#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:09:15 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179954 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/49/7024922.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_7024922
loop_
_publ_author_name
'Zhang, Suyun'
'Zhen, Lina'
'Xu, Bin'
'Inglis, Ross'
'Li, Kai'
'Chen, Wenqian'
'Zhang, Yong'
'Konidaris, Konstantis F.'
'Perlepes, Spyros P.'
'Brechin, Euan K.'
'Li, Yahong'
_publ_section_title
;
 Wheel-like Mn(II)6 and Ni(II)6 complexes from the use of
 2-pyridinealdoxime and carboxylates.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3563
_journal_page_last               3571
_journal_paper_doi               10.1039/b922672a
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C82 H54 Cl6 N12 Ni6 O20'
_chemical_formula_weight         2092.33
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_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                 112.460(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.278(18)
_cell_length_b                   11.302(5)
_cell_length_c                   27.664(16)
_cell_measurement_temperature    223(2)
_cell_volume                     8749(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0727
_diffrn_reflns_av_sigmaI/netI    0.0874
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20900
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.12
_exptl_absorpt_coefficient_mu    1.525
_exptl_absorpt_correction_T_max  0.8625
_exptl_absorpt_correction_T_min  0.5806
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4240
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         8052
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.1185
_refine_ls_R_factor_gt           0.0881
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0783P)²+29.3775P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1956
_refine_ls_wR_factor_ref         0.2142
_reflns_number_gt                6016
_reflns_number_total             8052
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b922672a.txt
_cod_data_source_block           3
_cod_original_cell_volume        8748(8)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7024922
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.56674(3) 0.29942(9) 0.54584(3) 0.0406(3) Uani 1 1 d . . .
Ni2 Ni 0.59987(3) 0.57173(9) 0.52060(3) 0.0400(3) Uani 1 1 d . . .
Ni3 Ni 0.50907(3) 0.58282(9) 0.40370(3) 0.0406(3) Uani 1 1 d . . .
Cl1 Cl 0.62852(13) -0.0886(3) 0.83776(10) 0.1114(12) Uani 1 1 d . . .
Cl2 Cl 0.85373(8) 0.1483(3) 0.58114(13) 0.0972(10) Uani 1 1 d . . .
Cl3 Cl 0.74140(9) 0.8665(3) 0.32829(12) 0.0916(9) Uani 1 1 d . . .
O1 O 0.46280(16) 0.3352(4) 0.52509(18) 0.0410(11) Uani 1 1 d . . .
O2 O 0.55688(16) 0.4374(4) 0.58672(18) 0.0417(11) Uani 1 1 d . . .
O3 O 0.56921(16) 0.4153(4) 0.48607(18) 0.0399(11) Uani 1 1 d . . .
O4 O 0.57558(17) 0.1957(5) 0.61023(19) 0.0472(12) Uani 1 1 d . . .
O5 O 0.52068(17) 0.2731(5) 0.63828(19) 0.0493(13) Uani 1 1 d . . .
O6 O 0.63931(17) 0.3037(5) 0.5744(2) 0.0515(13) Uani 1 1 d . . .
O7 O 0.66208(16) 0.4777(5) 0.55260(19) 0.0453(12) Uani 1 1 d . . .
O8 O 0.62732(16) 0.6320(5) 0.4690(2) 0.0495(13) Uani 1 1 d . . .
O9 O 0.56854(16) 0.6248(5) 0.38833(19) 0.0486(13) Uani 1 1 d . . .
N1 N 0.5632(2) 0.1513(6) 0.5001(2) 0.0465(15) Uani 1 1 d . . .
N2 N 0.49491(19) 0.2720(5) 0.5130(2) 0.0386(14) Uani 1 1 d . . .
N3 N 0.63227(19) 0.7111(5) 0.5702(2) 0.0434(14) Uani 1 1 d . . .
N4 N 0.58059(18) 0.5370(5) 0.5824(2) 0.0389(14) Uani 1 1 d . . .
N5 N 0.48585(19) 0.4746(6) 0.3382(2) 0.0420(14) Uani 1 1 d . . .
N6 N 0.53820(18) 0.4284(5) 0.4360(2) 0.0380(13) Uani 1 1 d . . .
C1 C 0.5991(3) 0.0916(7) 0.4930(3) 0.0505(19) Uani 1 1 d . . .
H1 H 0.6309 0.1123 0.5133 0.061 Uiso 1 1 calc R . .
C2 C 0.5906(3) 0.0017(7) 0.4570(3) 0.055(2) Uani 1 1 d . . .
H2 H 0.6163 -0.0370 0.4526 0.067 Uiso 1 1 calc R . .
C3 C 0.5447(3) -0.0314(8) 0.4277(3) 0.058(2) Uani 1 1 d . . .
H3 H 0.5384 -0.0929 0.4031 0.069 Uiso 1 1 calc R . .
C4 C 0.5074(3) 0.0278(7) 0.4349(3) 0.0513(19) Uani 1 1 d . . .
H4 H 0.4755 0.0062 0.4156 0.062 Uiso 1 1 calc R . .
C5 C 0.5180(2) 0.1198(7) 0.4713(3) 0.0416(16) Uani 1 1 d . . .
C6 C 0.4803(2) 0.1864(7) 0.4796(3) 0.0453(18) Uani 1 1 d . . .
H6 H 0.4478 0.1685 0.4619 0.054 Uiso 1 1 calc R . .
C7 C 0.6592(3) 0.7972(7) 0.5636(3) 0.0480(18) Uani 1 1 d . . .
H7 H 0.6630 0.8021 0.5314 0.058 Uiso 1 1 calc R . .
C8 C 0.6819(3) 0.8796(8) 0.6015(4) 0.067(2) Uani 1 1 d . . .
H8 H 0.7011 0.9386 0.5954 0.080 Uiso 1 1 calc R . .
C9 C 0.6763(3) 0.8747(9) 0.6484(4) 0.075(3) Uani 1 1 d . . .
H9 H 0.6914 0.9304 0.6748 0.090 Uiso 1 1 calc R . .
C10 C 0.6481(3) 0.7868(8) 0.6560(4) 0.065(2) Uani 1 1 d . . .
H10 H 0.6435 0.7821 0.6877 0.078 Uiso 1 1 calc R . .
C11 C 0.6263(2) 0.7044(7) 0.6159(3) 0.0460(18) Uani 1 1 d . . .
C12 C 0.5978(3) 0.6063(7) 0.6218(3) 0.0473(18) Uani 1 1 d . . .
H12 H 0.5923 0.5944 0.6526 0.057 Uiso 1 1 calc R . .
C13 C 0.4563(3) 0.5015(9) 0.2890(3) 0.059(2) Uani 1 1 d . . .
H13 H 0.4476 0.5810 0.2807 0.070 Uiso 1 1 calc R . .
C14 C 0.4382(3) 0.4165(9) 0.2502(3) 0.065(2) Uani 1 1 d . . .
H14 H 0.4182 0.4382 0.2160 0.078 Uiso 1 1 calc R . .
C15 C 0.4503(4) 0.2991(10) 0.2628(4) 0.078(3) Uani 1 1 d . . .
H15 H 0.4376 0.2394 0.2376 0.093 Uiso 1 1 calc R . .
C16 C 0.4811(3) 0.2711(8) 0.3128(3) 0.061(2) Uani 1 1 d . . .
H16 H 0.4905 0.1922 0.3217 0.073 Uiso 1 1 calc R . .
C17 C 0.4983(3) 0.3602(7) 0.3498(3) 0.0450(18) Uani 1 1 d . . .
C18 C 0.5314(3) 0.3385(7) 0.4041(3) 0.0433(17) Uani 1 1 d . . .
H18 H 0.5466 0.2651 0.4150 0.052 Uiso 1 1 calc R . .
C19 C 0.5552(3) 0.2041(7) 0.6419(3) 0.0456(18) Uani 1 1 d . . .
C20 C 0.5722(3) 0.1271(7) 0.6903(3) 0.0503(19) Uani 1 1 d . . .
C21 C 0.5484(3) 0.1259(8) 0.7242(3) 0.064(2) Uani 1 1 d . . .
H21 H 0.5204 0.1706 0.7164 0.076 Uiso 1 1 calc R . .
C22 C 0.5659(4) 0.0587(10) 0.7697(4) 0.077(3) Uani 1 1 d . . .
H22 H 0.5497 0.0575 0.7928 0.093 Uiso 1 1 calc R . .
C23 C 0.6068(4) -0.0057(9) 0.7805(3) 0.073(3) Uani 1 1 d . . .
C24 C 0.6296(4) -0.0091(8) 0.7474(3) 0.072(3) Uani 1 1 d . . .
H24 H 0.6569 -0.0566 0.7552 0.086 Uiso 1 1 calc R . .
C25 C 0.6130(3) 0.0570(8) 0.7016(3) 0.063(2) Uani 1 1 d . . .
H25 H 0.6290 0.0546 0.6785 0.075 Uiso 1 1 calc R . .
C26 C 0.6685(2) 0.3715(8) 0.5656(3) 0.0472(19) Uani 1 1 d . . .
C27 C 0.7160(2) 0.3167(7) 0.5719(3) 0.0464(19) Uani 1 1 d . . .
C28 C 0.7292(3) 0.2082(8) 0.5956(4) 0.069(3) Uani 1 1 d . . .
H28 H 0.7096 0.1690 0.6098 0.082 Uiso 1 1 calc R . .
C29 C 0.7725(3) 0.1560(9) 0.5985(4) 0.078(3) Uani 1 1 d . . .
H29 H 0.7816 0.0816 0.6143 0.094 Uiso 1 1 calc R . .
C30 C 0.8011(3) 0.2133(9) 0.5783(4) 0.068(3) Uani 1 1 d . . .
C31 C 0.7882(3) 0.3217(9) 0.5549(3) 0.059(2) Uani 1 1 d . . .
H31 H 0.8081 0.3608 0.5410 0.070 Uiso 1 1 calc R . .
C32 C 0.7449(2) 0.3745(8) 0.5516(3) 0.0502(19) Uani 1 1 d . . .
H32 H 0.7358 0.4488 0.5356 0.060 Uiso 1 1 calc R . .
C33 C 0.6102(3) 0.6457(7) 0.4200(3) 0.0462(18) Uani 1 1 d . . .
C34 C 0.6445(3) 0.6968(7) 0.3971(3) 0.0439(17) Uani 1 1 d . . .
C35 C 0.6884(2) 0.7408(8) 0.4289(3) 0.057(2) Uani 1 1 d . . .
H35 H 0.6980 0.7344 0.4654 0.068 Uiso 1 1 calc R . .
C36 C 0.7187(3) 0.7944(8) 0.4085(3) 0.056(2) Uani 1 1 d . . .
H36 H 0.7479 0.8275 0.4305 0.067 Uiso 1 1 calc R . .
C37 C 0.7045(3) 0.7973(8) 0.3556(4) 0.059(2) Uani 1 1 d . . .
C38 C 0.6612(3) 0.7509(9) 0.3219(3) 0.066(2) Uani 1 1 d . . .
H38 H 0.6525 0.7532 0.2855 0.079 Uiso 1 1 calc R . .
C39 C 0.6309(3) 0.7008(8) 0.3436(3) 0.058(2) Uani 1 1 d . . .
H39 H 0.6011 0.6697 0.3217 0.069 Uiso 1 1 calc R . .
C40 C 0.1936(5) 0.0914(15) 0.2037(6) 0.134(6) Uani 1 1 d D . .
C41 C 0.2019(7) 0.0120(19) 0.2509(6) 0.170(7) Uani 1 1 d . A .
O10 O 0.1482(5) 0.1439(16) 0.1946(5) 0.125(6) Uani 0.688(16) 1 d PD A 1
O10' O 0.1789(13) 0.213(2) 0.1881(11) 0.125(6) Uani 0.312(16) 1 d PD A 2
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'
Cl Cl 0.1484 0.1585 '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 Ni1 O6 97.7(2) . .
O2 Ni1 N2 90.4(2) . .
O6 Ni1 N2 171.8(2) . .
O2 Ni1 O4 87.3(2) . .
O6 Ni1 O4 85.0(2) . .
N2 Ni1 O4 93.6(2) . .
O2 Ni1 N1 169.1(2) . .
O6 Ni1 N1 93.0(2) . .
N2 Ni1 N1 78.9(2) . .
O4 Ni1 N1 91.6(2) . .
O2 Ni1 O3 90.94(19) . .
O6 Ni1 O3 86.20(19) . .
N2 Ni1 O3 95.47(19) . .
O4 Ni1 O3 170.77(19) . .
N1 Ni1 O3 91.8(2) . .
O8 Ni2 N4 168.4(2) . .
O8 Ni2 O7 85.5(2) . .
N4 Ni2 O7 92.8(2) . .
O8 Ni2 O3 101.3(2) . .
N4 Ni2 O3 90.1(2) . .
O7 Ni2 O3 86.1(2) . .
O8 Ni2 N3 89.6(2) . .
N4 Ni2 N3 78.9(2) . .
O7 Ni2 N3 89.1(2) . .
O3 Ni2 N3 167.7(2) . .
O8 Ni2 O1 85.84(19) . 5_666
N4 Ni2 O1 96.75(19) . 5_666
O7 Ni2 O1 169.87(19) . 5_666
O3 Ni2 O1 90.41(19) . 5_666
N3 Ni2 O1 96.2(2) . 5_666
O5 Ni3 N6 171.8(2) 5_666 .
O5 Ni3 O1 96.9(2) 5_666 5_666
N6 Ni3 O1 90.8(2) . 5_666
O5 Ni3 O9 85.9(2) 5_666 .
N6 Ni3 O9 91.3(2) . .
O1 Ni3 O9 91.1(2) 5_666 .
O5 Ni3 N5 92.6(2) 5_666 .
N6 Ni3 N5 79.7(2) . .
O1 Ni3 N5 170.5(2) 5_666 .
O9 Ni3 N5 89.3(2) . .
O5 Ni3 O2 85.65(19) 5_666 5_666
N6 Ni3 O2 97.2(2) . 5_666
O1 Ni3 O2 89.66(18) 5_666 5_666
O9 Ni3 O2 171.5(2) . 5_666
N5 Ni3 O2 91.4(2) . 5_666
N2 O1 Ni3 113.9(4) . 5_666
N2 O1 Ni2 133.1(4) . 5_666
Ni3 O1 Ni2 107.4(2) 5_666 5_666
N4 O2 Ni1 113.2(4) . .
N4 O2 Ni3 130.6(4) . 5_666
Ni1 O2 Ni3 109.5(2) . 5_666
N6 O3 Ni2 113.3(4) . .
N6 O3 Ni1 130.2(4) . .
Ni2 O3 Ni1 108.1(2) . .
C19 O4 Ni1 128.7(5) . .
C19 O5 Ni3 135.7(5) . 5_666
C26 O6 Ni1 132.2(5) . .
C26 O7 Ni2 129.8(5) . .
C33 O8 Ni2 133.5(5) . .
C33 O9 Ni3 128.7(5) . .
C5 N1 C1 118.3(7) . .
C5 N1 Ni1 112.2(5) . .
C1 N1 Ni1 129.2(5) . .
C6 N2 O1 119.5(6) . .
C6 N2 Ni1 116.6(5) . .
O1 N2 Ni1 123.9(4) . .
C7 N3 C11 118.7(7) . .
C7 N3 Ni2 128.9(5) . .
C11 N3 Ni2 112.3(5) . .
C12 N4 O2 119.2(6) . .
C12 N4 Ni2 116.1(5) . .
O2 N4 Ni2 124.0(4) . .
C17 N5 C13 118.2(7) . .
C17 N5 Ni3 112.8(5) . .
C13 N5 Ni3 128.5(6) . .
C18 N6 O3 118.3(6) . .
C18 N6 Ni3 116.4(5) . .
O3 N6 Ni3 124.6(4) . .
N1 C1 C2 122.2(7) . .
N1 C1 H1 118.9 . .
C2 C1 H1 118.9 . .
C3 C2 C1 119.9(7) . .
C3 C2 H2 120.0 . .
C1 C2 H2 120.0 . .
C2 C3 C4 118.7(8) . .
C2 C3 H3 120.7 . .
C4 C3 H3 120.7 . .
C3 C4 C5 119.1(7) . .
C3 C4 H4 120.5 . .
C5 C4 H4 120.5 . .
N1 C5 C4 121.7(7) . .
N1 C5 C6 116.9(7) . .
C4 C5 C6 121.3(7) . .
N2 C6 C5 115.2(6) . .
N2 C6 H6 122.4 . .
C5 C6 H6 122.4 . .
N3 C7 C8 123.2(8) . .
N3 C7 H7 118.4 . .
C8 C7 H7 118.4 . .
C9 C8 C7 119.1(9) . .
C9 C8 H8 120.4 . .
C7 C8 H8 120.4 . .
C8 C9 C10 118.8(9) . .
C8 C9 H9 120.6 . .
C10 C9 H9 120.6 . .
C9 C10 C11 119.2(8) . .
C9 C10 H10 120.4 . .
C11 C10 H10 120.4 . .
N3 C11 C10 120.9(7) . .
N3 C11 C12 116.5(7) . .
C10 C11 C12 122.6(7) . .
N4 C12 C11 116.0(7) . .
N4 C12 H12 122.0 . .
C11 C12 H12 122.0 . .
N5 C13 C14 122.7(8) . .
N5 C13 H13 118.7 . .
C14 C13 H13 118.7 . .
C15 C14 C13 118.7(8) . .
C15 C14 H14 120.7 . .
C13 C14 H14 120.7 . .
C16 C15 C14 119.0(9) . .
C16 C15 H15 120.5 . .
C14 C15 H15 120.5 . .
C15 C16 C17 119.5(9) . .
C15 C16 H16 120.2 . .
C17 C16 H16 120.2 . .
N5 C17 C16 121.9(7) . .
N5 C17 C18 114.9(7) . .
C16 C17 C18 123.2(8) . .
N6 C18 C17 115.4(7) . .
N6 C18 H18 122.3 . .
C17 C18 H18 122.3 . .
O4 C19 O5 126.7(7) . .
O4 C19 C20 118.8(7) . .
O5 C19 C20 114.5(6) . .
C21 C20 C25 119.1(7) . .
C21 C20 C19 121.0(7) . .
C25 C20 C19 119.9(7) . .
C20 C21 C22 120.3(8) . .
C20 C21 H21 119.9 . .
C22 C21 H21 119.9 . .
C23 C22 C21 119.1(9) . .
C23 C22 H22 120.4 . .
C21 C22 H22 120.4 . .
C24 C23 C22 121.7(8) . .
C24 C23 Cl1 119.5(8) . .
C22 C23 Cl1 118.8(8) . .
C23 C24 C25 120.4(9) . .
C23 C24 H24 119.8 . .
C25 C24 H24 119.8 . .
C24 C25 C20 119.4(8) . .
C24 C25 H25 120.3 . .
C20 C25 H25 120.3 . .
O7 C26 O6 126.8(6) . .
O7 C26 C27 117.6(7) . .
O6 C26 C27 115.6(7) . .
C32 C27 C28 120.3(7) . .
C32 C27 C26 118.9(7) . .
C28 C27 C26 120.8(7) . .
C27 C28 C29 119.7(9) . .
C27 C28 H28 120.2 . .
C29 C28 H28 120.2 . .
C30 C29 C28 120.0(9) . .
C30 C29 H29 120.0 . .
C28 C29 H29 120.0 . .
C29 C30 C31 120.5(7) . .
C29 C30 Cl2 119.9(8) . .
C31 C30 Cl2 119.6(8) . .
C30 C31 C32 120.0(8) . .
C30 C31 H31 120.0 . .
C32 C31 H31 120.0 . .
C27 C32 C31 119.5(8) . .
C27 C32 H32 120.2 . .
C31 C32 H32 120.2 . .
O9 C33 O8 128.2(7) . .
O9 C33 C34 116.3(7) . .
O8 C33 C34 115.4(7) . .
C35 C34 C39 119.6(7) . .
C35 C34 C33 121.0(7) . .
C39 C34 C33 119.3(7) . .
C34 C35 C36 121.6(8) . .
C34 C35 H35 119.2 . .
C36 C35 H35 119.2 . .
C37 C36 C35 117.6(7) . .
C37 C36 H36 121.2 . .
C35 C36 H36 121.2 . .
C36 C37 C38 122.8(7) . .
C36 C37 Cl3 118.9(7) . .
C38 C37 Cl3 118.3(7) . .
C37 C38 C39 118.2(8) . .
C37 C38 H38 120.9 . .
C39 C38 H38 120.9 . .
C34 C39 C38 120.1(8) . .
C34 C39 H39 120.0 . .
C38 C39 H39 120.0 . .
O10 C40 O10' 52.6(14) . .
O10 C40 C41 103.1(15) . .
O10' C40 C41 137.7(18) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O2 2.015(5) .
Ni1 O6 2.032(5) .
Ni1 N2 2.035(6) .
Ni1 O4 2.062(5) .
Ni1 N1 2.077(7) .
Ni1 O3 2.133(5) .
Ni2 O8 2.025(5) .
Ni2 N4 2.045(6) .
Ni2 O7 2.046(5) .
Ni2 O3 2.055(5) .
Ni2 N3 2.072(6) .
Ni2 O1 2.114(5) 5_666
Ni3 O5 2.003(5) 5_666
Ni3 N6 2.005(6) .
Ni3 O1 2.045(5) 5_666
Ni3 O9 2.057(5) .
Ni3 N5 2.073(6) .
Ni3 O2 2.125(5) 5_666
Cl1 C23 1.738(9) .
Cl2 C30 1.729(8) .
Cl3 C37 1.754(8) .
O1 N2 1.348(7) .
O1 Ni3 2.045(5) 5_666
O1 Ni2 2.115(5) 5_666
O2 N4 1.364(7) .
O2 Ni3 2.125(5) 5_666
O3 N6 1.351(7) .
O4 C19 1.255(8) .
O5 C19 1.276(9) .
O5 Ni3 2.003(5) 5_666
O6 C26 1.262(9) .
O7 C26 1.246(10) .
O8 C33 1.260(8) .
O9 C33 1.254(9) .
N1 C5 1.342(9) .
N1 C1 1.356(9) .
N2 C6 1.294(9) .
N3 C7 1.327(9) .
N3 C11 1.347(9) .
N4 C12 1.279(9) .
N5 C17 1.351(10) .
N5 C13 1.346(9) .
N6 C18 1.311(9) .
C1 C2 1.375(11) .
C1 H1 0.9400 .
C2 C3 1.366(11) .
C2 H2 0.9400 .
C3 C4 1.391(10) .
C3 H3 0.9400 .
C4 C5 1.397(11) .
C4 H4 0.9400 .
C5 C6 1.454(10) .
C6 H6 0.9400 .
C7 C8 1.374(12) .
C7 H7 0.9400 .
C8 C9 1.373(13) .
C8 H8 0.9400 .
C9 C10 1.378(13) .
C9 H9 0.9400 .
C10 C11 1.405(11) .
C10 H10 0.9400 .
C11 C12 1.452(11) .
C12 H12 0.9400 .
C13 C14 1.388(12) .
C13 H13 0.9400 .
C14 C15 1.385(13) .
C14 H14 0.9400 .
C15 C16 1.377(12) .
C15 H15 0.9400 .
C16 C17 1.388(11) .
C16 H16 0.9400 .
C17 C18 1.473(10) .
C18 H18 0.9400 .
C19 C20 1.512(10) .
C20 C21 1.384(11) .
C20 C25 1.397(11) .
C21 C22 1.390(12) .
C21 H21 0.9400 .
C22 C23 1.368(13) .
C22 H22 0.9400 .
C23 C24 1.342(13) .
C24 C25 1.388(12) .
C24 H24 0.9400 .
C25 H25 0.9400 .
C26 C27 1.515(9) .
C27 C32 1.372(11) .
C27 C28 1.375(11) .
C28 C29 1.411(11) .
C28 H28 0.9400 .
C29 C30 1.360(14) .
C29 H29 0.9400 .
C30 C31 1.370(13) .
C31 C32 1.411(10) .
C31 H31 0.9400 .
C32 H32 0.9400 .
C33 C34 1.521(10) .
C34 C35 1.377(10) .
C34 C39 1.377(11) .
C35 C36 1.387(11) .
C35 H35 0.9400 .
C36 C37 1.360(11) .
C36 H36 0.9400 .
C37 C38 1.389(12) .
C38 C39 1.394(11) .
C38 H38 0.9400 .
C39 H39 0.9400 .
C40 O10 1.428(14) .
C40 O10' 1.462(18) .
C40 C41 1.52(2) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O6 Ni1 O2 N4 51.6(4) . .
N2 Ni1 O2 N4 -130.1(4) . .
O4 Ni1 O2 N4 136.3(4) . .
N1 Ni1 O2 N4 -139.1(11) . .
O3 Ni1 O2 N4 -34.7(4) . .
O6 Ni1 O2 Ni3 -153.8(2) . 5_666
N2 Ni1 O2 Ni3 24.5(2) . 5_666
O4 Ni1 O2 Ni3 -69.1(2) . 5_666
N1 Ni1 O2 Ni3 15.5(13) . 5_666
O3 Ni1 O2 Ni3 119.9(2) . 5_666
O8 Ni2 O3 N6 -54.3(4) . .
N4 Ni2 O3 N6 128.2(4) . .
O7 Ni2 O3 N6 -139.0(4) . .
N3 Ni2 O3 N6 153.9(8) . .
O1 Ni2 O3 N6 31.5(4) 5_666 .
O8 Ni2 O3 Ni1 154.0(2) . .
N4 Ni2 O3 Ni1 -23.4(2) . .
O7 Ni2 O3 Ni1 69.4(2) . .
N3 Ni2 O3 Ni1 2.3(10) . .
O1 Ni2 O3 Ni1 -120.1(2) 5_666 .
O2 Ni1 O3 N6 -111.9(5) . .
O6 Ni1 O3 N6 150.4(5) . .
N2 Ni1 O3 N6 -21.5(5) . .
O4 Ni1 O3 N6 169.0(10) . .
N1 Ni1 O3 N6 57.5(5) . .
O2 Ni1 O3 Ni2 33.3(2) . .
O6 Ni1 O3 Ni2 -64.4(2) . .
N2 Ni1 O3 Ni2 123.7(2) . .
O4 Ni1 O3 Ni2 -45.8(13) . .
N1 Ni1 O3 Ni2 -157.3(2) . .
O2 Ni1 O4 C19 34.9(6) . .
O6 Ni1 O4 C19 132.9(6) . .
N2 Ni1 O4 C19 -55.3(6) . .
N1 Ni1 O4 C19 -134.3(6) . .
O3 Ni1 O4 C19 114.2(12) . .
O2 Ni1 O6 C26 -75.2(7) . .
N2 Ni1 O6 C26 117.3(15) . .
O4 Ni1 O6 C26 -161.8(7) . .
N1 Ni1 O6 C26 106.8(7) . .
O3 Ni1 O6 C26 15.3(7) . .
O8 Ni2 O7 C26 -132.4(6) . .
N4 Ni2 O7 C26 59.1(6) . .
O3 Ni2 O7 C26 -30.8(6) . .
N3 Ni2 O7 C26 137.9(6) . .
O1 Ni2 O7 C26 -100.8(13) 5_666 .
N4 Ni2 O8 C33 -142.8(10) . .
O7 Ni2 O8 C33 135.3(7) . .
O3 Ni2 O8 C33 50.2(7) . .
N3 Ni2 O8 C33 -135.6(7) . .
O1 Ni2 O8 C33 -39.4(7) 5_666 .
O5 Ni3 O9 C33 121.5(7) 5_666 .
N6 Ni3 O9 C33 -66.1(7) . .
O1 Ni3 O9 C33 24.7(7) 5_666 .
N5 Ni3 O9 C33 -145.8(7) . .
O2 Ni3 O9 C33 119.8(13) 5_666 .
O2 Ni1 N1 C5 13.1(15) . .
O6 Ni1 N1 C5 -177.6(5) . .
N2 Ni1 N1 C5 3.9(5) . .
O4 Ni1 N1 C5 97.3(5) . .
O3 Ni1 N1 C5 -91.3(5) . .
O2 Ni1 N1 C1 -172.6(10) . .
O6 Ni1 N1 C1 -3.2(6) . .
N2 Ni1 N1 C1 178.3(7) . .
O4 Ni1 N1 C1 -88.4(6) . .
O3 Ni1 N1 C1 83.0(6) . .
Ni3 O1 N2 C6 156.6(5) 5_666 .
Ni2 O1 N2 C6 -53.8(8) 5_666 .
Ni3 O1 N2 Ni1 -21.6(6) 5_666 .
Ni2 O1 N2 Ni1 127.9(4) 5_666 .
O2 Ni1 N2 C6 178.8(5) . .
O6 Ni1 N2 C6 -13.6(18) . .
O4 Ni1 N2 C6 -93.9(5) . .
N1 Ni1 N2 C6 -3.0(5) . .
O3 Ni1 N2 C6 87.8(5) . .
O2 Ni1 N2 O1 -2.9(5) . .
O6 Ni1 N2 O1 164.8(13) . .
O4 Ni1 N2 O1 84.4(5) . .
N1 Ni1 N2 O1 175.4(5) . .
O3 Ni1 N2 O1 -93.9(5) . .
O8 Ni2 N3 C7 -0.1(6) . .
N4 Ni2 N3 C7 178.4(6) . .
O7 Ni2 N3 C7 85.4(6) . .
O3 Ni2 N3 C7 152.2(8) . .
O1 Ni2 N3 C7 -85.9(6) 5_666 .
O8 Ni2 N3 C11 -175.6(5) . .
N4 Ni2 N3 C11 2.9(5) . .
O7 Ni2 N3 C11 -90.1(5) . .
O3 Ni2 N3 C11 -23.3(12) . .
O1 Ni2 N3 C11 98.6(5) 5_666 .
Ni1 O2 N4 C12 -145.3(5) . .
Ni3 O2 N4 C12 66.8(7) 5_666 .
Ni1 O2 N4 Ni2 24.8(5) . .
Ni3 O2 N4 Ni2 -123.0(4) 5_666 .
O8 Ni2 N4 C12 3.7(13) . .
O7 Ni2 N4 C12 84.9(5) . .
O3 Ni2 N4 C12 171.0(5) . .
N3 Ni2 N4 C12 -3.6(5) . .
O1 Ni2 N4 C12 -98.6(5) 5_666 .
O8 Ni2 N4 O2 -166.7(9) . .
O7 Ni2 N4 O2 -85.5(5) . .
O3 Ni2 N4 O2 0.6(4) . .
N3 Ni2 N4 O2 -174.0(5) . .
O1 Ni2 N4 O2 91.0(4) 5_666 .
O5 Ni3 N5 C17 -178.7(5) 5_666 .
N6 Ni3 N5 C17 4.1(4) . .
O1 Ni3 N5 C17 3.2(15) 5_666 .
O9 Ni3 N5 C17 95.5(5) . .
O2 Ni3 N5 C17 -93.0(5) 5_666 .
O5 Ni3 N5 C13 -7.3(6) 5_666 .
N6 Ni3 N5 C13 175.4(7) . .
O1 Ni3 N5 C13 174.6(10) 5_666 .
O9 Ni3 N5 C13 -93.1(6) . .
O2 Ni3 N5 C13 78.4(6) 5_666 .
Ni2 O3 N6 C18 152.9(5) . .
Ni1 O3 N6 C18 -63.3(7) . .
Ni2 O3 N6 Ni3 -17.3(6) . .
Ni1 O3 N6 Ni3 126.5(4) . .
O5 Ni3 N6 C18 -17.7(18) 5_666 .
O1 Ni3 N6 C18 -178.2(5) 5_666 .
O9 Ni3 N6 C18 -87.1(5) . .
N5 Ni3 N6 C18 1.9(5) . .
O2 Ni3 N6 C18 92.0(5) 5_666 .
O5 Ni3 N6 O3 152.7(13) 5_666 .
O1 Ni3 N6 O3 -7.8(5) 5_666 .
O9 Ni3 N6 O3 83.3(5) . .
N5 Ni3 N6 O3 172.3(5) . .
O2 Ni3 N6 O3 -97.6(5) 5_666 .
C5 N1 C1 C2 0.9(11) . .
Ni1 N1 C1 C2 -173.2(6) . .
N1 C1 C2 C3 -1.1(13) . .
C1 C2 C3 C4 0.2(13) . .
C2 C3 C4 C5 0.8(12) . .
C1 N1 C5 C4 0.3(11) . .
Ni1 N1 C5 C4 175.3(6) . .
C1 N1 C5 C6 -179.5(6) . .
Ni1 N1 C5 C6 -4.4(8) . .
C3 C4 C5 N1 -1.1(12) . .
C3 C4 C5 C6 178.6(7) . .
O1 N2 C6 C5 -176.9(5) . .
Ni1 N2 C6 C5 1.5(8) . .
N1 C5 C6 N2 2.1(10) . .
C4 C5 C6 N2 -177.6(7) . .
C11 N3 C7 C8 0.7(11) . .
Ni2 N3 C7 C8 -174.6(6) . .
N3 C7 C8 C9 -0.9(13) . .
C7 C8 C9 C10 0.2(14) . .
C8 C9 C10 C11 0.6(14) . .
C7 N3 C11 C10 0.1(10) . .
Ni2 N3 C11 C10 176.1(6) . .
C7 N3 C11 C12 -178.1(6) . .
Ni2 N3 C11 C12 -2.0(8) . .
C9 C10 C11 N3 -0.8(12) . .
C9 C10 C11 C12 177.3(8) . .
O2 N4 C12 C11 174.5(6) . .
Ni2 N4 C12 C11 3.6(8) . .
N3 C11 C12 N4 -1.0(10) . .
C10 C11 C12 N4 -179.1(7) . .
C17 N5 C13 C14 0.3(11) . .
Ni3 N5 C13 C14 -170.7(6) . .
N5 C13 C14 C15 1.3(14) . .
C13 C14 C15 C16 -2.4(15) . .
C14 C15 C16 C17 2.0(14) . .
C13 N5 C17 C16 -0.7(10) . .
Ni3 N5 C17 C16 171.7(6) . .
C13 N5 C17 C18 178.8(6) . .
Ni3 N5 C17 C18 -8.8(7) . .
C15 C16 C17 N5 -0.5(12) . .
C15 C16 C17 C18 -179.9(8) . .
O3 N6 C18 C17 -178.2(5) . .
Ni3 N6 C18 C17 -7.2(8) . .
N5 C17 C18 N6 10.7(9) . .
C16 C17 C18 N6 -169.7(7) . .
Ni1 O4 C19 O5 7.2(12) . .
Ni1 O4 C19 C20 -172.2(5) . .
Ni3 O5 C19 O4 -15.6(13) 5_666 .
Ni3 O5 C19 C20 163.8(5) 5_666 .
O4 C19 C20 C21 -174.6(8) . .
O5 C19 C20 C21 6.0(11) . .
O4 C19 C20 C25 6.2(12) . .
O5 C19 C20 C25 -173.3(8) . .
C25 C20 C21 C22 2.2(14) . .
C19 C20 C21 C22 -177.1(8) . .
C20 C21 C22 C23 0.1(15) . .
C21 C22 C23 C24 -2.5(16) . .
C21 C22 C23 Cl1 179.6(8) . .
C22 C23 C24 C25 2.5(16) . .
Cl1 C23 C24 C25 -179.6(8) . .
C23 C24 C25 C20 -0.1(15) . .
C21 C20 C25 C24 -2.2(14) . .
C19 C20 C25 C24 177.0(8) . .
Ni2 O7 C26 O6 -19.5(12) . .
Ni2 O7 C26 C27 160.9(5) . .
Ni1 O6 C26 O7 29.4(12) . .
Ni1 O6 C26 C27 -150.9(5) . .
O7 C26 C27 C32 -15.5(11) . .
O6 C26 C27 C32 164.8(7) . .
O7 C26 C27 C28 167.4(8) . .
O6 C26 C27 C28 -12.2(11) . .
C32 C27 C28 C29 -0.5(14) . .
C26 C27 C28 C29 176.5(8) . .
C27 C28 C29 C30 0.5(15) . .
C28 C29 C30 C31 -0.2(15) . .
C28 C29 C30 Cl2 -179.2(8) . .
C29 C30 C31 C32 -0.1(13) . .
Cl2 C30 C31 C32 178.9(6) . .
C28 C27 C32 C31 0.3(12) . .
C26 C27 C32 C31 -176.8(7) . .
C30 C31 C32 C27 0.0(12) . .
Ni3 O9 C33 O8 9.6(12) . .
Ni3 O9 C33 C34 -168.8(5) . .
Ni2 O8 C33 O9 0.6(13) . .
Ni2 O8 C33 C34 179.1(5) . .
O9 C33 C34 C35 169.3(8) . .
O8 C33 C34 C35 -9.3(11) . .
O9 C33 C34 C39 -9.5(11) . .
O8 C33 C34 C39 171.8(7) . .
C39 C34 C35 C36 3.0(13) . .
C33 C34 C35 C36 -175.9(8) . .
C34 C35 C36 C37 -2.9(13) . .
C35 C36 C37 C38 0.9(14) . .
C35 C36 C37 Cl3 179.0(7) . .
C36 C37 C38 C39 0.9(15) . .
Cl3 C37 C38 C39 -177.1(7) . .
C35 C34 C39 C38 -1.0(13) . .
C33 C34 C39 C38 177.9(8) . .
C37 C38 C39 C34 -0.9(14) . .
