#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:47:51 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179263 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/83/4318355.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_4318355
loop_
_publ_author_name
'Daniel L. Reger'
'Christine A. Little'
'Mark D. Smith'
'Gary J. Long'
_publ_section_title
;
 Solid-State Structural and Magnetic Investigations of
 {M[HC(3,5-Me2pz)3]2}(BF4)2 (M = Fe, Co, Ni, Cu): Observation of a
 Thermally Induced Solid-State Phase Change Controlling an Iron(II)
 Spin-State Crossover
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4453
_journal_page_last               4460
_journal_paper_doi               10.1021/ic0112645
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C32 H44 B2 F8 N12 Ni'
_chemical_formula_weight         829.12
_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                91.130(9)
_cell_angle_beta                 104.627(5)
_cell_angle_gamma                116.302(11)
_cell_formula_units_Z            2
_cell_length_a                   10.261(4)
_cell_length_b                   11.327(4)
_cell_length_c                   18.952(7)
_cell_measurement_reflns_used    2312
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      23.246
_cell_measurement_theta_min      2.686
_cell_volume                     1888.6(12)
_computing_cell_refinement       'SAINT+ NT V6.02a (Bruker, 1998)'
_computing_data_collection       'SMART NT V5.624 (Bruker, 2000)'
_computing_data_reduction        'SAINT+ NT V6.02a'
_computing_molecular_graphics    'SHELXTL V5.1 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL V5.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      125(2)
_diffrn_measured_fraction_theta_full 0.912
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1364
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7992
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.12
_exptl_absorpt_coefficient_mu    0.596
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.079
_refine_diff_density_min         -1.433
_refine_diff_density_rms         0.169
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         7992
_refine_ls_number_restraints     164
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1275
_refine_ls_R_factor_gt           0.0897
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0900P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2051
_refine_ls_wR_factor_ref         0.2199
_reflns_number_gt                4618
_reflns_number_total             7992
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0112645_4.cif
_cod_data_source_block           ni125k
_cod_original_cell_volume        1888.4(11)
_cod_database_code               4318355
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 0.5000 1.0000 0.5000 0.0129(4) Uani 1 2 d SU . .
C1 C 0.3079(9) 0.9443(8) 0.6086(4) 0.0130(14) Uani 1 1 d U . .
H1 H 0.2466 0.9268 0.6442 0.016 Uiso 1 1 calc R . .
C11 C 0.0757(9) 0.7517(8) 0.5265(4) 0.0143(18) Uani 1 1 d U . .
C12 C 0.0321(10) 0.6975(9) 0.4535(4) 0.0195(19) Uani 1 1 d U . .
H12 H -0.0617 0.6241 0.4267 0.023 Uiso 1 1 calc R . .
C13 C 0.1550(10) 0.7733(9) 0.4272(4) 0.0172(18) Uani 1 1 d U . .
C14 C -0.0142(10) 0.7074(9) 0.5821(4) 0.022(2) Uani 1 1 d U . .
H14A H 0.0205 0.6531 0.6135 0.034 Uiso 1 1 calc R . .
H14B H -0.1225 0.6546 0.5558 0.034 Uiso 1 1 calc R . .
H14C H 0.0014 0.7859 0.6127 0.034 Uiso 1 1 calc R . .
C15 C 0.1638(11) 0.7584(10) 0.3496(4) 0.032(2) Uani 1 1 d U . .
H15A H 0.1186 0.8079 0.3198 0.048 Uiso 1 1 calc R . .
H15B H 0.1082 0.6640 0.3282 0.048 Uiso 1 1 calc R . .
H15C H 0.2704 0.7937 0.3505 0.048 Uiso 1 1 calc R . .
C21 C 0.4978(10) 0.9176(8) 0.7134(4) 0.0159(18) Uani 1 1 d U . .
C22 C 0.6270(10) 0.9064(9) 0.7161(4) 0.0197(19) Uani 1 1 d U . .
H22 H 0.6937 0.8985 0.7585 0.024 Uiso 1 1 calc R . .
C23 C 0.6419(10) 0.9089(9) 0.6452(4) 0.0169(17) Uani 1 1 d U . .
C24 C 0.4259(10) 0.9226(10) 0.7722(4) 0.026(2) Uani 1 1 d U . .
H24A H 0.4492 1.0149 0.7867 0.040 Uiso 1 1 calc R . .
H24B H 0.4660 0.8888 0.8151 0.040 Uiso 1 1 calc R . .
H24C H 0.3156 0.8675 0.7532 0.040 Uiso 1 1 calc R . .
C25 C 0.7590(12) 0.8905(11) 0.6186(5) 0.038(3) Uani 1 1 d U . .
H25A H 0.7198 0.7962 0.6001 0.057 Uiso 1 1 calc R . .
H25B H 0.8522 0.9202 0.6596 0.057 Uiso 1 1 calc R . .
H25C H 0.7811 0.9433 0.5789 0.057 Uiso 1 1 calc R . .
C31 C 0.3053(10) 1.1682(8) 0.6144(4) 0.0181(17) Uani 1 1 d U . .
C32 C 0.3863(10) 1.2839(9) 0.5893(4) 0.0211(18) Uani 1 1 d U . .
H32 H 0.3791 1.3642 0.5947 0.025 Uiso 1 1 calc R . .
C33 C 0.4797(10) 1.2635(9) 0.5549(4) 0.0218(18) Uani 1 1 d U . .
C34 C 0.1859(11) 1.1278(9) 0.6542(5) 0.029(2) Uani 1 1 d U . .
H34A H 0.0905 1.0552 0.6228 0.043 Uiso 1 1 calc R . .
H34B H 0.1697 1.2042 0.6654 0.043 Uiso 1 1 calc R . .
H34C H 0.2195 1.0976 0.7002 0.043 Uiso 1 1 calc R . .
C35 C 0.5874(11) 1.3546(9) 0.5191(5) 0.035(2) Uani 1 1 d U . .
H35A H 0.6895 1.3975 0.5542 0.052 Uiso 1 1 calc R . .
H35B H 0.5572 1.4227 0.5027 0.052 Uiso 1 1 calc R . .
H35C H 0.5876 1.3045 0.4764 0.052 Uiso 1 1 calc R . .
N31 N 0.4574(8) 1.1361(7) 0.5557(3) 0.0204(15) Uani 1 1 d U . .
N32 N 0.3532(8) 1.0786(7) 0.5941(3) 0.0158(13) Uani 1 1 d U . .
N21 N 0.5322(8) 0.9257(7) 0.5990(3) 0.0203(15) Uani 1 1 d U . .
N22 N 0.4415(8) 0.9276(7) 0.6417(3) 0.0159(15) Uani 1 1 d U . .
N11 N 0.2646(8) 0.8683(7) 0.4802(3) 0.0163(15) Uani 1 1 d U . .
N12 N 0.2138(8) 0.8503(7) 0.5405(3) 0.0140(15) Uani 1 1 d U . .
Ni2 Ni 0.0000 0.5000 0.0000 0.0138(4) Uani 1 2 d SU . .
C2 C 0.2478(9) 0.4527(8) 0.1068(4) 0.0118(14) Uani 1 1 d U . .
H2 H 0.3275 0.4361 0.1410 0.014 Uiso 1 1 calc R . .
C41 C 0.2007(10) 0.2449(8) 0.0289(4) 0.0163(18) Uani 1 1 d U . .
C42 C 0.0975(11) 0.1736(9) -0.0383(4) 0.025(2) Uani 1 1 d U . .
H42 H 0.0869 0.0950 -0.0635 0.030 Uiso 1 1 calc R . .
C43 C 0.0115(10) 0.2413(8) -0.0618(4) 0.0198(19) Uani 1 1 d U . .
C44 C 0.3210(11) 0.2176(10) 0.0808(4) 0.030(2) Uani 1 1 d U . .
H44A H 0.4218 0.2924 0.0868 0.045 Uiso 1 1 calc R . .
H44B H 0.3169 0.1357 0.0600 0.045 Uiso 1 1 calc R . .
H44C H 0.3016 0.2073 0.1289 0.045 Uiso 1 1 calc R . .
C45 C -0.1128(11) 0.2030(10) -0.1326(4) 0.037(3) Uani 1 1 d U . .
H45A H -0.0839 0.2742 -0.1630 0.055 Uiso 1 1 calc R . .
H45B H -0.2067 0.1895 -0.1220 0.055 Uiso 1 1 calc R . .
H45C H -0.1291 0.1203 -0.1593 0.055 Uiso 1 1 calc R . .
C51 C 0.1480(9) 0.4326(8) 0.2167(4) 0.0131(16) Uani 1 1 d U . .
C52 C 0.0196(10) 0.4352(9) 0.2245(4) 0.022(2) Uani 1 1 d U . .
H52 H -0.0129 0.4248 0.2677 0.027 Uiso 1 1 calc R . .
C53 C -0.0528(10) 0.4558(9) 0.1581(4) 0.0187(18) Uani 1 1 d U . .
C54 C 0.2707(10) 0.4164(9) 0.2698(4) 0.023(2) Uani 1 1 d U . .
H54A H 0.3696 0.4887 0.2702 0.034 Uiso 1 1 calc R . .
H54B H 0.2653 0.3306 0.2550 0.034 Uiso 1 1 calc R . .
H54C H 0.2582 0.4193 0.3193 0.034 Uiso 1 1 calc R . .
C55 C -0.1992(10) 0.4689(10) 0.1398(5) 0.034(2) Uani 1 1 d U . .
H55A H -0.1922 0.5315 0.1788 0.051 Uiso 1 1 calc R . .
H55B H -0.2856 0.3816 0.1365 0.051 Uiso 1 1 calc R . .
H55C H -0.2135 0.5020 0.0926 0.051 Uiso 1 1 calc R . .
C61 C 0.4718(9) 0.6739(8) 0.1054(4) 0.0191(17) Uani 1 1 d U . .
C62 C 0.4817(10) 0.7807(9) 0.0706(4) 0.0237(19) Uani 1 1 d U . .
H62 H 0.5715 0.8607 0.0740 0.028 Uiso 1 1 calc R . .
C63 C 0.3310(10) 0.7484(9) 0.0282(5) 0.0223(18) Uani 1 1 d U . .
C64 C 0.5914(10) 0.6528(10) 0.1566(5) 0.034(2) Uani 1 1 d U . .
H64A H 0.6892 0.7075 0.1475 0.051 Uiso 1 1 calc R . .
H64B H 0.5668 0.5586 0.1487 0.051 Uiso 1 1 calc R . .
H64C H 0.5979 0.6783 0.2076 0.051 Uiso 1 1 calc R . .
C65 C 0.2812(11) 0.8305(9) -0.0223(5) 0.036(3) Uani 1 1 d U . .
H65A H 0.3217 0.8377 -0.0646 0.055 Uiso 1 1 calc R . .
H65B H 0.3194 0.9197 0.0044 0.055 Uiso 1 1 calc R . .
H65C H 0.1699 0.7878 -0.0399 0.055 Uiso 1 1 calc R . .
N41 N 0.0588(8) 0.3485(7) -0.0131(3) 0.0187(15) Uani 1 1 d U . .
N42 N 0.1728(7) 0.3501(7) 0.0436(3) 0.0128(14) Uani 1 1 d U . .
N51 N 0.0216(8) 0.4653(7) 0.1085(3) 0.0193(15) Uani 1 1 d U . .
N52 N 0.1431(8) 0.4490(7) 0.1451(3) 0.0143(14) Uani 1 1 d U . .
N61 N 0.2354(8) 0.6289(7) 0.0365(3) 0.0195(15) Uani 1 1 d U . .
N62 N 0.3226(8) 0.5830(7) 0.0844(3) 0.0162(14) Uani 1 1 d U . .
B1 B 0.9414(12) 0.0591(10) 0.1952(5) 0.0239(19) Uani 1 1 d U . .
F1 F 0.8066(6) 0.0149(5) 0.1444(3) 0.0438(16) Uani 1 1 d U . .
F2 F 0.9512(6) 0.1313(5) 0.2577(2) 0.0270(12) Uani 1 1 d U . .
F3 F 0.9634(6) -0.0535(5) 0.2149(3) 0.0368(13) Uani 1 1 d U . .
F4 F 1.0600(7) 0.1365(6) 0.1666(3) 0.0466(16) Uani 1 1 d U . .
B2 B 0.6705(12) 0.4396(11) 0.3032(5) 0.0210(18) Uani 1 1 d U . .
F5 F 0.5562(6) 0.3798(5) 0.2364(2) 0.0265(13) Uani 1 1 d U . .
F6 F 0.6044(6) 0.4306(6) 0.3603(2) 0.0385(15) Uani 1 1 d U . .
F7 F 0.7572(6) 0.3719(5) 0.3182(3) 0.0375(14) Uani 1 1 d U . .
F8 F 0.7603(6) 0.5694(5) 0.2993(2) 0.0357(14) Uani 1 1 d U . .
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'
B B 0.0013 0.0007 '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'
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'
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
N21 Ni1 N21 180.00(17) 2_676 . ?
N21 Ni1 N31 93.0(3) 2_676 . ?
N21 Ni1 N31 87.0(3) . . ?
N21 Ni1 N31 87.0(3) 2_676 2_676 ?
N21 Ni1 N31 93.0(3) . 2_676 ?
N31 Ni1 N31 180.000(3) . 2_676 ?
N21 Ni1 N11 86.2(3) 2_676 2_676 ?
N21 Ni1 N11 93.8(3) . 2_676 ?
N31 Ni1 N11 94.7(3) . 2_676 ?
N31 Ni1 N11 85.3(3) 2_676 2_676 ?
N21 Ni1 N11 93.8(3) 2_676 . ?
N21 Ni1 N11 86.2(3) . . ?
N31 Ni1 N11 85.3(3) . . ?
N31 Ni1 N11 94.7(3) 2_676 . ?
N11 Ni1 N11 180.0(3) 2_676 . ?
N32 C1 N22 109.8(7) . . ?
N32 C1 N12 110.3(6) . . ?
N22 C1 N12 111.0(7) . . ?
N12 C11 C12 106.7(8) . . ?
N12 C11 C14 125.3(7) . . ?
C12 C11 C14 128.0(8) . . ?
C11 C12 C13 105.5(7) . . ?
N11 C13 C12 109.9(7) . . ?
N11 C13 C15 123.1(8) . . ?
C12 C13 C15 127.0(7) . . ?
N22 C21 C22 105.1(7) . . ?
N22 C21 C24 123.3(8) . . ?
C22 C21 C24 131.5(7) . . ?
C21 C22 C23 107.2(7) . . ?
N21 C23 C22 111.2(8) . . ?
N21 C23 C25 121.1(7) . . ?
C22 C23 C25 127.6(8) . . ?
C32 C31 N32 105.4(8) . . ?
C32 C31 C34 133.5(8) . . ?
N32 C31 C34 121.0(8) . . ?
C31 C32 C33 108.4(8) . . ?
N31 C33 C32 109.8(8) . . ?
N31 C33 C35 120.3(8) . . ?
C32 C33 C35 129.9(9) . . ?
C33 N31 N32 105.9(7) . . ?
C33 N31 Ni1 138.3(6) . . ?
N32 N31 Ni1 114.3(5) . . ?
N31 N32 C31 110.4(7) . . ?
N31 N32 C1 121.0(7) . . ?
C31 N32 C1 128.6(7) . . ?
C23 N21 N22 104.3(6) . . ?
C23 N21 Ni1 137.4(6) . . ?
N22 N21 Ni1 115.2(5) . . ?
C21 N22 N21 112.0(7) . . ?
C21 N22 C1 128.4(7) . . ?
N21 N22 C1 119.5(6) . . ?
C13 N11 N12 105.6(7) . . ?
C13 N11 Ni1 136.7(6) . . ?
N12 N11 Ni1 115.7(5) . . ?
C11 N12 N11 112.4(6) . . ?
C11 N12 C1 128.4(7) . . ?
N11 N12 C1 119.0(7) . . ?
N51 Ni2 N51 180.0(4) . 2_565 ?
N51 Ni2 N41 94.5(3) . 2_565 ?
N51 Ni2 N41 85.5(3) 2_565 2_565 ?
N51 Ni2 N41 85.5(3) . . ?
N51 Ni2 N41 94.5(3) 2_565 . ?
N41 Ni2 N41 180.0(3) 2_565 . ?
N51 Ni2 N61 94.1(3) . 2_565 ?
N51 Ni2 N61 85.9(3) 2_565 2_565 ?
N41 Ni2 N61 86.0(3) 2_565 2_565 ?
N41 Ni2 N61 94.0(3) . 2_565 ?
N51 Ni2 N61 85.9(3) . . ?
N51 Ni2 N61 94.1(3) 2_565 . ?
N41 Ni2 N61 94.0(3) 2_565 . ?
N41 Ni2 N61 86.0(3) . . ?
N61 Ni2 N61 180.0 2_565 . ?
N52 C2 N42 110.9(7) . . ?
N52 C2 N62 111.2(7) . . ?
N42 C2 N62 110.2(6) . . ?
N42 C41 C42 106.4(7) . . ?
N42 C41 C44 124.0(7) . . ?
C42 C41 C44 129.7(8) . . ?
C41 C42 C43 106.0(7) . . ?
N41 C43 C42 110.6(7) . . ?
N41 C43 C45 123.7(8) . . ?
C42 C43 C45 125.7(7) . . ?
N52 C51 C52 104.5(7) . . ?
N52 C51 C54 124.1(8) . . ?
C52 C51 C54 131.5(8) . . ?
C53 C52 C51 107.0(7) . . ?
N51 C53 C52 111.6(8) . . ?
N51 C53 C55 121.8(7) . . ?
C52 C53 C55 126.6(8) . . ?
N62 C61 C62 106.3(7) . . ?
N62 C61 C64 123.6(8) . . ?
C62 C61 C64 130.2(8) . . ?
C61 C62 C63 106.6(8) . . ?
N61 C63 C62 110.0(8) . . ?
N61 C63 C65 122.3(8) . . ?
C62 C63 C65 127.6(8) . . ?
C43 N41 N42 106.5(7) . . ?
C43 N41 Ni2 137.6(6) . . ?
N42 N41 Ni2 115.8(5) . . ?
N41 N42 C41 110.5(6) . . ?
N41 N42 C2 121.0(7) . . ?
C41 N42 C2 128.5(7) . . ?
C53 N51 N52 104.1(6) . . ?
C53 N51 Ni2 137.5(6) . . ?
N52 N51 Ni2 118.3(5) . . ?
N51 N52 C51 112.8(7) . . ?
N51 N52 C2 118.7(6) . . ?
C51 N52 C2 128.6(7) . . ?
C63 N61 N62 105.7(7) . . ?
C63 N61 Ni2 138.2(6) . . ?
N62 N61 Ni2 116.0(5) . . ?
C61 N62 N61 111.4(7) . . ?
C61 N62 C2 129.4(7) . . ?
N61 N62 C2 119.1(6) . . ?
F1 B1 F2 112.2(9) . . ?
F1 B1 F4 111.3(7) . . ?
F2 B1 F4 109.5(7) . . ?
F1 B1 F3 108.3(8) . . ?
F2 B1 F3 109.4(7) . . ?
F4 B1 F3 105.9(9) . . ?
F8 B2 F7 110.2(8) . . ?
F8 B2 F5 109.4(8) . . ?
F7 B2 F5 109.9(7) . . ?
F8 B2 F6 110.5(8) . . ?
F7 B2 F6 107.5(8) . . ?
F5 B2 F6 109.3(8) . . ?
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 N21 2.082(7) 2_676 ?
Ni1 N21 2.082(7) . ?
Ni1 N31 2.109(7) . ?
Ni1 N31 2.109(7) 2_676 ?
Ni1 N11 2.128(7) 2_676 ?
Ni1 N11 2.128(7) . ?
C1 N32 1.435(10) . ?
C1 N22 1.452(10) . ?
C1 N12 1.461(10) . ?
C11 N12 1.312(10) . ?
C11 C12 1.380(11) . ?
C11 C14 1.520(12) . ?
C12 C13 1.396(12) . ?
C13 N11 1.321(10) . ?
C13 C15 1.505(12) . ?
C21 N22 1.363(10) . ?
C21 C22 1.376(12) . ?
C21 C24 1.495(11) . ?
C22 C23 1.389(12) . ?
C23 N21 1.330(11) . ?
C23 C25 1.505(12) . ?
C31 C32 1.376(12) . ?
C31 N32 1.393(10) . ?
C31 C34 1.504(12) . ?
C32 C33 1.379(12) . ?
C33 N31 1.358(11) . ?
C33 C35 1.464(12) . ?
N31 N32 1.376(9) . ?
N21 N22 1.385(9) . ?
N11 N12 1.355(9) . ?
Ni2 N51 2.076(6) . ?
Ni2 N51 2.076(6) 2_565 ?
Ni2 N41 2.085(7) 2_565 ?
Ni2 N41 2.085(7) . ?
Ni2 N61 2.106(7) 2_565 ?
Ni2 N61 2.106(7) . ?
C2 N52 1.428(10) . ?
C2 N42 1.437(9) . ?
C2 N62 1.461(10) . ?
C41 N42 1.382(10) . ?
C41 C42 1.385(11) . ?
C41 C44 1.523(12) . ?
C42 C43 1.406(13) . ?
C43 N41 1.330(10) . ?
C43 C45 1.497(11) . ?
C51 N52 1.365(10) . ?
C51 C52 1.375(12) . ?
C51 C54 1.484(11) . ?
C52 C53 1.372(12) . ?
C53 N51 1.330(10) . ?
C53 C55 1.528(12) . ?
C61 N62 1.357(10) . ?
C61 C62 1.365(12) . ?
C61 C64 1.474(12) . ?
C62 C63 1.425(12) . ?
C63 N61 1.316(11) . ?
C63 C65 1.501(12) . ?
N41 N42 1.366(9) . ?
N51 N52 1.357(9) . ?
N61 N62 1.384(9) . ?
B1 F1 1.336(11) . ?
B1 F2 1.382(12) . ?
B1 F4 1.396(12) . ?
B1 F3 1.432(12) . ?
B2 F8 1.363(12) . ?
B2 F7 1.394(12) . ?
B2 F5 1.397(11) . ?
B2 F6 1.397(11) . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N12 C11 C12 C13 -0.5(10) . . . . ?
C14 C11 C12 C13 -179.6(9) . . . . ?
C11 C12 C13 N11 -0.9(10) . . . . ?
C11 C12 C13 C15 -177.7(9) . . . . ?
N22 C21 C22 C23 -0.6(10) . . . . ?
C24 C21 C22 C23 -179.0(9) . . . . ?
C21 C22 C23 N21 2.2(11) . . . . ?
C21 C22 C23 C25 -175.5(9) . . . . ?
N32 C31 C32 C33 0.0(9) . . . . ?
C34 C31 C32 C33 -178.7(9) . . . . ?
C31 C32 C33 N31 1.7(10) . . . . ?
C31 C32 C33 C35 179.9(9) . . . . ?
C32 C33 N31 N32 -2.7(9) . . . . ?
C35 C33 N31 N32 178.9(7) . . . . ?
C32 C33 N31 Ni1 161.9(7) . . . . ?
C35 C33 N31 Ni1 -16.5(13) . . . . ?
N21 Ni1 N31 C33 -33.6(9) 2_676 . . . ?
N21 Ni1 N31 C33 146.4(9) . . . . ?
N31 Ni1 N31 C33 151(100) 2_676 . . . ?
N11 Ni1 N31 C33 52.8(9) 2_676 . . . ?
N11 Ni1 N31 C33 -127.2(9) . . . . ?
N21 Ni1 N31 N32 130.1(5) 2_676 . . . ?
N21 Ni1 N31 N32 -49.9(5) . . . . ?
N31 Ni1 N31 N32 -45(100) 2_676 . . . ?
N11 Ni1 N31 N32 -143.5(5) 2_676 . . . ?
N11 Ni1 N31 N32 36.5(5) . . . . ?
C33 N31 N32 C31 2.7(8) . . . . ?
Ni1 N31 N32 C31 -166.1(5) . . . . y
C33 N31 N32 C1 -177.2(6) . . . . ?
Ni1 N31 N32 C1 14.0(8) . . . . ?
C32 C31 N32 N31 -1.7(9) . . . . ?
C34 C31 N32 N31 177.2(7) . . . . ?
C32 C31 N32 C1 178.1(7) . . . . ?
C34 C31 N32 C1 -2.9(12) . . . . ?
N22 C1 N32 N31 51.7(9) . . . . ?
N12 C1 N32 N31 -70.9(9) . . . . ?
N22 C1 N32 C31 -128.1(8) . . . . ?
N12 C1 N32 C31 109.2(9) . . . . ?
C22 C23 N21 N22 -2.8(10) . . . . ?
C25 C23 N21 N22 175.1(8) . . . . ?
C22 C23 N21 Ni1 155.1(6) . . . . ?
C25 C23 N21 Ni1 -27.1(14) . . . . ?
N21 Ni1 N21 C23 119(100) 2_676 . . . ?
N31 Ni1 N21 C23 -121.9(9) . . . . ?
N31 Ni1 N21 C23 58.1(9) 2_676 . . . ?
N11 Ni1 N21 C23 -27.4(9) 2_676 . . . ?
N11 Ni1 N21 C23 152.6(9) . . . . ?
N21 Ni1 N21 N22 -85(100) 2_676 . . . ?
N31 Ni1 N21 N22 34.3(6) . . . . ?
N31 Ni1 N21 N22 -145.7(6) 2_676 . . . ?
N11 Ni1 N21 N22 128.8(6) 2_676 . . . ?
N11 Ni1 N21 N22 -51.2(6) . . . . ?
C22 C21 N22 N21 -1.1(9) . . . . ?
C24 C21 N22 N21 177.4(8) . . . . ?
C22 C21 N22 C1 -178.6(8) . . . . ?
C24 C21 N22 C1 -0.1(13) . . . . ?
C23 N21 N22 C21 2.4(9) . . . . ?
Ni1 N21 N22 C21 -161.2(5) . . . . y
C23 N21 N22 C1 -179.8(7) . . . . ?
Ni1 N21 N22 C1 16.6(9) . . . . ?
N32 C1 N22 C21 105.7(9) . . . . ?
N12 C1 N22 C21 -132.1(8) . . . . ?
N32 C1 N22 N21 -71.6(9) . . . . ?
N12 C1 N22 N21 50.6(10) . . . . ?
C12 C13 N11 N12 1.9(10) . . . . ?
C15 C13 N11 N12 178.8(8) . . . . ?
C12 C13 N11 Ni1 164.3(7) . . . . ?
C15 C13 N11 Ni1 -18.8(14) . . . . ?
N21 Ni1 N11 C13 53.9(9) 2_676 . . . ?
N21 Ni1 N11 C13 -126.1(9) . . . . ?
N31 Ni1 N11 C13 146.6(9) . . . . ?
N31 Ni1 N11 C13 -33.4(9) 2_676 . . . ?
N11 Ni1 N11 C13 115(87) 2_676 . . . ?
N21 Ni1 N11 N12 -145.0(6) 2_676 . . . ?
N21 Ni1 N11 N12 35.0(6) . . . . ?
N31 Ni1 N11 N12 -52.2(6) . . . . ?
N31 Ni1 N11 N12 127.8(6) 2_676 . . . ?
N11 Ni1 N11 N12 -84(87) 2_676 . . . ?
C12 C11 N12 N11 1.7(10) . . . . ?
C14 C11 N12 N11 -179.2(8) . . . . ?
C12 C11 N12 C1 176.3(8) . . . . ?
C14 C11 N12 C1 -4.5(14) . . . . ?
C13 N11 N12 C11 -2.3(10) . . . . ?
Ni1 N11 N12 C11 -169.0(6) . . . . y
C13 N11 N12 C1 -177.5(8) . . . . ?
Ni1 N11 N12 C1 15.8(9) . . . . ?
N32 C1 N12 C11 -123.3(9) . . . . ?
N22 C1 N12 C11 114.8(9) . . . . ?
N32 C1 N12 N11 51.0(10) . . . . ?
N22 C1 N12 N11 -70.9(9) . . . . ?
N42 C41 C42 C43 0.5(10) . . . . ?
C44 C41 C42 C43 178.9(9) . . . . ?
C41 C42 C43 N41 0.8(10) . . . . ?
C41 C42 C43 C45 178.7(9) . . . . ?
N52 C51 C52 C53 -1.2(10) . . . . ?
C54 C51 C52 C53 178.7(9) . . . . ?
C51 C52 C53 N51 0.5(11) . . . . ?
C51 C52 C53 C55 -178.7(9) . . . . ?
N62 C61 C62 C63 0.2(9) . . . . ?
C64 C61 C62 C63 -179.5(9) . . . . ?
C61 C62 C63 N61 -0.3(10) . . . . ?
C61 C62 C63 C65 -177.6(9) . . . . ?
C42 C43 N41 N42 -1.7(10) . . . . ?
C45 C43 N41 N42 -179.7(8) . . . . ?
C42 C43 N41 Ni2 -178.4(7) . . . . ?
C45 C43 N41 Ni2 3.6(15) . . . . ?
N51 Ni2 N41 C43 134.8(9) . . . . ?
N51 Ni2 N41 C43 -45.2(9) 2_565 . . . ?
N41 Ni2 N41 C43 119(100) 2_565 . . . ?
N61 Ni2 N41 C43 41.0(9) 2_565 . . . ?
N61 Ni2 N41 C43 -139.0(9) . . . . ?
N51 Ni2 N41 N42 -41.6(6) . . . . ?
N51 Ni2 N41 N42 138.4(6) 2_565 . . . ?
N41 Ni2 N41 N42 -57(100) 2_565 . . . ?
N61 Ni2 N41 N42 -135.4(6) 2_565 . . . ?
N61 Ni2 N41 N42 44.6(6) . . . . ?
C43 N41 N42 C41 2.1(9) . . . . ?
Ni2 N41 N42 C41 179.6(5) . . . . y
C43 N41 N42 C2 -178.8(7) . . . . ?
Ni2 N41 N42 C2 -1.4(9) . . . . ?
C42 C41 N42 N41 -1.6(10) . . . . ?
C44 C41 N42 N41 179.9(8) . . . . ?
C42 C41 N42 C2 179.4(8) . . . . ?
C44 C41 N42 C2 1.0(14) . . . . ?
N52 C2 N42 N41 62.3(9) . . . . ?
N62 C2 N42 N41 -61.3(10) . . . . ?
N52 C2 N42 C41 -118.8(9) . . . . ?
N62 C2 N42 C41 117.6(9) . . . . ?
C52 C53 N51 N52 0.5(10) . . . . ?
C55 C53 N51 N52 179.8(8) . . . . ?
C52 C53 N51 Ni2 -177.8(6) . . . . ?
C55 C53 N51 Ni2 1.4(15) . . . . ?
N51 Ni2 N51 C53 -154(100) 2_565 . . . ?
N41 Ni2 N51 C53 42.3(9) 2_565 . . . ?
N41 Ni2 N51 C53 -137.7(9) . . . . ?
N61 Ni2 N51 C53 -44.1(9) 2_565 . . . ?
N61 Ni2 N51 C53 135.9(9) . . . . ?
N51 Ni2 N51 N52 28(100) 2_565 . . . ?
N41 Ni2 N51 N52 -135.9(6) 2_565 . . . ?
N41 Ni2 N51 N52 44.1(6) . . . . ?
N61 Ni2 N51 N52 137.7(6) 2_565 . . . ?
N61 Ni2 N51 N52 -42.3(6) . . . . ?
C53 N51 N52 C51 -1.4(9) . . . . ?
Ni2 N51 N52 C51 177.4(5) . . . . y
C53 N51 N52 C2 179.5(8) . . . . ?
Ni2 N51 N52 C2 -1.8(9) . . . . ?
C52 C51 N52 N51 1.7(9) . . . . ?
C54 C51 N52 N51 -178.3(7) . . . . ?
C52 C51 N52 C2 -179.3(8) . . . . ?
C54 C51 N52 C2 0.7(13) . . . . ?
N42 C2 N52 N51 -59.7(9) . . . . ?
N62 C2 N52 N51 63.3(9) . . . . ?
N42 C2 N52 C51 121.3(8) . . . . ?
N62 C2 N52 C51 -115.7(8) . . . . ?
C62 C63 N61 N62 0.3(10) . . . . ?
C65 C63 N61 N62 177.7(8) . . . . ?
C62 C63 N61 Ni2 178.8(6) . . . . ?
C65 C63 N61 Ni2 -3.8(15) . . . . ?
N51 Ni2 N61 C63 -135.9(9) . . . . ?
N51 Ni2 N61 C63 44.1(9) 2_565 . . . ?
N41 Ni2 N61 C63 -41.6(9) 2_565 . . . ?
N41 Ni2 N61 C63 138.4(9) . . . . ?
N61 Ni2 N61 C63 -123(100) 2_565 . . . ?
N51 Ni2 N61 N62 42.5(5) . . . . ?
N51 Ni2 N61 N62 -137.5(5) 2_565 . . . ?
N41 Ni2 N61 N62 136.8(5) 2_565 . . . ?
N41 Ni2 N61 N62 -43.2(5) . . . . ?
N61 Ni2 N61 N62 55(100) 2_565 . . . ?
C62 C61 N62 N61 0.0(9) . . . . ?
C64 C61 N62 N61 179.6(8) . . . . ?
C62 C61 N62 C2 -178.0(7) . . . . ?
C64 C61 N62 C2 1.7(13) . . . . ?
C63 N61 N62 C61 -0.2(9) . . . . ?
Ni2 N61 N62 C61 -179.1(5) . . . . y
C63 N61 N62 C2 178.1(7) . . . . ?
Ni2 N61 N62 C2 -0.8(8) . . . . ?
N52 C2 N62 C61 116.4(9) . . . . ?
N42 C2 N62 C61 -120.2(8) . . . . ?
N52 C2 N62 N61 -61.4(8) . . . . ?
N42 C2 N62 N61 61.9(9) . . . . ?
