#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/84/4338479.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_4338479
loop_
_publ_author_name
'López-Banet, Luisa'
'Santana, M. Dolores'
'Piernas, María José'
'García, Gabriel'
'Cerezo, Javier'
'Requena, Alberto'
'Zúñiga, José'
'Pérez, José'
'García, Luís'
_publ_section_title
;
 Structure and Spectroscopic Properties of Nickel Benzazolate Complexes
 with Hydrotris(pyrazolyl)borate Ligand.
;
_journal_issue                   11
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5502
_journal_page_last               5514
_journal_paper_doi               10.1021/ic5001655
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C29.5 H33 B N7 Ni O2.5'
_chemical_formula_weight         595.15
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_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                66.678(2)
_cell_angle_beta                 68.761(2)
_cell_angle_gamma                74.156(2)
_cell_formula_units_Z            2
_cell_length_a                   11.1853(13)
_cell_length_b                   11.2043(13)
_cell_length_c                   13.4087(15)
_cell_measurement_temperature    100(2)
_cell_volume                     1421.7(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.000
_diffrn_measured_fraction_theta_max 0.917
_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  0.0195
_diffrn_reflns_av_sigmaI/netI    0.0223
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17753
_diffrn_reflns_theta_full        0.50
_diffrn_reflns_theta_max         28.64
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.725
_exptl_absorpt_correction_T_max  0.8173
_exptl_absorpt_correction_T_min  0.7958
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.787
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.520
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         6681
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.520
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0421
_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)+(0.1525P)²+7.7006P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1227
_refine_ls_wR_factor_ref         0.1247
_reflns_number_gt                6340
_reflns_number_total             6681
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5001655_si_002.cif
_cod_data_source_block           lu79as
_cod_depositor_comments
'Adding full bibliography for 4338477--4338479.cif.'
_cod_original_formula_sum        'C29.50 H33 B N7 Ni O2.50'
_cod_database_code               4338479
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
Ni1 Ni 0.56368(2) 0.52740(2) 0.723773(19) 0.01120(9) Uani 1 1 d .
O2 O 0.97334(13) 0.48335(14) 0.63476(13) 0.0171(3) Uani 1 1 d .
O1 O 0.59823(14) 0.70806(14) 0.65378(14) 0.0200(3) Uani 1 1 d .
N5 N 0.36058(15) 0.58434(16) 0.76216(13) 0.0130(3) Uani 1 1 d .
N3 N 0.54139(15) 0.40178(16) 0.66007(13) 0.0131(3) Uani 1 1 d .
N6 N 0.29162(15) 0.47992(16) 0.81319(13) 0.0135(3) Uani 1 1 d .
N7 N 0.76128(16) 0.46820(16) 0.68958(14) 0.0135(3) Uani 1 1 d .
C27 C 0.7945(2) 0.2197(2) 0.73520(18) 0.0188(4) Uani 1 1 d .
H27 H 0.7057 0.2093 0.7612 0.023 Uiso 1 1 calc R
C28 C 0.83257(19) 0.34202(19) 0.69855(16) 0.0146(4) Uani 1 1 d .
C23 C 0.96325(19) 0.35341(19) 0.66298(17) 0.0163(4) Uani 1 1 d .
C24 C 1.0632(2) 0.2498(2) 0.65692(19) 0.0228(4) Uani 1 1 d .
H24 H 1.1518 0.2610 0.6303 0.027 Uiso 1 1 calc R
C21 C 0.82556(18) 0.68434(19) 0.63550(16) 0.0144(3) Uani 1 1 d .
C26 C 0.8940(2) 0.1130(2) 0.73180(19) 0.0222(4) Uani 1 1 d .
H26 H 0.8720 0.0276 0.7569 0.027 Uiso 1 1 calc R
C19 C 0.9124(2) 0.8774(2) 0.60089(18) 0.0210(4) Uani 1 1 d .
H19 H 0.9818 0.9171 0.5928 0.025 Uiso 1 1 calc R
C20 C 0.92904(19) 0.7450(2) 0.62010(17) 0.0180(4) Uani 1 1 d .
H20 H 1.0114 0.6934 0.6231 0.022 Uiso 1 1 calc R
C18 C 0.7915(2) 0.9532(2) 0.59335(18) 0.0214(4) Uani 1 1 d .
H18 H 0.7801 1.0453 0.5777 0.026 Uiso 1 1 calc R
C22 C 0.84709(18) 0.54603(19) 0.65393(16) 0.0135(3) Uani 1 1 d .
C25 C 1.0250(2) 0.1279(2) 0.6925(2) 0.0244(4) Uani 1 1 d .
H25 H 1.0894 0.0528 0.6901 0.029 Uiso 1 1 calc R
C12 C 0.14710(19) 0.6609(2) 0.79445(17) 0.0178(4) Uani 1 1 d .
H12 H 0.0677 0.7199 0.7972 0.021 Uiso 1 1 calc R
C3 C 0.58937(19) 0.3607(2) 0.96608(16) 0.0160(4) Uani 1 1 d .
C13 C 0.27282(18) 0.69390(19) 0.75088(16) 0.0148(4) Uani 1 1 d .
C5 C 0.6947(2) 0.4281(2) 0.95402(17) 0.0193(4) Uani 1 1 d .
H5A H 0.7140 0.4959 0.8791 0.029 Uiso 1 1 calc R
H5B H 0.7729 0.3636 0.9621 0.029 Uiso 1 1 calc R
H5C H 0.6663 0.4690 1.0130 0.029 Uiso 1 1 calc R
C11 C 0.16247(19) 0.5255(2) 0.83249(16) 0.0169(4) Uani 1 1 d .
C15 C 0.3093(2) 0.82852(19) 0.69944(18) 0.0184(4) Uani 1 1 d .
H15A H 0.4039 0.8220 0.6763 0.028 Uiso 1 1 calc R
H15B H 0.2706 0.8744 0.7552 0.028 Uiso 1 1 calc R
H15C H 0.2773 0.8776 0.6330 0.028 Uiso 1 1 calc R
C14 C 0.0614(2) 0.4372(2) 0.8833(2) 0.0237(4) Uani 1 1 d .
H14A H 0.1032 0.3452 0.9017 0.036 Uiso 1 1 calc R
H14B H 0.0138 0.4557 0.8289 0.036 Uiso 1 1 calc R
H14C H 0.0009 0.4528 0.9526 0.036 Uiso 1 1 calc R
C1 C 0.4401(2) 0.2319(2) 1.02536(17) 0.0201(4) Uani 1 1 d .
C2 C 0.5315(2) 0.2585(2) 1.05821(17) 0.0213(4) Uani 1 1 d .
H2 H 0.5509 0.2160 1.1287 0.026 Uiso 1 1 calc R
C9 C 0.3767(2) 0.1273(2) 0.7276(2) 0.0243(4) Uani 1 1 d .
H9A H 0.3209 0.1296 0.8027 0.036 Uiso 1 1 calc R
H9B H 0.4326 0.0419 0.7352 0.036 Uiso 1 1 calc R
H9C H 0.3227 0.1406 0.6795 0.036 Uiso 1 1 calc R
C4 C 0.3486(3) 0.1334(3) 1.0894(2) 0.0326(6) Uani 1 1 d .
H4A H 0.2964 0.1395 1.0420 0.049 Uiso 1 1 calc R
H4B H 0.2912 0.1513 1.1586 0.049 Uiso 1 1 calc R
H4C H 0.3980 0.0448 1.1094 0.049 Uiso 1 1 calc R
C16 C 0.70037(19) 0.75848(19) 0.63366(17) 0.0160(4) Uani 1 1 d .
C17 C 0.6891(2) 0.8959(2) 0.60829(18) 0.0200(4) Uani 1 1 d .
H17 H 0.6087 0.9499 0.6014 0.024 Uiso 1 1 calc R
B1 B 0.3618(2) 0.3368(2) 0.84065(18) 0.0150(4) Uani 1 1 d .
H1 H 0.2973 0.2741 0.8782 0.018 Uiso 1 1 calc R
N1 N 0.53562(15) 0.39459(16) 0.88236(13) 0.0135(3) Uani 1 1 d .
N2 N 0.44381(16) 0.31506(16) 0.91908(14) 0.0149(3) Uani 1 1 d .
N4 N 0.45367(15) 0.31663(15) 0.72820(14) 0.0136(3) Uani 1 1 d .
C6 C 0.45873(19) 0.23378(19) 0.67499(17) 0.0166(4) Uani 1 1 d .
C8 C 0.60073(18) 0.37220(19) 0.56462(16) 0.0150(4) Uani 1 1 d .
C7 C 0.5511(2) 0.2671(2) 0.57049(18) 0.0182(4) Uani 1 1 d .
H7 H 0.5758 0.2267 0.5142 0.022 Uiso 1 1 calc R
C10 C 0.70365(19) 0.4464(2) 0.47182(17) 0.0184(4) Uani 1 1 d .
H10A H 0.7164 0.5148 0.4936 0.028 Uiso 1 1 calc R
H10B H 0.6770 0.4872 0.4021 0.028 Uiso 1 1 calc R
H10C H 0.7850 0.3858 0.4589 0.028 Uiso 1 1 calc R
C29 C 0.9055(4) 0.0930(4) 1.0126(3) 0.0636(11) Uani 1 1 d .
H29A H 0.8924 0.1785 1.0220 0.095 Uiso 1 1 calc R
H29B H 0.8490 0.0359 1.0786 0.095 Uiso 1 1 calc R
H29C H 0.8844 0.1054 0.9440 0.095 Uiso 1 1 calc R
C30 C 1.0348(5) 0.0351(6) 1.0027(4) 0.0360(12) Uani 0.50 1 d P
O3 O 1.1089(7) 0.0979(6) 0.9976(7) 0.096(3) 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'
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'
Ni Ni 0.3393 1.1124 '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'
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
O1 Ni1 N3 131.98(7) . .
O1 Ni1 N1 135.24(7) . .
N3 Ni1 N1 92.79(6) . .
O1 Ni1 N7 87.76(6) . .
N3 Ni1 N7 92.66(6) . .
N1 Ni1 N7 90.78(6) . .
O1 Ni1 N5 93.32(6) . .
N3 Ni1 N5 87.14(6) . .
N1 Ni1 N5 87.96(6) . .
N7 Ni1 N5 178.71(6) . .
C22 O2 C23 104.46(15) . .
C16 O1 Ni1 131.28(13) . .
C13 N5 N6 106.51(15) . .
C13 N5 Ni1 139.68(13) . .
N6 N5 Ni1 113.80(12) . .
C8 N3 N4 107.47(15) . .
C8 N3 Ni1 134.67(13) . .
N4 N3 Ni1 117.65(12) . .
C11 N6 N5 109.82(16) . .
C11 N6 B1 129.20(17) . .
N5 N6 B1 120.99(15) . .
C22 N7 C28 105.61(16) . .
C22 N7 Ni1 124.93(13) . .
C28 N7 Ni1 129.46(13) . .
C28 C27 C26 116.40(19) . .
C23 C28 C27 120.33(18) . .
C23 C28 N7 107.64(17) . .
C27 C28 N7 132.03(18) . .
C24 C23 O2 127.36(19) . .
C24 C23 C28 124.29(19) . .
O2 C23 C28 108.35(16) . .
C23 C24 C25 115.2(2) . .
C20 C21 C16 120.85(18) . .
C20 C21 C22 119.34(17) . .
C16 C21 C22 119.81(17) . .
C27 C26 C25 122.0(2) . .
C20 C19 C18 119.02(19) . .
C19 C20 C21 120.95(19) . .
C17 C18 C19 120.95(19) . .
N7 C22 O2 113.92(16) . .
N7 C22 C21 128.45(17) . .
O2 C22 C21 117.61(16) . .
C24 C25 C26 121.69(19) . .
C11 C12 C13 105.98(17) . .
N1 C3 C2 109.39(18) . .
N1 C3 C5 121.49(18) . .
C2 C3 C5 129.12(18) . .
N5 C13 C12 109.93(18) . .
N5 C13 C15 122.88(17) . .
C12 C13 C15 127.19(18) . .
N6 C11 C12 107.77(17) . .
N6 C11 C14 123.13(19) . .
C12 C11 C14 129.07(19) . .
N2 C1 C2 107.75(18) . .
N2 C1 C4 122.50(19) . .
C2 C1 C4 129.74(19) . .
C1 C2 C3 105.85(18) . .
O1 C16 C17 119.38(18) . .
O1 C16 C21 124.34(18) . .
C17 C16 C21 116.27(18) . .
C18 C17 C16 121.81(19) . .
N2 B1 N6 108.67(16) . .
N2 B1 N4 108.81(15) . .
N6 B1 N4 108.24(15) . .
C3 N1 N2 107.33(16) . .
C3 N1 Ni1 134.68(14) . .
N2 N1 Ni1 117.98(12) . .
C1 N2 N1 109.67(16) . .
C1 N2 B1 131.76(17) . .
N1 N2 B1 118.49(15) . .
C6 N4 N3 109.42(16) . .
C6 N4 B1 131.79(17) . .
N3 N4 B1 118.51(15) . .
N4 C6 C7 107.63(17) . .
N4 C6 C9 122.77(19) . .
C7 C6 C9 129.60(19) . .
N3 C8 C7 109.39(17) . .
N3 C8 C10 121.27(17) . .
C7 C8 C10 129.33(18) . .
C6 C7 C8 106.09(17) . .
O3 C30 C30 172.9(9) . 2_757
O3 C30 C29 118.2(7) . .
C30 C30 C29 66.3(5) 2_757 .
O3 C30 C29 114.8(6) . 2_757
C30 C30 C29 60.4(5) 2_757 2_757
C29 C30 C29 126.8(4) . 2_757
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O1 1.9462(15) .
Ni1 N3 2.0176(16) .
Ni1 N1 2.0249(16) .
Ni1 N7 2.0594(16) .
Ni1 N5 2.1105(16) .
O2 C22 1.375(2) .
O2 C23 1.378(2) .
O1 C16 1.306(2) .
N5 C13 1.340(2) .
N5 N6 1.381(2) .
N3 C8 1.337(2) .
N3 N4 1.371(2) .
N6 C11 1.358(3) .
N6 B1 1.542(3) .
N7 C22 1.306(2) .
N7 C28 1.403(2) .
C27 C28 1.391(3) .
C27 C26 1.396(3) .
C28 C23 1.389(3) .
C23 C24 1.380(3) .
C24 C25 1.390(3) .
C21 C20 1.410(3) .
C21 C16 1.423(3) .
C21 C22 1.434(3) .
C26 C25 1.399(3) .
C19 C20 1.373(3) .
C19 C18 1.401(3) .
C18 C17 1.378(3) .
C12 C11 1.379(3) .
C12 C13 1.405(3) .
C3 N1 1.339(2) .
C3 C2 1.401(3) .
C3 C5 1.496(3) .
C13 C15 1.492(3) .
C11 C14 1.497(3) .
C1 N2 1.352(3) .
C1 C2 1.387(3) .
C1 C4 1.495(3) .
C9 C6 1.491(3) .
C16 C17 1.418(3) .
B1 N2 1.543(3) .
B1 N4 1.550(3) .
N1 N2 1.370(2) .
N4 C6 1.357(2) .
C6 C7 1.385(3) .
C8 C7 1.397(3) .
C8 C10 1.493(3) .
C29 C30 1.395(7) .
C30 O3 1.193(8) .
C30 C30 1.285(12) 2_757
C30 C29 1.470(7) 2_757
