#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/34/7203411.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_7203411
loop_
_publ_author_name
'Catala, Laure'
'Wurst, Klaus'
'Amabilino, David B.'
'Veciana, Jaume'
_publ_section_title
;
 Polymorphs of a pyrazole nitronyl nitroxide and its complexes with
 metal(ii) hexafluoroacetylacetonates
;
_journal_issue                   26
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              2736
_journal_paper_doi               10.1039/b604598g
_journal_volume                  16
_journal_year                    2006
_chemical_formula_sum            'C30.5 H32.5 Cl1.5 F12 N8 Ni O8'
_chemical_formula_weight         979.03
_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                95.901(8)
_cell_angle_beta                 110.85(1)
_cell_angle_gamma                103.85(1)
_cell_formula_units_Z            2
_cell_length_a                   13.111(3)
_cell_length_b                   13.153(4)
_cell_length_c                   13.664(4)
_cell_measurement_reflns_used    4413
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      19.0
_cell_measurement_theta_min      1.0
_cell_volume                     2091.6(10)
_computing_data_collection       COLLECT
_computing_data_reduction        'DENZO and SCALEPACK'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi-and omega scan'
_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  0.1717
_diffrn_reflns_av_sigmaI/netI    0.2349
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5862
_diffrn_reflns_theta_full        19.00
_diffrn_reflns_theta_max         19.00
_diffrn_reflns_theta_min         1.63
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             994
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       0.0031(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         3347
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.2209
_refine_ls_R_factor_gt           0.0922
_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)+(0.0762P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1718
_refine_ls_wR_factor_ref         0.2124
_reflns_number_gt                1500
_reflns_number_total             3347
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b604598g.txt
_cod_data_source_block           ni
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C30.50 H32.50 Cl1.50 F12 N8 Ni O8'
_cod_database_code               7203411
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.32862(18) 0.05687(19) 0.69670(18) 0.0543(9) Uani 1 1 d . . .
O1 O 0.1764(14) -0.4445(13) 0.3739(18) 0.229(12) Uani 1 1 d . . .
O2 O -0.0744(9) -0.2755(10) 0.4005(11) 0.106(6) Uani 1 1 d . . .
O3 O 0.4488(11) 0.1611(12) 0.3467(11) 0.100(5) Uani 1 1 d . . .
O4 O 0.1289(13) 0.2694(12) 0.2450(11) 0.121(6) Uani 1 1 d . . .
O5 O 0.3979(8) 0.1999(8) 0.8076(8) 0.053(3) Uani 1 1 d . . .
O6 O 0.4875(10) 0.0656(10) 0.7024(9) 0.059(4) Uani 1 1 d . . .
O7 O 0.3508(10) -0.0242(9) 0.8183(8) 0.060(3) Uani 1 1 d . . .
O8 O 0.1767(10) 0.0593(8) 0.6942(9) 0.057(4) Uani 1 1 d . . .
N1 N 0.0854(15) -0.4252(14) 0.3630(15) 0.113(7) Uani 1 1 d . . .
N2 N -0.0385(11) -0.3452(12) 0.3687(10) 0.046(4) Uani 1 1 d . . .
N3 N 0.2659(13) -0.0922(10) 0.5952(10) 0.045(4) Uani 1 1 d . . .
N4 N 0.3381(11) -0.1490(14) 0.5931(12) 0.065(4) Uani 1 1 d . . .
H4 H 0.4119 -0.1256 0.6284 0.078 Uiso 1 1 calc . . .
N5 N 0.3668(14) 0.1933(11) 0.2880(11) 0.057(4) Uani 1 1 d . . .
N6 N 0.2154(17) 0.2454(13) 0.2434(15) 0.081(5) Uani 1 1 d . . .
N7 N 0.2989(12) 0.1391(10) 0.5712(11) 0.051(4) Uani 1 1 d . . .
N8 N 0.2217(12) 0.1925(12) 0.5502(13) 0.061(4) Uani 1 1 d . . .
H8 H 0.1856 0.2026 0.5910 0.073 Uiso 1 1 calc . . .
C1 C 0.0699(17) -0.3397(15) 0.4086(15) 0.052(5) Uiso 1 1 d . . .
C2 C -0.0306(17) -0.5032(16) 0.2837(18) 0.084(6) Uani 1 1 d . . .
C3 C -0.1112(15) -0.4439(15) 0.2855(16) 0.065(6) Uani 1 1 d . . .
C4 C 0.1657(17) -0.2560(13) 0.4836(14) 0.057(5) Uani 1 1 d . . .
C5 C 0.1641(13) -0.1560(18) 0.5291(15) 0.059(5) Uani 1 1 d . . .
H5 H 0.0967 -0.1361 0.5140 0.071 Uiso 1 1 calc . . .
C6 C 0.2825(18) -0.2454(17) 0.5301(17) 0.072(6) Uani 1 1 d . . .
H6A H 0.3164 -0.2984 0.5186 0.087 Uiso 1 1 calc . . .
C7 C 0.2878(16) 0.2108(14) 0.322(2) 0.057(5) Uani 1 1 d . . .
C8 C 0.3597(19) 0.2273(14) 0.1838(15) 0.066(6) Uani 1 1 d . . .
C9 C 0.2432(17) 0.2399(16) 0.1461(19) 0.074(6) Uani 1 1 d . . .
C10 C 0.2767(14) 0.1936(13) 0.4208(16) 0.046(5) Uani 1 1 d . . .
C11 C 0.3344(13) 0.1386(14) 0.4916(17) 0.051(5) Uani 1 1 d . . .
H11 H 0.3890 0.1066 0.4846 0.061 Uiso 1 1 calc . . .
C12 C 0.2062(15) 0.2280(15) 0.4614(18) 0.073(6) Uani 1 1 d . . .
H12 H 0.1571 0.2685 0.4319 0.088 Uiso 1 1 calc . . .
C13 C 0.4958(16) 0.2615(15) 0.8318(14) 0.055(5) Uiso 1 1 d . . .
C14 C 0.5791(15) 0.2425(15) 0.8054(16) 0.073(6) Uani 1 1 d . . .
H14 H 0.6472 0.2989 0.8274 0.087 Uiso 1 1 calc . . .
C15 C 0.5739(15) 0.1467(18) 0.7481(15) 0.052(5) Uani 1 1 d . . .
C16 C 0.2754(18) -0.0615(16) 0.8488(13) 0.058(5) Uani 1 1 d . . .
C17 C 0.1640(17) -0.0481(15) 0.8178(17) 0.061(5) Uani 1 1 d . . .
H17 H 0.1133 -0.0836 0.8461 0.073 Uiso 1 1 calc . . .
C18 C 0.1296(16) 0.0172(15) 0.7457(16) 0.051(5) Uani 1 1 d . . .
C21 C -0.017(2) -0.533(2) 0.183(2) 0.154(11) Uani 1 1 d . . .
H21A H 0.0388 -0.5728 0.1948 0.230 Uiso 1 1 calc . . .
H21B H 0.0092 -0.4692 0.1582 0.230 Uiso 1 1 calc . . .
H21C H -0.0897 -0.5779 0.1286 0.230 Uiso 1 1 calc . . .
C22 C -0.0410(17) -0.6035(19) 0.3335(18) 0.117(8) Uani 1 1 d . . .
H22A H -0.0464 -0.5859 0.4019 0.176 Uiso 1 1 calc . . .
H22B H 0.0258 -0.6276 0.3441 0.176 Uiso 1 1 calc . . .
H22C H -0.1091 -0.6599 0.2858 0.176 Uiso 1 1 calc . . .
C31 C -0.1625(18) -0.401(2) 0.1837(19) 0.142(10) Uani 1 1 d . . .
H31A H -0.1015 -0.3634 0.1646 0.214 Uiso 1 1 calc . . .
H31B H -0.2037 -0.3530 0.1970 0.214 Uiso 1 1 calc . . .
H31C H -0.2145 -0.4609 0.1255 0.214 Uiso 1 1 calc . . .
C32 C -0.2077(18) -0.4987(18) 0.313(2) 0.160(12) Uani 1 1 d . . .
H32A H -0.2580 -0.4544 0.3085 0.241 Uiso 1 1 calc . . .
H32B H -0.1776 -0.5105 0.3858 0.241 Uiso 1 1 calc . . .
H32C H -0.2501 -0.5670 0.2639 0.241 Uiso 1 1 calc . . .
C81 C 0.4600(19) 0.3285(18) 0.2177(19) 0.135(10) Uani 1 1 d . . .
H81A H 0.5311 0.3103 0.2442 0.202 Uiso 1 1 calc . . .
H81B H 0.4573 0.3779 0.2739 0.202 Uiso 1 1 calc . . .
H81C H 0.4556 0.3617 0.1568 0.202 Uiso 1 1 calc . . .
C82 C 0.3857(17) 0.1440(16) 0.1184(16) 0.102(7) Uani 1 1 d . . .
H82A H 0.4649 0.1460 0.1539 0.153 Uiso 1 1 calc . . .
H82B H 0.3724 0.1594 0.0477 0.153 Uiso 1 1 calc . . .
H82C H 0.3363 0.0735 0.1118 0.153 Uiso 1 1 calc . . .
C91 C 0.234(2) 0.339(2) 0.1041(17) 0.134(9) Uani 1 1 d . . .
H91A H 0.1556 0.3409 0.0796 0.201 Uiso 1 1 calc . . .
H91B H 0.2587 0.3403 0.0450 0.201 Uiso 1 1 calc . . .
H91C H 0.2827 0.4016 0.1606 0.201 Uiso 1 1 calc . . .
C92 C 0.153(2) 0.145(2) 0.0626(19) 0.134(10) Uani 1 1 d . . .
H92A H 0.0791 0.1582 0.0405 0.201 Uiso 1 1 calc . . .
H92B H 0.1490 0.0811 0.0929 0.201 Uiso 1 1 calc . . .
H92C H 0.1724 0.1341 0.0010 0.201 Uiso 1 1 calc . . .
C131 C 0.521(2) 0.365(2) 0.907(2) 0.084(7) Uani 1 1 d . . .
C151 C 0.6743(18) 0.138(2) 0.721(2) 0.089(7) Uani 1 1 d . . .
C161 C 0.3055(17) -0.1364(17) 0.927(2) 0.067(6) Uani 1 1 d . . .
C181 C 0.011(2) 0.033(2) 0.7319(19) 0.080(7) Uani 1 1 d . . .
F1 F 0.4699(14) 0.4263(11) 0.8557(13) 0.164(6) Uani 1 1 d . . .
F2 F 0.6240(12) 0.4202(12) 0.9477(14) 0.188(9) Uani 1 1 d . . .
F3 F 0.479(2) 0.3541(11) 0.9717(14) 0.239(12) Uani 1 1 d . . .
F4 F 0.7575(11) 0.2260(10) 0.7472(12) 0.142(6) Uani 1 1 d . . .
F5 F 0.7240(10) 0.0716(12) 0.7789(12) 0.140(6) Uani 1 1 d . . .
F6 F 0.6483(10) 0.0971(10) 0.6227(11) 0.111(4) Uani 1 1 d . . .
F7 F 0.2324(11) -0.1721(11) 0.9689(10) 0.137(5) Uani 1 1 d . . .
F8 F 0.4058(11) -0.0962(10) 1.0050(10) 0.118(5) Uani 1 1 d . . .
F9 F 0.3133(11) -0.2252(10) 0.8794(10) 0.120(4) Uani 1 1 d . . .
F10 F -0.0426(8) -0.0202(10) 0.7834(9) 0.105(4) Uani 1 1 d . . .
F11 F 0.0319(9) 0.1354(11) 0.7733(11) 0.113(4) Uani 1 1 d . . .
F12 F -0.0542(8) 0.0156(10) 0.6314(10) 0.099(4) Uani 1 1 d . . .
C19 C 0.510(3) -0.559(2) 0.521(3) 0.043(8) Uiso 0.50 1 d P . .
Cl1 Cl 0.3910(9) -0.5143(9) 0.4757(11) 0.287(6) Uani 1 1 d . . .
Cl2 Cl 0.5236(18) -0.5974(13) 0.6194(15) 0.238(9) Uani 0.50 1 d P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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
_geom_angle_publ_flag
O8 Ni1 O6 176.0(5) . . ?
O8 Ni1 O7 90.1(5) . . ?
O6 Ni1 O7 91.6(5) . . ?
O8 Ni1 O5 87.5(4) . . ?
O6 Ni1 O5 88.9(4) . . ?
O7 Ni1 O5 89.6(4) . . ?
O8 Ni1 N3 94.2(5) . . ?
O6 Ni1 N3 89.5(5) . . ?
O7 Ni1 N3 86.1(5) . . ?
O5 Ni1 N3 175.4(5) . . ?
O8 Ni1 N7 87.6(6) . . ?
O6 Ni1 N7 90.8(5) . . ?
O7 Ni1 N7 177.6(6) . . ?
O5 Ni1 N7 90.7(5) . . ?
N3 Ni1 N7 93.7(5) . . ?
C13 O5 Ni1 124.1(11) . . ?
C15 O6 Ni1 124.6(11) . . ?
C16 O7 Ni1 123.7(12) . . ?
C18 O8 Ni1 126.9(12) . . ?
O1 N1 C1 128.6(18) . . ?
O1 N1 C2 120.9(16) . . ?
C1 N1 C2 110.4(17) . . ?
O2 N2 C1 121.9(15) . . ?
O2 N2 C3 124.8(12) . . ?
C1 N2 C3 113.2(14) . . ?
C5 N3 N4 104.3(13) . . ?
C5 N3 Ni1 136.2(14) . . ?
N4 N3 Ni1 119.4(12) . . ?
C6 N4 N3 111.4(13) . . ?
C6 N4 H4 124.3 . . ?
N3 N4 H4 124.3 . . ?
O3 N5 C7 121.1(18) . . ?
O3 N5 C8 123.8(16) . . ?
C7 N5 C8 114.7(17) . . ?
O4 N6 C7 126.0(17) . . ?
O4 N6 C9 122(2) . . ?
C7 N6 C9 111.2(17) . . ?
C11 N7 N8 106.7(14) . . ?
C11 N7 Ni1 130.7(15) . . ?
N8 N7 Ni1 121.9(13) . . ?
C12 N8 N7 112.8(13) . . ?
C12 N8 H8 123.6 . . ?
N7 N8 H8 123.6 . . ?
N2 C1 N1 109.9(18) . . ?
N2 C1 C4 129.9(18) . . ?
N1 C1 C4 120.0(18) . . ?
C3 C2 C21 120(2) . . ?
C3 C2 C22 115.4(17) . . ?
C21 C2 C22 107.0(19) . . ?
C3 C2 N1 102.7(16) . . ?
C21 C2 N1 106.8(18) . . ?
C22 C2 N1 103.4(17) . . ?
C2 C3 N2 103.5(14) . . ?
C2 C3 C32 116.2(18) . . ?
N2 C3 C32 109.3(16) . . ?
C2 C3 C31 115.6(18) . . ?
N2 C3 C31 103.9(16) . . ?
C32 C3 C31 107.5(18) . . ?
C6 C4 C5 100.7(15) . . ?
C6 C4 C1 132.8(18) . . ?
C5 C4 C1 126.5(18) . . ?
N3 C5 C4 114.1(15) . . ?
N3 C5 H5 123.0 . . ?
C4 C5 H5 123.0 . . ?
N4 C6 C4 109.5(15) . . ?
N4 C6 H6A 125.2 . . ?
C4 C6 H6A 125.2 . . ?
N5 C7 N6 107(2) . . ?
N5 C7 C10 128(2) . . ?
N6 C7 C10 125.5(18) . . ?
C9 C8 N5 99.6(14) . . ?
C9 C8 C82 119.9(19) . . ?
N5 C8 C82 108.1(15) . . ?
C9 C8 C81 117.3(17) . . ?
N5 C8 C81 104.0(16) . . ?
C82 C8 C81 106.3(16) . . ?
C8 C9 C91 114.5(17) . . ?
C8 C9 N6 104.7(16) . . ?
C91 C9 N6 108.3(18) . . ?
C8 C9 C92 113.4(18) . . ?
C91 C9 C92 108.4(19) . . ?
N6 C9 C92 107.1(16) . . ?
C12 C10 C11 107.3(17) . . ?
C12 C10 C7 126(2) . . ?
C11 C10 C7 126.4(18) . . ?
N7 C11 C10 107.8(14) . . ?
N7 C11 H11 126.1 . . ?
C10 C11 H11 126.1 . . ?
N8 C12 C10 105.3(16) . . ?
N8 C12 H12 127.3 . . ?
C10 C12 H12 127.3 . . ?
O5 C13 C14 127.8(18) . . ?
O5 C13 C131 113.5(18) . . ?
C14 C13 C131 118.6(19) . . ?
C13 C14 C15 125.6(17) . . ?
C13 C14 H14 117.2 . . ?
C15 C14 H14 117.2 . . ?
O6 C15 C14 127.0(16) . . ?
O6 C15 C151 112.6(18) . . ?
C14 C15 C151 119.8(19) . . ?
O7 C16 C17 128.6(19) . . ?
O7 C16 C161 114.0(18) . . ?
C17 C16 C161 117.4(19) . . ?
C18 C17 C16 120.8(15) . . ?
C18 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?
O8 C18 C17 129.0(17) . . ?
O8 C18 C181 117.6(19) . . ?
C17 C18 C181 113.3(19) . . ?
C2 C21 H21A 109.5 . . ?
C2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C2 C22 H22A 109.5 . . ?
C2 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C2 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C3 C31 H31A 109.5 . . ?
C3 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C3 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C3 C32 H32A 109.5 . . ?
C3 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C3 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C8 C81 H81A 109.5 . . ?
C8 C81 H81B 109.5 . . ?
H81A C81 H81B 109.5 . . ?
C8 C81 H81C 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
C8 C82 H82A 109.5 . . ?
C8 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
C8 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
C9 C91 H91A 109.5 . . ?
C9 C91 H91B 109.5 . . ?
H91A C91 H91B 109.5 . . ?
C9 C91 H91C 109.5 . . ?
H91A C91 H91C 109.5 . . ?
H91B C91 H91C 109.5 . . ?
C9 C92 H92A 109.5 . . ?
C9 C92 H92B 109.5 . . ?
H92A C92 H92B 109.5 . . ?
C9 C92 H92C 109.5 . . ?
H92A C92 H92C 109.5 . . ?
H92B C92 H92C 109.5 . . ?
F3 C131 F2 113(2) . . ?
F3 C131 F1 100(2) . . ?
F2 C131 F1 104(2) . . ?
F3 C131 C13 113(2) . . ?
F2 C131 C13 115.4(19) . . ?
F1 C131 C13 110(2) . . ?
F6 C151 F4 107(2) . . ?
F6 C151 F5 106(2) . . ?
F4 C151 F5 103.7(18) . . ?
F6 C151 C15 114.9(17) . . ?
F4 C151 C15 116(2) . . ?
F5 C151 C15 108(2) . . ?
F7 C161 F8 108(2) . . ?
F7 C161 F9 102.9(17) . . ?
F8 C161 F9 103.2(17) . . ?
F7 C161 C16 116.9(17) . . ?
F8 C161 C16 113.4(17) . . ?
F9 C161 C16 111.4(19) . . ?
F12 C181 F10 110.6(19) . . ?
F12 C181 F11 107(2) . . ?
F10 C181 F11 104.7(19) . . ?
F12 C181 C18 110.7(18) . . ?
F10 C181 C18 117(2) . . ?
F11 C181 C18 106.3(17) . . ?
Cl1 C19 Cl2 114(2) 2_646 . ?
Cl1 C19 Cl1 113(2) 2_646 . ?
Cl2 C19 Cl1 112(2) . . ?
Cl1 C19 C19 65.1(19) 2_646 2_646 ?
Cl2 C19 C19 135(3) . 2_646 ?
Cl1 C19 C19 47.6(15) . 2_646 ?
C19 Cl1 C19 67(2) 2_646 . ?
C19 Cl1 Cl2 33.5(15) 2_646 2_646 ?
C19 Cl1 Cl2 90.2(14) . 2_646 ?
C19 Cl2 Cl1 32.4(13) . 2_646 ?
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 O8 1.989(11) . ?
Ni1 O6 2.031(10) . ?
Ni1 O7 2.038(12) . ?
Ni1 O5 2.068(9) . ?
Ni1 N3 2.073(12) . ?
Ni1 N7 2.090(14) . ?
O1 N1 1.241(16) . ?
O2 N2 1.233(13) . ?
O3 N5 1.285(15) . ?
O4 N6 1.254(17) . ?
O5 C13 1.248(17) . ?
O6 C15 1.262(19) . ?
O7 C16 1.222(18) . ?
O8 C18 1.186(19) . ?
N1 C1 1.32(2) . ?
N1 C2 1.55(2) . ?
N2 C1 1.308(18) . ?
N2 C3 1.490(19) . ?
N3 C5 1.323(17) . ?
N3 N4 1.346(15) . ?
N4 C6 1.330(19) . ?
N4 H4 0.8700 . ?
N5 C7 1.333(19) . ?
N5 C8 1.514(19) . ?
N6 C7 1.36(2) . ?
N6 C9 1.50(2) . ?
N7 C11 1.327(17) . ?
N7 N8 1.331(15) . ?
N8 C12 1.311(19) . ?
N8 H8 0.8700 . ?
C1 C4 1.42(2) . ?
C2 C3 1.46(2) . ?
C2 C21 1.48(2) . ?
C2 C22 1.54(3) . ?
C3 C32 1.49(2) . ?
C3 C31 1.54(3) . ?
C4 C6 1.40(2) . ?
C4 C5 1.40(2) . ?
C5 H5 0.9400 . ?
C6 H6A 0.9400 . ?
C7 C10 1.44(2) . ?
C8 C9 1.48(2) . ?
C8 C82 1.52(2) . ?
C8 C81 1.52(2) . ?
C9 C91 1.50(3) . ?
C9 C92 1.52(3) . ?
C10 C12 1.37(2) . ?
C10 C11 1.38(2) . ?
C11 H11 0.9400 . ?
C12 H12 0.9400 . ?
C13 C14 1.33(2) . ?
C13 C131 1.50(3) . ?
C14 C15 1.39(2) . ?
C14 H14 0.9400 . ?
C15 C151 1.51(2) . ?
C16 C17 1.43(2) . ?
C16 C161 1.54(2) . ?
C17 C18 1.40(2) . ?
C17 H17 0.9400 . ?
C18 C181 1.56(3) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 H22C 0.9700 . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 H31C 0.9700 . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 H32C 0.9700 . ?
C81 H81A 0.9700 . ?
C81 H81B 0.9700 . ?
C81 H81C 0.9700 . ?
C82 H82A 0.9700 . ?
C82 H82B 0.9700 . ?
C82 H82C 0.9700 . ?
C91 H91A 0.9700 . ?
C91 H91B 0.9700 . ?
C91 H91C 0.9700 . ?
C92 H92A 0.9700 . ?
C92 H92B 0.9700 . ?
C92 H92C 0.9700 . ?
C131 F3 1.21(2) . ?
C131 F2 1.25(2) . ?
C131 F1 1.28(2) . ?
C151 F6 1.28(2) . ?
C151 F4 1.30(2) . ?
C151 F5 1.36(2) . ?
C161 F7 1.302(19) . ?
C161 F8 1.302(19) . ?
C161 F9 1.322(19) . ?
C181 F12 1.30(2) . ?
C181 F10 1.303(18) . ?
C181 F11 1.33(2) . ?
C19 Cl1 1.41(3) 2_646 ?
C19 Cl2 1.45(3) . ?
C19 Cl1 1.73(3) . ?
C19 C19 1.76(7) 2_646 ?
Cl1 C19 1.41(3) 2_646 ?
Cl1 Cl2 2.40(2) 2_646 ?
Cl2 Cl1 2.40(2) 2_646 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N4 H4 O3 0.87 1.92 2.666(19) 143.6 2_656
N8 H8 O2 0.87 1.96 2.676(18) 139.4 2_556
