.071(11) Uani 1 d . .
C27 C -0.2802(11) 0.2030(13) 0.1137(5) 0.052(8) Uani 1 d . .
C28 C -0.0915(9) 0.2341(10) 0.1269(4) 0.033(6) Uani 1 d . .
C29 C -0.1873(9) 0.1845(11) 0.1423(5) 0.040(7) Uani 1 d . .
C34 C 0.3701(10) 0.4596(10) 0.3652(5) 0.044(7) Uani 1 d . .
C35 C 0.4521(12) 0.5413(13) 0.3461(6) 0.052(8) Uani 1 d . .
C36 C 0.4530(10) 0.5386(12) 0.2914(6) 0.052(7) Uani 1 d . .
C37 C 0.3723(10) 0.4557(11) 0.2537(5) 0.045(7) Uani 1 d . .
H37 H 0.3730(10) 0.4543(11) 0.2178(5) 0.010(26) Uiso 1 calc R .
C38 C 0.2884(8) 0.3729(10) 0.3256(4) 0.034(6) Uani 1 d . .
C39 C 0.2882(8) 0.3725(9) 0.2711(4) 0.033(6) Uani 1 d . .
C44 C -0.3613(10) -0.3372(12) 0.1946(6) 0.056(7) Uani 1 d . .
C45 C -0.3778(12) -0.4537(14) 0.1811(7) 0.072(9) Uani 1 d . .
C46 C -0.2945(12) -0.4915(13) 0.1779(7) 0.075(9) Uani 1 d . .
C47 C -0.1902(12) -0.4101(12) 0.1854(6) 0.058(9) Uani 1 d . .
C48 C -0.2540(9) -0.2547(10) 0.2055(5) 0.042(6) Uani 1 d . .
C49 C -0.1716(9) -0.2909(10) 0.2001(5) 0.040(6) Uani 1 d . .
C51 C 0.2410(11) 0.3918(11) 0.4784(5) 0.053(8) Uani 1 d . .
C52 C 0.3365(13) 0.3736(14) 0.5006(5) 0.056(9) Uani 1 d . .
C53 C 0.3695(10) 0.2939(11) 0.4780(5) 0.050(7) Uani 1 d . .
C54 C 0.2199(17) 0.4881(17) 0.5069(8) 0.094(14) Uani 1 d G .
H54A H 0.1951(64) 0.4952(90) 0.4930(26) 0.228(64) Uiso 1 calc G .
H54B H 0.1623(102) 0.4581(213) 0.5245(67) 0.228(64) Uiso 1 calc G .
H54C H 0.2853(110) 0.5319(193) 0.5425(53) 0.228(64) Uiso 1 calc G .
C55 C 0.4761(13) 0.2869(17) 0.5052(7) 0.083(10) Uani 1 d G .
H55A H 0.4966(78) 0.2716(108) 0.4820(27) 0.163(42) Uiso 1 calc G .
H55B H 0.4744(137) 0.2307(91) 0.5329(38) 0.163(42) Uiso 1 calc G .
H55C H 0.5295(109) 0.3511(118) 0.5449(38) 0.163(42) Uiso 1 calc G .
C56 C 0.2555(11) 0.3750(11) 0.1040(6) 0.054(9) Uani 1 d . .
C57 C 0.3347(11) 0.3265(12) 0.1101(5) 0.047(7) Uani 1 d . .
C58 C 0.3413(9) 0.2311(11) 0.1397(6) 0.048(6) Uani 1 d . .
C59 C 0.2669(20) 0.4855(22) 0.0737(11) 0.098(16) Uani 1 d G .
H59A H 0.2177(107) 0.5272(134) 0.0738(76) 0.070(48) Uiso 1 calc G .
H59B H 0.2499(108) 0.4589(160) 0.0470(36) 0.070(48) Uiso 1 calc G .
H59C H 0.3304(64) 0.5290(110) 0.0700(87) 0.070(48) Uiso 1 calc G .
C60 C 0.4334(12) 0.1901(16) 0.1413(7) 0.072(9) Uani 1 d G .
H60A H 0.4117(141) 0.1142(44) 0.1268(56) 0.173(51) Uiso 1 calc G .
H60B H 0.4689(90) 0.2092(121) 0.1717(17) 0.173(51) Uiso 1 calc G .
H60C H 0.4751(143) 0.2495(135) 0.1078(55) 0.173(51) Uiso 1 calc G .
C61 C -0.4864(10) -0.1404(11) 0.2410(7) 0.054(7) Uani 1 d . .
C62 C -0.5346(11) -0.1507(13) 0.1869(7) 0.062(7) Uani 1 d . .
C63 C -0.4815(10) -0.1155(12) 0.1450(6) 0.055(8) Uani 1 d . .
C64 C -0.5564(12) -0.1783(14) 0.2797(8) 0.074(9) Uani 1 d G .
H64A H -0.5461(130) -0.2520(86) 0.2960(69) 0.116(51) Uiso 1 calc G .
H64B H -0.6400(56) -0.2235(135) 0.2559(67) 0.116(51) Uiso 1 calc G .
H64C H -0.5438(94) -0.1241(61) 0.2948(45) 0.116(51) Uiso 1 calc G .
C65 C -0.5437(15) -0.1388(18) 0.0872(8) 0.093(11) Uani 1 d G .
H65A H -0.5196(108) -0.0650(67) 0.0697(56) 0.085(37) Uiso 1 calc G .
H65B H -0.6131(18) -0.1678(98) 0.0798(58) 0.085(37) Uiso 1 calc G .
H65C H -0.5248(110) -0.1989(84) 0.0728(57) 0.085(37) Uiso 1 calc G .
C66 C 0.1078(11) -0.3565(11) 0.1805(7) 0.058(9) Uani 1 d . .
C67 C 0.0810(16) -0.3398(16) 0.1261(6) 0.071(15) Uani 1 d . .
C68 C 0.0511(13) -0.2490(14) 0.1049(6) 0.064(11) Uani 1 d . .
C69 C 0.1476(18) -0.4553(15) 0.1971(9) 0.097(17) Uani 1 d G .
H69A H 0.1959(67) -0.4443(111) 0.2323(21) 0.083(31) Uiso 1 calc G .
H69B H 0.1450(81) -0.5124(59) 0.1805(37) 0.083(31) Uiso 1 calc G .
H69C H 0.0749(65) -0.5157(109) 0.2121(50) 0.083(31) Uiso 1 calc G .
C70 C 0.0213(28) -0.2460(26) 0.0436(8) 0.127(34) Uani 1 d G .
H70A H -0.0371(182) -0.2353(329) 0.0252(105) 0.331(103) Uiso 1 calc G .
H70B H 0.0377(178) -0.2889(151) 0.0378(84) 0.331(103) Uiso 1 calc G .
H70C H 0.0450(212) -0.2652(259) 0.0186(79) 0.331(103) Uiso 1 calc G .
O21 O 0.9141(9) 0.8605(11) 0.4368(4) 0.081(7) Uani 1 d . .
C71 C 0.8573(12) 0.8082(13) 0.3936(6) 0.060(9) Uani 1 d . .
C72 C 0.9069(17) 0.7723(19) 0.3550(7) 0.099(15) Uani 1 d . .
C73 C 0.7392(14) 0.7810(20) 0.3794(9) 0.107(11) Uani 1 d . .
O22 O 0.4949(9) 0.1183(11) 0.2743(5) 0.078(7) Uani 1 d . .
C74 C 0.4954(12) 0.1872(14) 0.3086(8) 0.070(9) Uani 1 d . .
C75 C 0.4113(17) 0.1451(20) 0.3384(10) 0.116(15) Uani 1 d . .
C76 C 0.5777(17) 0.3119(18) 0.3211(11) 0.116(13) Uani 1 d . .
O23 O 0.8202(13) 0.3545(14) 0.3004(9) 0.140(11) Uani 1 d . .
C77 C 0.9148(18) 0.4104(17) 0.3178(9) 0.093(14) Uani 1 d . .
C78 C 0.9572(31) 0.4725(26) 0.3741(10) 0.178(40) Uani 1 d . .
C79 C 0.9923(26) 0.4142(26) 0.2881(19) 0.200(28) Uani 1 d . .
O24 O 0.8326(16) 0.8808(19) -0.0025(6) 0.101(14) Uani 0.70 d P .
C80 C 0.7889(17) 0.9139(20) 0.0255(7) 0.061(13) Uani 0.70 d P .
C81 C 0.7946(19) 0.8826(24) 0.0812(8) 0.074(16) Uani 0.70 d P .
C82 C 0.7168(33) 0.9779(32) 0.0024(11) 0.127(38) Uani 0.70 d P .
C83 C 0.4873(63) 0.5419(73) -0.0112(31) 0.198(25) Uiso 0.50 d P .
C84 C 0.4015(45) 0.4455(53) -0.0402(22) 0.126(17) Uiso 0.50 d P .
C85 C 0.4951(50) 0.6189(61) -0.0002(25) 0.181(21) Uiso 0.50 d P .
HO H 0.0170(159) -0.0058(174) 0.1781(78) 0.065(68) Uiso 1 d . .
H4 H -0.0033(94) 0.2162(100) 0.4602(46) 0.017(31) Uiso 1 d . .
H5 H -0.1587(118) 0.2228(133) 0.4775(61) 0.135(46) Uiso 1 d . .
H6 H -0.3260(118) 0.1253(125) 0.4197(56) 0.047(43) Uiso 1 d . .
H7 H -0.3461(87) 0.0482(91) 0.3328(42) 0.039(27) Uiso 1 d . .
H14 H 0.2195(111) -0.2737(128) 0.3082(58) 0.067(43) Uiso 1 d . .
H15 H 0.3388(157) -0.2727(178) 0.4162(79) 0.072(70) Uiso 1 d . .
H17 H 0.2828(86) -0.0117(96) 0.4606(46) 0.105(29) Uiso 1 d . .
H24 H -0.0094(94) 0.3384(98) 0.0779(43) 0.027(30) Uiso 1 d . .
H25 H -0.1718(164) 0.3680(182) 0.0430(81) 0.038(76) Uiso 1 d . .
H26 H -0.3221(113) 0.2957(122) 0.0603(55) 0.040(42) Uiso 1 d . .
H27 H -0.3538(115) 0.1707(124) 0.1181(55) 0.046(42) Uiso 1 d . .
H34 H 0.3749(97) 0.4664(108) 0.4093(52) 0.062(35) Uiso 1 d . .
H35 H 0.5002(104) 0.5864(115) 0.3692(51) 0.054(39) Uiso 1 d . .
H36 H 0.5094(83) 0.5950(92) 0.2792(39) 0.020(25) Uiso 1 d . .
H44 H -0.4262(117) -0.3103(126) 0.1950(56) 0.083(43) Uiso 1 d . .
H45 H -0.4617(103) -0.5181(113) 0.1718(48) 0.079(35) Uiso 1 d . .
H46 H -0.2989(110) -0.5814(128) 0.1740(54) 0.192(42) Uiso 1 d . .
H47 H -0.1352(91) -0.4309(100) 0.1767(45) 0.074(31) Uiso 1 d . .
H52 H 0.3769(83) 0.4171(92) 0.5272(44) 0.030(28) Uiso 1 d . .
H57 H 0.3887(90) 0.3595(96) 0.0905(43) 0.028(29) Uiso 1 d . .
H62 H -0.6009(108) -0.1766(109) 0.1739(49) 0.052(35) Uiso 1 d . .
H67 H 0.0835(132) -0.3914(150) 0.0959(67) 0.129(56) Uiso 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'
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
O Ni1 N22 84.7(3) . . ?
O Ni1 N32 88.1(3) . . ?
N22 Ni1 N32 93.0(3) . . ?
O Ni1 N42 84.5(3) . . ?
N22 Ni1 N42 87.6(3) . . ?
N32 Ni1 N42 172.5(3) . . ?
O Ni1 N2 177.5(3) . . ?
N22 Ni1 N2 93.8(3) . . ?
N32 Ni1 N2 93.9(3) . . ?
N42 Ni1 N2 93.5(3) . . ?
O Ni1 N12 87.4(3) . . ?
N22 Ni1 N12 172.0(3) . . ?
N32 Ni1 N12 85.7(3) . . ?
N42 Ni1 N12 92.7(3) . . ?
N2 Ni1 N12 94.2(3) . . ?
O2 Ni2 O1 88.5(3) . . ?
O2 Ni2 N3 174.4(3) . . ?
O1 Ni2 N3 89.9(3) . . ?
O2 Ni2 N11 87.9(3) . . ?
O1 Ni2 N11 174.0(4) . . ?
N3 Ni2 N11 93.2(3) . . ?
O2 Ni2 N33 92.6(3) . . ?
O1 Ni2 N33 93.2(3) . . ?
N3 Ni2 N33 92.8(3) . . ?
N11 Ni2 N33 91.8(3) . . ?
O2 Ni2 O10 86.3(3) . . ?
O1 Ni2 O10 91.1(3) . . ?
N3 Ni2 O10 88.4(3) . . ?
N11 Ni2 O10 83.9(3) . . ?
N33 Ni2 O10 175.6(3) . . ?
O3 Ni3 O4 90.6(3) . . ?
O3 Ni3 O 174.1(3) . . ?
O4 Ni3 O 90.2(3) . . ?
O3 Ni3 N31 98.2(3) . . ?
O4 Ni3 N31 92.3(3) . . ?
O Ni3 N31 87.6(3) . . ?
O3 Ni3 N23 92.5(3) . . ?
O4 Ni3 N23 175.8(3) . . ?
O Ni3 N23 86.3(3) . . ?
N31 Ni3 N23 89.9(3) . . ?
O3 Ni3 O11 90.3(3) . . ?
O4 Ni3 O11 86.1(3) . . ?
O Ni3 O11 84.0(3) . . ?
N31 Ni3 O11 171.3(3) . . ?
N23 Ni3 O11 91.2(3) . . ?
O6 Ni4 O5 89.6(3) . . ?
O6 Ni4 N43 91.2(3) . . ?
O5 Ni4 N43 94.4(3) . . ?
O6 Ni4 N21 87.6(3) . . ?
O5 Ni4 N21 170.9(3) . . ?
N43 Ni4 N21 94.3(3) . . ?
O6 Ni4 N1 178.5(3) . . ?
O5 Ni4 N1 89.2(3) . . ?
N43 Ni4 N1 89.9(3) . . ?
N21 Ni4 N1 93.4(3) . . ?
O6 Ni4 O9 90.1(4) . . ?
O5 Ni4 O9 88.1(3) . . ?
N43 Ni4 O9 177.2(3) . . ?
N21 Ni4 O9 83.2(3) . . ?
N1 Ni4 O9 88.9(3) . . ?
O7 Ni5 O8 92.0(3) . . ?
O7 Ni5 O 173.2(3) . . ?
O8 Ni5 O 85.8(3) . . ?
O7 Ni5 N13 91.8(3) . . ?
O8 Ni5 N13 175.9(3) . . ?
O Ni5 N13 90.3(3) . . ?
O7 Ni5 N41 100.5(3) . . ?
O8 Ni5 N41 93.3(4) . . ?
O Ni5 N41 86.1(3) . . ?
N13 Ni5 N41 87.5(3) . . ?
O7 Ni5 O12 89.9(3) . . ?
O8 Ni5 O12 86.5(3) . . ?
O Ni5 O12 83.6(3) . . ?
N13 Ni5 O12 92.0(3) . . ?
N41 Ni5 O12 169.6(3) . . ?
C51 O1 Ni2 126.3(8) . . ?
C53 O2 Ni2 126.4(8) . . ?
C56 O3 Ni3 126.1(8) . . ?
C58 O4 Ni3 124.9(8) . . ?
C61 O5 Ni4 123.4(9) . . ?
C63 O6 Ni4 125.9(9) . . ?
C66 O7 Ni5 123.7(9) . . ?
C68 O8 Ni5 122.2(9) . . ?
N2 N1 C9 107.7(9) . . ?
N2 N1 Ni4 122.1(7) . . ?
C9 N1 Ni4 130.1(7) . . ?
N1 N2 N3 111.4(8) . . ?
N1 N2 Ni1 125.1(7) . . ?
N3 N2 Ni1 123.5(6) . . ?
N2 N3 C8 105.8(8) . . ?
N2 N3 Ni2 124.0(6) . . ?
C8 N3 Ni2 130.2(8) . . ?
N12 N11 C19 106.3(9) . . ?
N12 N11 Ni2 120.4(6) . . ?
C19 N11 Ni2 132.3(7) . . ?
N13 N12 N11 112.6(8) . . ?
N13 N12 Ni1 120.8(7) . . ?
N11 N12 Ni1 126.6(6) . . ?
N12 N13 C18 106.9(9) . . ?
N12 N13 Ni5 114.8(6) . . ?
C18 N13 Ni5 137.4(7) . . ?
N22 N21 C29 106.3(9) . . ?
N22 N21 Ni4 120.0(7) . . ?
C29 N21 Ni4 132.9(7) . . ?
N23 N22 N21 112.8(8) . . ?
N23 N22 Ni1 120.0(6) . . ?
N21 N22 Ni1 127.2(7) . . ?
N22 N23 C28 106.0(8) . . ?
N22 N23 Ni3 115.2(7) . . ?
C28 N23 Ni3 137.2(7) . . ?
N32 N31 C39 105.0(8) . . ?
N32 N31 Ni3 117.0(6) . . ?
C39 N31 Ni3 137.5(7) . . ?
N33 N32 N31 113.8(8) . . ?
N33 N32 Ni1 127.2(6) . . ?
N31 N32 Ni1 118.3(6) . . ?
N32 N33 C38 106.0(8) . . ?
N32 N33 Ni2 120.3(6) . . ?
C38 N33 Ni2 130.9(7) . . ?
N42 N41 C49 106.1(8) . . ?
N42 N41 Ni5 115.1(6) . . ?
C49 N41 Ni5 138.2(7) . . ?
N41 N42 N43 113.7(8) . . ?
N41 N42 Ni1 119.6(6) . . ?
N43 N42 Ni1 126.7(7) . . ?
N42 N43 C48 105.3(9) . . ?
N42 N43 Ni4 119.7(7) . . ?
C48 N43 Ni4 133.9(7) . . ?
Ni1 O Ni3 105.5(3) . . ?
Ni1 O Ni5 105.0(3) . . ?
Ni3 O Ni5 148.6(4) . . ?
C5 C4 C8 117.6(13) . . ?
C4 C5 C6 120.6(13) . . ?
C7 C6 C5 123.1(12) . . ?
C6 C7 C9 116.3(13) . . ?
N3 C8 C9 107.9(10) . . ?
N3 C8 C4 130.7(11) . . ?
C9 C8 C4 121.3(10) . . ?
N1 C9 C8 107.2(9) . . ?
N1 C9 C7 131.6(11) . . ?
C8 C9 C7 121.2(11) . . ?
C15 C14 C18 116.3(13) . . ?
C14 C15 C16 122.1(13) . . ?
C17 C16 C15 122.4(14) . . ?
C16 C17 C19 117.1(13) . . ?
N13 C18 C19 107.9(9) . . ?
N13 C18 C14 131.3(11) . . ?
C19 C18 C14 120.8(11) . . ?
N11 C19 C17 132.4(11) . . ?
N11 C19 C18 106.3(9) . . ?
C17 C19 C18 121.2(11) . . ?
C25 C24 C28 116.0(13) . . ?
C24 C25 C26 122.9(14) . . ?
C27 C26 C25 120.9(14) . . ?
C26 C27 C29 117.7(14) . . ?
N23 C28 C29 107.2(9) . . ?
N23 C28 C24 131.2(11) . . ?
C29 C28 C24 121.6(10) . . ?
N21 C29 C28 107.7(9) . . ?
N21 C29 C27 131.5(11) . . ?
C28 C29 C27 120.8(11) . . ?
C35 C34 C38 114.8(12) . . ?
C34 C35 C36 122.8(13) . . ?
C37 C36 C35 121.5(12) . . ?
C36 C37 C39 117.5(12) . . ?
N33 C38 C39 107.1(9) . . ?
N33 C38 C34 130.7(10) . . ?
C39 C38 C34 122.2(10) . . ?
N31 C39 C38 108.2(9) . . ?
N31 C39 C37 130.6(11) . . ?
C38 C39 C37 121.2(10) . . ?
C45 C44 C48 115.8(13) . . ?
C44 C45 C46 123.4(13) . . ?
C47 C46 C45 121.2(14) . . ?
C46 C47 C49 115.9(13) . . ?
N43 C48 C49 108.1(9) . . ?
N43 C48 C44 130.9(11) . . ?
C49 C48 C44 121.0(11) . . ?
N41 C49 C48 106.7(9) . . ?
N41 C49 C47 130.6(11) . . ?
C48 C49 C47 122.5(11) . . ?
O1 C51 C52 125.7(12) . . ?
O1 C51 C54 116.0(13) . . ?
C52 C51 C54 118.3(13) . . ?
C51 C52 C53 125.0(12) . . ?
O2 C53 C52 125.1(12) . . ?
O2 C53 C55 115.6(12) . . ?
C52 C53 C55 119.2(13) . . ?
O3 C56 C57 126.0(12) . . ?
O3 C56 C59 115.4(13) . . ?
C57 C56 C59 118.6(13) . . ?
C58 C57 C56 126.4(12) . . ?
O4 C58 C57 125.2(12) . . ?
O4 C58 C60 115.8(12) . . ?
C57 C58 C60 119.0(12) . . ?
O5 C61 C62 126.5(13) . . ?
O5 C61 C64 114.6(14) . . ?
C62 C61 C64 118.9(13) . . ?
C61 C62 C63 126.4(12) . . ?
O6 C63 C62 123.7(13) . . ?
O6 C63 C65 115.4(14) . . ?
C62 C63 C65 120.9(14) . . ?
O7 C66 C67 126.6(13) . . ?
O7 C66 C69 115.2(15) . . ?
C67 C66 C69 118.2(14) . . ?
C68 C67 C66 125.3(13) . . ?
O8 C68 C67 128.7(14) . . ?
O8 C68 C70 112.9(15) . . ?
C67 C68 C70 118.4(14) . . ?
O21 C71 C72 119.2(15) . . ?
O21 C71 C73 119.8(16) . . ?
C72 C71 C73 121.0(16) . . ?
O22 C74 C75 118.7(16) . . ?
O22 C74 C76 121.6(16) . . ?
C75 C74 C76 119.7(17) . . ?
O23 C77 C79 122.6(28) . . ?
O23 C77 C78 119.2(26) . . ?
C79 C77 C78 118.1(27) . . ?
O24 C80 C82 120.4(21) . . ?
O24 C80 C81 122.4(23) . . ?
C82 C80 C81 116.9(23) . . ?
C85 C83 C84 133.0(91) . . ?
C85 C83 C83 136.2(100) . 2_665 ?
C84 C83 C83 81.0(82) . 2_665 ?
C85 C83 C84 89.4(85) . 2_665 ?
C84 C83 C84 133.0(55) . 2_665 ?
C83 C83 C84 52.0(56) 2_665 2_665 ?
C83 C84 C83 47.0(55) . 2_665 ?
C83 C84 C85 74.0(49) . 2_665 ?
C83 C84 C85 28.6(29) 2_665 2_665 ?
C83 C85 C84 61.9(72) . 2_665 ?
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 O 2.044(7) . ?
Ni1 N22 2.047(9) . ?
Ni1 N32 2.065(8) . ?
Ni1 N42 2.065(9) . ?
Ni1 N2 2.065(8) . ?
Ni1 N12 2.066(9) . ?
Ni2 O2 2.018(8) . ?
Ni2 O1 2.024(8) . ?
Ni2 N3 2.063(9) . ?
Ni2 N11 2.094(9) . ?
Ni2 N33 2.112(8) . ?
Ni2 O10 2.194(8) . ?
Ni3 O3 1.995(8) . ?
Ni3 O4 2.039(8) . ?
Ni3 O 2.063(7) . ?
Ni3 N31 2.081(9) . ?
Ni3 N23 2.113(9) . ?
Ni3 O11 2.179(8) . ?
Ni4 O6 2.028(9) . ?
Ni4 O5 2.028(8) . ?
Ni4 N43 2.114(9) . ?
Ni4 N21 2.112(9) . ?
Ni4 N1 2.118(9) . ?
Ni4 O9 2.175(8) . ?
Ni5 O7 1.996(8) . ?
Ni5 O8 2.020(8) . ?
Ni5 O 2.076(7) . ?
Ni5 N13 2.081(9) . ?
Ni5 N41 2.124(9) . ?
Ni5 O12 2.194(8) . ?
O1 C51 1.252(15) . ?
O2 C53 1.260(15) . ?
O3 C56 1.255(14) . ?
O4 C58 1.273(14) . ?
O5 C61 1.277(15) . ?
O6 C63 1.274(15) . ?
O7 C66 1.267(16) . ?
O8 C68 1.262(16) . ?
N1 N2 1.325(12) . ?
N1 C9 1.354(14) . ?
N2 N3 1.351(12) . ?
N3 C8 1.368(13) . ?
N11 N12 1.335(12) . ?
N11 C19 1.376(13) . ?
N12 N13 1.320(12) . ?
N13 C18 1.352(14) . ?
N21 N22 1.333(12) . ?
N21 C29 1.358(14) . ?
N22 N23 1.322(12) . ?
N23 C28 1.375(13) . ?
N31 N32 1.348(11) . ?
N31 C39 1.377(14) . ?
N32 N33 1.318(11) . ?
N33 C38 1.387(13) . ?
N41 N42 1.328(12) . ?
N41 C49 1.379(14) . ?
N42 N43 1.330(12) . ?
N43 C48 1.378(14) . ?
C4 C5 1.377(18) . ?
C4 C8 1.392(17) . ?
C5 C6 1.408(21) . ?
C6 C7 1.355(19) . ?
C7 C9 1.417(16) . ?
C8 C9 1.390(16) . ?
C14 C15 1.356(20) . ?
C14 C18 1.424(16) . ?
C15 C16 1.394(21) . ?
C16 C17 1.371(19) . ?
C17 C19 1.375(17) . ?
C18 C19 1.406(16) . ?
C24 C25 1.366(20) . ?
C24 C28 1.399(16) . ?
C25 C26 1.410(23) . ?
C26 C27 1.351(21) . ?
C27 C29 1.404(16) . ?
C28 C29 1.394(16) . ?
C34 C35 1.390(18) . ?
C34 C38 1.403(16) . ?
C35 C36 1.406(20) . ?
C36 C37 1.352(17) . ?
C37 C39 1.394(16) . ?
C38 C39 1.396(15) . ?
C44 C45 1.367(20) . ?
C44 C48 1.405(16) . ?
C45 C46 1.408(22) . ?
C46 C47 1.378(19) . ?
C47 C49 1.398(17) . ?
C48 C49 1.400(16) . ?
C51 C52 1.397(20) . ?
C51 C54 1.532(20) . ?
C52 C53 1.391(20) . ?
C53 C55 1.497(19) . ?
C56 C57 1.397(19) . ?
C56 C59 1.504(20) . ?
C57 C58 1.383(18) . ?
C58 C60 1.521(18) . ?
C61 C62 1.361(21) . ?
C61 C64 1.510(19) . ?
C62 C63 1.423(21) . ?
C63 C65 1.482(21) . ?
C66 C67 1.377(21) . ?
C66 C69 1.498(20) . ?
C67 C68 1.363(22) . ?
C68 C70 1.520(25) . ?
O21 C71 1.205(16) . ?
C71 C72 1.489(23) . ?
C71 C73 1.490(23) . ?
O22 C74 1.214(19) . ?
C74 C75 1.483(22) . ?
C74 C76 1.486(24) . ?
O23 C77 1.195(22) . ?
C77 C79 1.453(33) . ?
C77 C78 1.504(31) . ?
O24 C80 1.204(26) . ?
C80 C82 1.480(38) . ?
C80 C81 1.461(27) . ?
C83 C85 0.929(85) . ?
C83 C84 1.366(85) . ?
C83 C83 1.268(131) 2_665 ?
C83 C84 1.712(92) 2_665 ?
C84 C83 1.712(92) 2_665 ?
C84 C85 1.940(81) 2_665 ?
C85 C84 1.940(81) 2_665 ?
