#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:32:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179115 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/77/4307763.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_4307763
loop_
_publ_author_name
'Theocharis C. Stamatatos'
'Eleanna Diamantopoulou'
'Catherine P. Raptopoulou'
'Vassilis Psycharis'
'Albert Escuer'
'Spyros P. Perlepes'
_publ_section_title
;
Acetate/Di-2-pyridyl Ketone Oximate "Blend" as a Source of
High-Nuclearity Nickel(II) Clusters: Dependence of the Nuclearity on the
Nature of the Inorganic Anion Present
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2350
_journal_page_last               2352
_journal_paper_doi               10.1021/ic062262t
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C82 H100.4 N26 Ni7 O32.2'
_chemical_formula_weight         2376.46
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ya'
_symmetry_space_group_name_H-M   'P 1 2/a 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                 96.393(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   21.475(9)
_cell_length_b                   21.955(9)
_cell_length_c                   11.352(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      11.7
_cell_measurement_theta_min      5.4
_cell_volume                     5319(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Crystal Logic Dual Goniometer'
_diffrn_measurement_method       θ/2θ
_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  0.0204
_diffrn_reflns_av_sigmaI/netI    0.0601
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8547
_diffrn_reflns_theta_full        23.75
_diffrn_reflns_theta_max         23.75
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        -0.6
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.299
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   'psi-scan empirical'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parall
_exptl_crystal_F_000             2456
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     773
_refine_ls_number_reflns         8087
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0476P)²+8.1249P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1150
_refine_ls_wR_factor_ref         0.1307
_reflns_number_gt                6028
_reflns_number_total             8087
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062262tsi20061128_095127.cif
_cod_data_source_block           ped435c
_cod_database_code               4307763
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y, z'
'-x, -y, -z'
'-x-1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.2500 0.21046(4) 0.0000 0.0317(2) Uani 1 2 d S . .
Ni2 Ni 0.13822(3) 0.14450(3) 0.18504(5) 0.03111(16) Uani 1 1 d . . .
Ni3 Ni -0.05017(3) 0.22446(3) 0.02829(6) 0.03479(17) Uani 1 1 d . . .
Ni4 Ni 0.07331(3) 0.28045(3) 0.20538(6) 0.03440(17) Uani 1 1 d . . .
O1 O 0.18463(14) 0.21642(13) 0.1214(3) 0.0344(7) Uani 1 1 d . . .
N1 N 0.20360(18) 0.27521(17) -0.1081(4) 0.0357(9) Uani 1 1 d . . .
N2 N 0.16038(17) 0.27139(16) 0.1433(3) 0.0316(9) Uani 1 1 d . . .
N3 N 0.10497(19) 0.36962(18) 0.2066(4) 0.0416(10) Uani 1 1 d . . .
O11 O 0.05744(13) 0.18972(14) 0.1987(3) 0.0324(7) Uani 1 1 d . . .
N11 N 0.08870(18) 0.07159(17) 0.2455(4) 0.0356(9) Uani 1 1 d . . .
N12 N 0.00628(17) 0.16836(17) 0.1309(4) 0.0321(9) Uani 1 1 d . . .
N13 N -0.10155(18) 0.14294(19) 0.0220(4) 0.0415(10) Uani 1 1 d . . .
O21 O 0.01701(17) 0.15740(18) -0.1489(4) 0.0554(10) Uani 1 1 d . . .
N21 N -0.11278(18) 0.27377(18) -0.0824(4) 0.0396(10) Uani 1 1 d . . .
N22 N -0.02543(19) 0.19795(19) -0.1337(4) 0.0410(10) Uani 1 1 d . . .
O31 O 0.20624(15) 0.14332(15) -0.1049(3) 0.0396(8) Uani 1 1 d . . .
O32 O 0.21820(14) 0.09466(15) 0.1882(3) 0.0405(8) Uani 1 1 d . . .
O33 O 0.16555(15) 0.17110(15) 0.3603(3) 0.0404(8) Uani 1 1 d . . .
O34 O 0.12101(16) 0.26303(16) 0.3720(3) 0.0461(9) Uani 1 1 d . . .
O35 O -0.08717(16) 0.25812(17) 0.1774(3) 0.0458(9) Uani 1 1 d . . .
O36 O -0.00600(16) 0.30164(16) 0.2863(3) 0.0465(9) Uani 1 1 d . . .
N31 N 0.01930(18) 0.29285(18) 0.0418(4) 0.0380(9) Uani 1 1 d . . .
OW1 O 0.1074(2) 0.11875(17) 0.0115(4) 0.0375(8) Uani 1 1 d . . .
C1 C 0.1404(2) 0.2731(2) -0.1285(5) 0.0413(12) Uani 1 1 d . . .
C2 C 0.1056(3) 0.3122(3) -0.2016(5) 0.0498(14) Uani 1 1 d . . .
C3 C 0.1359(3) 0.3565(3) -0.2597(6) 0.0541(15) Uani 1 1 d . . .
C4 C 0.2004(3) 0.3592(3) -0.2419(6) 0.0492(14) Uani 1 1 d . . .
C5 C 0.2336(2) 0.3183(2) -0.1658(4) 0.0358(11) Uani 1 1 d . . .
C6 C 0.1969(2) 0.3184(2) 0.1533(4) 0.0351(11) Uani 1 1 d . . .
C7 C 0.1618(2) 0.3763(2) 0.1686(5) 0.0416(12) Uani 1 1 d . . .
C8 C 0.1846(3) 0.4333(3) 0.1428(6) 0.0570(16) Uani 1 1 d . . .
C9 C 0.1485(3) 0.4840(3) 0.1577(8) 0.073(2) Uani 1 1 d . . .
C10 C 0.0917(3) 0.4775(3) 0.1999(8) 0.073(2) Uani 1 1 d . . .
C11 C 0.0710(3) 0.4195(2) 0.2219(6) 0.0556(16) Uani 1 1 d . . .
C21 C 0.1184(3) 0.0315(3) 0.3198(6) 0.0508(15) Uani 1 1 d . . .
C22 C 0.0891(3) -0.0146(3) 0.3740(7) 0.0679(19) Uani 1 1 d . . .
C23 C 0.0251(3) -0.0190(3) 0.3520(7) 0.069(2) Uani 1 1 d . . .
C24 C -0.0070(3) 0.0221(3) 0.2759(6) 0.0514(14) Uani 1 1 d . . .
C25 C 0.0254(2) 0.0667(2) 0.2220(5) 0.0360(11) Uani 1 1 d . . .
C26 C -0.0081(2) 0.1113(2) 0.1400(4) 0.0327(10) Uani 1 1 d . . .
C27 C -0.0662(2) 0.0948(2) 0.0633(4) 0.0358(11) Uani 1 1 d . . .
C28 C -0.0835(3) 0.0358(2) 0.0300(5) 0.0436(13) Uani 1 1 d . . .
C29 C -0.1393(3) 0.0257(3) -0.0402(5) 0.0506(14) Uani 1 1 d . . .
C30 C -0.1759(3) 0.0747(3) -0.0781(6) 0.0580(16) Uani 1 1 d . . .
C31 C -0.1551(2) 0.1325(3) -0.0459(6) 0.0531(15) Uani 1 1 d . . .
C41 C -0.1543(3) 0.3153(3) -0.0509(6) 0.0507(14) Uani 1 1 d . . .
C42 C -0.1919(3) 0.3490(3) -0.1317(7) 0.0626(17) Uani 1 1 d . . .
C43 C -0.1866(4) 0.3413(3) -0.2484(8) 0.077(2) Uani 1 1 d . . .
C44 C -0.1448(4) 0.2989(3) -0.2820(7) 0.071(2) Uani 1 1 d . . .
C45 C -0.1079(3) 0.2654(2) -0.1988(5) 0.0479(13) Uani 1 1 d . . .
C46 C -0.0615(2) 0.2196(2) -0.2275(5) 0.0436(12) Uani 1 1 d . . .
C47 C -0.0581(3) 0.1980(3) -0.3491(5) 0.0494(13) Uani 1 1 d . . .
C48 C -0.0029(3) 0.1932(3) -0.3992(6) 0.0654(18) Uani 1 1 d . . .
C49 C -0.0039(4) 0.1742(4) -0.5157(7) 0.076(2) Uani 1 1 d . . .
C50 C -0.0598(4) 0.1592(3) -0.5770(6) 0.0684(19) Uani 1 1 d . . .
C51 C -0.1132(4) 0.1636(3) -0.5215(6) 0.0650(18) Uani 1 1 d . . .
N23 N -0.1131(2) 0.1828(2) -0.4103(4) 0.0581(13) Uani 1 1 d . . .
C61 C 0.2739(2) 0.1030(2) 0.1708(4) 0.0361(11) Uani 1 1 d . . .
C62 C 0.3222(3) 0.0611(3) 0.2339(6) 0.0596(16) Uani 1 1 d . . .
H62A H 0.3183 0.0615 0.3173 0.077 Uiso 1 1 calc R . .
H62B H 0.3633 0.0746 0.2206 0.077 Uiso 1 1 calc R . .
H62C H 0.3156 0.0204 0.2039 0.077 Uiso 1 1 calc R . .
C63 C 0.1513(2) 0.2174(2) 0.4157(5) 0.0407(12) Uani 1 1 d . . .
C64 C 0.1709(3) 0.2192(3) 0.5476(5) 0.0639(17) Uani 1 1 d . . .
H64A H 0.1867 0.1800 0.5737 0.083 Uiso 1 1 calc R . .
H64B H 0.1354 0.2293 0.5882 0.083 Uiso 1 1 calc R . .
H64C H 0.2030 0.2493 0.5648 0.083 Uiso 1 1 calc R . .
C65 C -0.0633(3) 0.2901(2) 0.2615(5) 0.0454(13) Uani 1 1 d . . .
C66 C -0.1073(3) 0.3182(3) 0.3425(7) 0.073(2) Uani 1 1 d . . .
H66A H -0.0856 0.3233 0.4204 0.095 Uiso 1 1 calc R . .
H66B H -0.1427 0.2918 0.3465 0.095 Uiso 1 1 calc R . .
H66C H -0.1215 0.3571 0.3116 0.095 Uiso 1 1 calc R . .
N32 N 0.0074(2) 0.3416(2) -0.0030(4) 0.0467(11) Uani 1 1 d . . .
N33 N -0.0042(3) 0.3871(3) -0.0481(6) 0.087(2) Uani 1 1 d . . .
N41 N 0.1963(4) 0.5350(4) 0.8475(12) 0.166(5) Uani 1 1 d . . .
C71 C 0.1468(4) 0.5245(4) 0.8517(9) 0.094(3) Uani 1 1 d . . .
C72 C 0.0817(4) 0.5080(5) 0.8556(11) 0.129(4) Uani 1 1 d . . .
H72A H 0.0793 0.4684 0.8905 0.168 Uiso 1 1 calc R . .
H72B H 0.0605 0.5075 0.7766 0.168 Uiso 1 1 calc R . .
H72C H 0.0621 0.5374 0.9023 0.168 Uiso 1 1 calc R . .
OW2 O 0.2500 0.0858(3) 0.5000 0.0691(17) Uani 1 2 d S . .
OW3 O 0.2500 0.9556(4) 0.5000 0.141(4) Uani 1 2 d S . .
OW4 O 0.2327(3) 0.8551(4) 0.3402(7) 0.149(3) Uani 1 1 d . . .
OW5 O 0.2143(3) 0.7892(3) 0.8372(8) 0.143(3) Uani 1 1 d . . .
OW6 O 0.0424(4) 0.3529(4) 0.4983(7) 0.170(4) Uani 1 1 d . . .
OW7 O 0.1858(6) 0.3786(6) 0.4576(10) 0.252(6) Uani 1 1 d . . .
OW8 O 0.5210(9) 0.4097(9) 0.3464(18) 0.180(7) Uiso 0.50 1 d P . .
OW9 O 0.6598(16) 0.4764(16) 0.516(3) 0.272(16) Uiso 0.40 1 d P . .
OW10 O 0.7500 0.450(3) 0.5000 0.32(3) Uiso 0.40 2 d SP . .
H1 H 0.122(2) 0.242(2) -0.084(4) 0.026(11) Uiso 1 1 d . . .
H2 H 0.062(3) 0.309(3) -0.211(5) 0.063(18) Uiso 1 1 d . . .
H3 H 0.113(3) 0.380(2) -0.311(5) 0.049(16) Uiso 1 1 d . . .
H4 H 0.227(3) 0.382(3) -0.286(6) 0.07(2) Uiso 1 1 d . . .
H8 H 0.223(3) 0.435(2) 0.109(5) 0.049(15) Uiso 1 1 d . . .
H9 H 0.170(3) 0.525(3) 0.159(6) 0.08(2) Uiso 1 1 d . . .
H10 H 0.068(3) 0.509(3) 0.206(6) 0.069(19) Uiso 1 1 d . . .
H11 H 0.030(3) 0.413(2) 0.255(5) 0.054(16) Uiso 1 1 d . . .
H21 H 0.156(2) 0.0343(19) 0.322(4) 0.021(12) Uiso 1 1 d . . .
H22 H 0.111(3) -0.040(3) 0.427(5) 0.055(17) Uiso 1 1 d . . .
H23 H 0.006(3) -0.046(3) 0.390(6) 0.08(2) Uiso 1 1 d . . .
H24 H -0.054(2) 0.022(2) 0.265(4) 0.034(13) Uiso 1 1 d . . .
H28 H -0.059(2) 0.011(2) 0.055(4) 0.031(14) Uiso 1 1 d . . .
H29 H -0.148(2) -0.014(3) -0.067(5) 0.048(15) Uiso 1 1 d . . .
H30 H -0.213(3) 0.071(3) -0.131(6) 0.061(18) Uiso 1 1 d . . .
H31 H -0.176(2) 0.172(2) -0.076(4) 0.030(12) Uiso 1 1 d . . .
H41 H -0.151(2) 0.323(2) 0.038(5) 0.037(13) Uiso 1 1 d . . .
H42 H -0.219(2) 0.378(2) -0.109(5) 0.041(14) Uiso 1 1 d . . .
H43 H -0.209(4) 0.359(4) -0.307(7) 0.10(3) Uiso 1 1 d . . .
H44 H -0.142(4) 0.297(3) -0.349(7) 0.08(3) Uiso 1 1 d . . .
H48 H 0.034(3) 0.201(3) -0.345(7) 0.09(2) Uiso 1 1 d . . .
H49 H 0.038(4) 0.162(4) -0.544(8) 0.12(3) Uiso 1 1 d . . .
H50 H -0.068(3) 0.149(3) -0.671(7) 0.10(3) Uiso 1 1 d . . .
H51 H -0.149(4) 0.153(4) -0.567(8) 0.11(3) Uiso 1 1 d . . .
HW1A H 0.080(3) 0.133(3) -0.023(6) 0.05(2) Uiso 1 1 d . . .
HW1B H 0.134(3) 0.122(2) -0.026(5) 0.034(16) Uiso 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O31 Ni1 O31 88.4(2) . 4_655 ?
O31 Ni1 N1 177.69(15) . 4_655 ?
O31 Ni1 N1 89.43(15) 4_655 4_655 ?
O31 Ni1 N1 89.43(15) . . ?
O31 Ni1 N1 177.69(15) 4_655 . ?
N1 Ni1 N1 92.8(2) 4_655 . ?
O31 Ni1 O1 87.71(13) . 4_655 ?
O31 Ni1 O1 97.49(13) 4_655 4_655 ?
N1 Ni1 O1 91.96(14) 4_655 4_655 ?
N1 Ni1 O1 83.05(14) . 4_655 ?
O31 Ni1 O1 97.49(13) . . ?
O31 Ni1 O1 87.71(13) 4_655 . ?
N1 Ni1 O1 83.05(14) 4_655 . ?
N1 Ni1 O1 91.96(14) . . ?
O1 Ni1 O1 172.78(16) 4_655 . ?
O11 Ni2 O32 173.83(14) . . ?
O11 Ni2 O1 95.98(12) . . ?
O32 Ni2 O1 88.74(13) . . ?
O11 Ni2 N11 82.99(14) . . ?
O32 Ni2 N11 92.40(14) . . ?
O1 Ni2 N11 178.19(15) . . ?
O11 Ni2 OW1 91.19(15) . . ?
O32 Ni2 OW1 92.83(16) . . ?
O1 Ni2 OW1 89.52(14) . . ?
N11 Ni2 OW1 89.02(16) . . ?
O11 Ni2 O33 86.70(13) . . ?
O32 Ni2 O33 89.21(14) . . ?
O1 Ni2 O33 91.39(14) . . ?
N11 Ni2 O33 90.03(15) . . ?
OW1 Ni2 O33 177.78(15) . . ?
N12 Ni3 N21 174.06(16) . . ?
N12 Ni3 N22 98.40(16) . . ?
N21 Ni3 N22 79.50(17) . . ?
N12 Ni3 O35 90.36(15) . . ?
N21 Ni3 O35 91.58(16) . . ?
N22 Ni3 O35 170.99(16) . . ?
N12 Ni3 N13 77.16(15) . . ?
N21 Ni3 N13 97.08(16) . . ?
N22 Ni3 N13 85.15(17) . . ?
O35 Ni3 N13 94.78(16) . . ?
N12 Ni3 N31 91.03(16) . . ?
N21 Ni3 N31 94.54(16) . . ?
N22 Ni3 N31 90.89(16) . . ?
O35 Ni3 N31 91.08(15) . . ?
N13 Ni3 N31 166.82(16) . . ?
O11 Ni4 N3 170.20(14) . . ?
O11 Ni4 O36 95.41(13) . . ?
N3 Ni4 O36 94.02(15) . . ?
O11 Ni4 N2 92.71(13) . . ?
N3 Ni4 N2 77.64(15) . . ?
O36 Ni4 N2 169.79(14) . . ?
O11 Ni4 O34 85.25(13) . . ?
N3 Ni4 O34 92.27(16) . . ?
O36 Ni4 O34 89.08(15) . . ?
N2 Ni4 O34 85.43(15) . . ?
O11 Ni4 N31 91.16(14) . . ?
N3 Ni4 N31 91.84(17) . . ?
O36 Ni4 N31 87.85(16) . . ?
N2 Ni4 N31 98.18(16) . . ?
O34 Ni4 N31 175.04(15) . . ?
N2 O1 Ni2 114.4(2) . . ?
N2 O1 Ni1 118.8(2) . . ?
Ni2 O1 Ni1 125.33(15) . . ?
C1 N1 C5 117.7(4) . . ?
C1 N1 Ni1 119.2(3) . . ?
C5 N1 Ni1 123.0(3) . . ?
C6 N2 O1 119.2(4) . . ?
C6 N2 Ni4 116.9(3) . . ?
O1 N2 Ni4 121.9(3) . . ?
C11 N3 C7 118.5(5) . . ?
C11 N3 Ni4 126.3(4) . . ?
C7 N3 Ni4 114.2(3) . . ?
N12 O11 Ni2 115.9(2) . . ?
N12 O11 Ni4 119.1(2) . . ?
Ni2 O11 Ni4 110.17(14) . . ?
C21 N11 C25 118.0(4) . . ?
C21 N11 Ni2 119.4(3) . . ?
C25 N11 Ni2 122.2(3) . . ?
C26 N12 O11 118.3(4) . . ?
C26 N12 Ni3 120.4(3) . . ?
O11 N12 Ni3 121.1(3) . . ?
C31 N13 C27 118.7(4) . . ?
C31 N13 Ni3 125.7(4) . . ?
C27 N13 Ni3 112.4(3) . . ?
C45 N21 C41 118.5(5) . . ?
C45 N21 Ni3 114.3(3) . . ?
C41 N21 Ni3 127.0(4) . . ?
O21 N22 C46 119.4(4) . . ?
O21 N22 Ni3 124.6(3) . . ?
C46 N22 Ni3 115.4(3) . . ?
C61 O31 Ni1 133.1(3) 4_655 . ?
C61 O32 Ni2 137.8(3) . . ?
C63 O33 Ni2 130.2(3) . . ?
C63 O34 Ni4 132.9(3) . . ?
C65 O35 Ni3 131.3(3) . . ?
C65 O36 Ni4 133.4(3) . . ?
N32 N31 Ni4 124.2(4) . . ?
N32 N31 Ni3 119.2(3) . . ?
Ni4 N31 Ni3 106.81(18) . . ?
Ni2 OW1 HW1A 122(5) . . ?
Ni2 OW1 HW1B 109(4) . . ?
HW1A OW1 HW1B 106(6) . . ?
N1 C1 C2 123.8(5) . . ?
N1 C1 H1 114(3) . . ?
C2 C1 H1 122(3) . . ?
C1 C2 C3 118.8(5) . . ?
C1 C2 H2 120(4) . . ?
C3 C2 H2 121(4) . . ?
C4 C3 C2 118.6(5) . . ?
C4 C3 H3 124(4) . . ?
C2 C3 H3 118(4) . . ?
C3 C4 C5 120.2(5) . . ?
C3 C4 H4 127(4) . . ?
C5 C4 H4 112(4) . . ?
N1 C5 C4 120.9(5) . . ?
N1 C5 C6 118.9(4) . 4_655 ?
C4 C5 C6 120.0(5) . 4_655 ?
N2 C6 C5 126.9(4) . 4_655 ?
N2 C6 C7 112.3(4) . . ?
C5 C6 C7 120.4(4) 4_655 . ?
N3 C7 C8 121.4(5) . . ?
N3 C7 C6 115.5(4) . . ?
C8 C7 C6 123.1(5) . . ?
C9 C8 C7 119.1(6) . . ?
C9 C8 H8 122(3) . . ?
C7 C8 H8 118(3) . . ?
C10 C9 C8 119.6(6) . . ?
C10 C9 H9 121(4) . . ?
C8 C9 H9 117(4) . . ?
C9 C10 C11 118.5(6) . . ?
C9 C10 H10 120(4) . . ?
C11 C10 H10 121(4) . . ?
N3 C11 C10 122.8(6) . . ?
N3 C11 H11 116(3) . . ?
C10 C11 H11 121(3) . . ?
N11 C21 C22 124.0(6) . . ?
N11 C21 H21 112(3) . . ?
C22 C21 H21 123(3) . . ?
C23 C22 C21 118.1(6) . . ?
C23 C22 H22 121(4) . . ?
C21 C22 H22 121(4) . . ?
C22 C23 C24 119.2(6) . . ?
C22 C23 H23 119(5) . . ?
C24 C23 H23 122(5) . . ?
C23 C24 C25 119.9(5) . . ?
C23 C24 H24 120(3) . . ?
C25 C24 H24 120(3) . . ?
N11 C25 C24 120.7(5) . . ?
N11 C25 C26 118.4(4) . . ?
C24 C25 C26 120.9(4) . . ?
N12 C26 C25 125.9(4) . . ?
N12 C26 C27 112.4(4) . . ?
C25 C26 C27 121.6(4) . . ?
N13 C27 C28 120.7(5) . . ?
N13 C27 C26 114.5(4) . . ?
C28 C27 C26 124.7(5) . . ?
C29 C28 C27 119.7(5) . . ?
C29 C28 H28 127(4) . . ?
C27 C28 H28 114(4) . . ?
C30 C29 C28 119.0(5) . . ?
C30 C29 H29 123(3) . . ?
C28 C29 H29 118(3) . . ?
C29 C30 C31 118.7(6) . . ?
C29 C30 H30 122(4) . . ?
C31 C30 H30 119(4) . . ?
N13 C31 C30 123.0(5) . . ?
N13 C31 H31 112(3) . . ?
C30 C31 H31 125(3) . . ?
N21 C41 C42 123.0(6) . . ?
N21 C41 H41 114(3) . . ?
C42 C41 H41 123(3) . . ?
C43 C42 C41 118.7(6) . . ?
C43 C42 H42 119(3) . . ?
C41 C42 H42 122(3) . . ?
C42 C43 C44 119.0(7) . . ?
C42 C43 H43 127(6) . . ?
C44 C43 H43 114(6) . . ?
C43 C44 C45 121.0(7) . . ?
C43 C44 H44 116(6) . . ?
C45 C44 H44 123(6) . . ?
N21 C45 C44 119.8(6) . . ?
N21 C45 C46 115.9(5) . . ?
C44 C45 C46 124.3(6) . . ?
N22 C46 C47 123.4(5) . . ?
N22 C46 C45 114.3(5) . . ?
C47 C46 C45 122.2(5) . . ?
N23 C47 C48 121.1(6) . . ?
N23 C47 C46 115.7(5) . . ?
C48 C47 C46 123.3(6) . . ?
C47 C48 C49 119.7(7) . . ?
C47 C48 H48 114(5) . . ?
C49 C48 H48 126(5) . . ?
C50 C49 C48 118.8(7) . . ?
C50 C49 H49 122(5) . . ?
C48 C49 H49 117(5) . . ?
C49 C50 C51 118.9(7) . . ?
C49 C50 H50 126(4) . . ?
C51 C50 H50 115(4) . . ?
N23 C51 C50 123.1(7) . . ?
N23 C51 H51 122(6) . . ?
C50 C51 H51 115(6) . . ?
C51 N23 C47 118.4(6) . . ?
O32 C61 O31 126.1(4) . 4_655 ?
O32 C61 C62 117.1(4) . . ?
O31 C61 C62 116.8(4) 4_655 . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
O33 C63 O34 126.1(5) . . ?
O33 C63 C64 117.6(5) . . ?
O34 C63 C64 116.3(5) . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
O35 C65 O36 126.3(5) . . ?
O35 C65 C66 117.5(5) . . ?
O36 C65 C66 116.2(5) . . ?
C65 C66 H66A 109.5 . . ?
C65 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C65 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
N33 N32 N31 178.3(6) . . ?
N41 C71 C72 177.7(11) . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
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 O31 2.055(3) . ?
Ni1 O31 2.055(3) 4_655 ?
Ni1 N1 2.061(4) 4_655 ?
Ni1 N1 2.061(4) . ?
Ni1 O1 2.078(3) 4_655 ?
Ni1 O1 2.078(3) . ?
Ni2 O11 2.020(3) . ?
Ni2 O32 2.033(3) . ?
Ni2 O1 2.042(3) . ?
Ni2 N11 2.080(4) . ?
Ni2 OW1 2.085(4) . ?
Ni2 O33 2.094(4) . ?
Ni3 N12 2.007(4) . ?
Ni3 N21 2.045(4) . ?
Ni3 N22 2.054(4) . ?
Ni3 O35 2.084(4) . ?
Ni3 N13 2.100(4) . ?
Ni3 N31 2.110(4) . ?
Ni4 O11 2.021(3) . ?
Ni4 N3 2.072(4) . ?
Ni4 O36 2.076(3) . ?
Ni4 N2 2.080(4) . ?
Ni4 O34 2.084(4) . ?
Ni4 N31 2.095(4) . ?
O1 N2 1.348(4) . ?
N1 C1 1.351(6) . ?
N1 C5 1.353(6) . ?
N2 C6 1.294(6) . ?
N3 C11 1.338(6) . ?
N3 C7 1.346(7) . ?
O11 N12 1.353(5) . ?
N11 C21 1.331(7) . ?
N11 C25 1.361(6) . ?
N12 C26 1.297(6) . ?
N13 C31 1.331(7) . ?
N13 C27 1.355(6) . ?
O21 N22 1.299(5) . ?
N21 C45 1.349(7) . ?
N21 C41 1.351(7) . ?
N22 C46 1.333(7) . ?
O31 C61 1.263(6) 4_655 ?
O32 C61 1.248(5) . ?
O33 C63 1.251(6) . ?
O34 C63 1.265(6) . ?
O35 C65 1.248(6) . ?
O36 C65 1.258(6) . ?
N31 N32 1.200(6) . ?
OW1 HW1A 0.74(6) . ?
OW1 HW1B 0.76(6) . ?
C1 C2 1.359(8) . ?
C1 H1 0.98(5) . ?
C2 C3 1.378(8) . ?
C2 H2 0.94(6) . ?
C3 C4 1.378(8) . ?
C3 H3 0.89(6) . ?
C4 C5 1.388(7) . ?
C4 H4 0.94(6) . ?
C5 C6 1.483(6) 4_655 ?
C6 C5 1.483(6) 4_655 ?
C6 C7 1.498(7) . ?
C7 C8 1.387(7) . ?
C8 C9 1.379(8) . ?
C8 H8 0.95(5) . ?
C9 C10 1.367(10) . ?
C9 H9 1.00(7) . ?
C10 C11 1.380(9) . ?
C10 H10 0.86(6) . ?
C11 H11 1.01(5) . ?
C21 C22 1.373(8) . ?
C21 H21 0.80(4) . ?
C22 C23 1.372(9) . ?
C22 H22 0.92(6) . ?
C23 C24 1.379(9) . ?
C23 H23 0.87(7) . ?
C24 C25 1.383(7) . ?
C24 H24 1.00(5) . ?
C25 C26 1.481(7) . ?
C26 C27 1.485(7) . ?
C27 C28 1.388(7) . ?
C28 C29 1.381(8) . ?
C28 H28 0.78(5) . ?
C29 C30 1.372(9) . ?
C29 H29 0.94(5) . ?
C30 C31 1.381(8) . ?
C30 H30 0.95(6) . ?
C31 H31 1.01(5) . ?
C41 C42 1.370(9) . ?
C41 H41 1.02(5) . ?
C42 C43 1.354(11) . ?
C42 H42 0.92(5) . ?
C43 C44 1.376(10) . ?
C43 H43 0.87(8) . ?
C44 C45 1.377(9) . ?
C44 H44 0.77(7) . ?
C45 C46 1.477(7) . ?
C46 C47 1.468(8) . ?
C47 N23 1.345(7) . ?
C47 C48 1.376(8) . ?
C48 C49 1.385(10) . ?
C48 H48 0.96(7) . ?
C49 C50 1.359(10) . ?
C49 H49 1.02(8) . ?
C50 C51 1.371(10) . ?
C50 H50 1.09(8) . ?
C51 N23 1.331(8) . ?
C51 H51 0.91(8) . ?
C61 O31 1.263(6) 4_655 ?
C61 C62 1.507(7) . ?
C62 H62A 0.9600 . ?
C62 H62B 0.9600 . ?
C62 H62C 0.9600 . ?
C63 C64 1.510(8) . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
C65 C66 1.520(7) . ?
C66 H66A 0.9600 . ?
C66 H66B 0.9600 . ?
C66 H66C 0.9600 . ?
N32 N33 1.138(7) . ?
N41 C71 1.095(10) . ?
C71 C72 1.449(12) . ?
C72 H72A 0.9600 . ?
C72 H72B 0.9600 . ?
C72 H72C 0.9600 . ?
