#------------------------------------------------------------------------------
#$Date: 2016-08-07 11:39:55 +0300 (Sun, 07 Aug 2016) $
#$Revision: 185303 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/03/91/7039162.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_7039162
loop_
_publ_author_name
'Li, Jing'
'Han, Yuan'
'Cao, Fan'
'Wei, Rong-Min'
'Zhang, Yi-Quan'
'Song, You'
_publ_section_title
;
 Two field-induced slow magnetic relaxation processes in a mononuclear
 Co(ii) complex with a distorted octahedral geometry.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9279
_journal_page_last               9284
_journal_paper_doi               10.1039/c6dt00979d
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C30 H44 B2 Co N12'
_chemical_formula_sum            'C30 H44 B2 Co N12'
_chemical_formula_weight         653.32
_chemical_name_common            Co(Tp*)2
_chemical_name_systematic
'Cobalt Bis-hydridotris(3,5-dimethylpyrazole)borate '
_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
_audit_update_record
;
2016-04-29 deposited with the CCDC.
2016-04-29 downloaded from the CCDC.
;
_cell_angle_alpha                106.446(3)
_cell_angle_beta                 108.868(3)
_cell_angle_gamma                109.701(2)
_cell_formula_units_Z            1
_cell_length_a                   8.8252(14)
_cell_length_b                   10.8259(17)
_cell_length_c                   11.028(3)
_cell_measurement_reflns_used    2472
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.16
_cell_measurement_theta_min      2.23
_cell_volume                     842.8(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0181
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5541
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    0.549
_exptl_absorpt_correction_T_max  0.835
_exptl_absorpt_correction_T_min  0.736
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       strip
_exptl_crystal_F_000             345
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.74
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.235
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3837
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0714P)²+0.1439P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.1258
_reflns_number_gt                3274
_reflns_number_total             3837
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt00979d2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7039162.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7039162
_solvent_exptl_crystal_recrystallization_method 'CH2Cl2 and iPrOH'
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
Co1 Co 0.5000 0.5000 0.5000 0.03743(14) Uani 1 2 d S
N1 N 0.2785(2) 0.28980(18) 0.18506(17) 0.0424(4) Uani 1 1 d .
N2 N 0.2603(2) 0.36664(19) 0.29747(17) 0.0447(4) Uani 1 1 d .
N3 N 0.6023(2) 0.45967(19) 0.25892(17) 0.0418(4) Uani 1 1 d .
N4 N 0.6447(2) 0.56542(18) 0.38646(18) 0.0446(4) Uani 1 1 d .
N5 N 0.5316(2) 0.24847(18) 0.32480(17) 0.0407(4) Uani 1 1 d .
N6 N 0.5540(2) 0.31869(18) 0.45944(17) 0.0435(4) Uani 1 1 d .
C1 C 0.0929(4) 0.1248(3) -0.0763(2) 0.0649(7) Uani 1 1 d .
H1A H 0.1846 0.1772 -0.0977 0.097 Uiso 1 1 calc R
H1B H -0.0249 0.0960 -0.1491 0.097 Uiso 1 1 calc R
H1C H 0.1011 0.0395 -0.0730 0.097 Uiso 1 1 calc R
C2 C 0.1208(3) 0.2210(2) 0.0650(2) 0.0478(5) Uani 1 1 d .
C3 C -0.0032(3) 0.2528(3) 0.0999(3) 0.0563(6) Uani 1 1 d .
H3 H -0.1241 0.2200 0.0385 0.068 Uiso 1 1 calc R
C4 C 0.0908(3) 0.3443(2) 0.2463(2) 0.0508(5) Uani 1 1 d .
C5 C 0.0182(3) 0.4094(3) 0.3387(3) 0.0667(7) Uani 1 1 d .
H5A H 0.1168 0.4797 0.4316 0.100 Uiso 1 1 calc R
H5B H -0.0666 0.3334 0.3473 0.100 Uiso 1 1 calc R
H5C H -0.0419 0.4567 0.2961 0.100 Uiso 1 1 calc R
C6 C 0.5666(4) 0.0412(3) 0.1870(3) 0.0664(7) Uani 1 1 d .
H6A H 0.4435 -0.0132 0.1122 0.100 Uiso 1 1 calc R
H6B H 0.6086 -0.0253 0.2072 0.100 Uiso 1 1 calc R
H6C H 0.6423 0.0990 0.1573 0.100 Uiso 1 1 calc R
C7 C 0.5750(3) 0.1392(2) 0.3183(2) 0.0469(5) Uani 1 1 d .
C8 C 0.6266(3) 0.1390(2) 0.4490(2) 0.0528(5) Uani 1 1 d .
H8 H 0.6645 0.0762 0.4758 0.063 Uiso 1 1 calc R
C9 C 0.6110(3) 0.2514(2) 0.5340(2) 0.0484(5) Uani 1 1 d .
C10 C 0.6511(5) 0.2972(3) 0.6869(3) 0.0699(7) Uani 1 1 d .
H10A H 0.7800 0.3432 0.7462 0.105 Uiso 1 1 calc R
H10B H 0.5925 0.2129 0.6996 0.105 Uiso 1 1 calc R
H10C H 0.6067 0.3649 0.7130 0.105 Uiso 1 1 calc R
C11 C 0.6760(4) 0.4358(3) 0.0549(3) 0.0673(7) Uani 1 1 d .
H11A H 0.6591 0.3403 0.0442 0.101 Uiso 1 1 calc R
H11B H 0.7836 0.4861 0.0484 0.101 Uiso 1 1 calc R
H11C H 0.5727 0.4269 -0.0192 0.101 Uiso 1 1 calc R
C12 C 0.6954(3) 0.5205(3) 0.1975(2) 0.0498(5) Uani 1 1 d .
C13 C 0.8019(4) 0.6661(3) 0.2875(3) 0.0594(6) Uani 1 1 d .
H13 H 0.8832 0.7354 0.2743 0.071 Uiso 1 1 calc R
C14 C 0.7646(3) 0.6903(2) 0.4030(3) 0.0518(5) Uani 1 1 d .
C15 C 0.8445(4) 0.8322(3) 0.5312(3) 0.0728(8) Uani 1 1 d .
H15A H 0.8050 0.8142 0.5988 0.109 Uiso 1 1 calc R
H15B H 0.8050 0.8964 0.5024 0.109 Uiso 1 1 calc R
H15C H 0.9747 0.8767 0.5743 0.109 Uiso 1 1 calc R
B1 B 0.4651(3) 0.2989(3) 0.2091(2) 0.0423(5) Uani 1 1 d .
H1 H 0.4476 0.2282 0.1063 0.051 Uiso 1 1 d R
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'
Co Co 0.3494 0.9721 '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'
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
N6 Co1 N6 180.0 2_666 .
N6 Co1 N2 86.61(7) 2_666 2_666
N6 Co1 N2 93.39(7) . 2_666
N6 Co1 N2 93.39(7) 2_666 .
N6 Co1 N2 86.61(7) . .
N2 Co1 N2 180.0 2_666 .
N6 Co1 N4 93.51(6) 2_666 .
N6 Co1 N4 86.49(6) . .
N2 Co1 N4 92.49(7) 2_666 .
N2 Co1 N4 87.51(7) . .
N6 Co1 N4 86.49(6) 2_666 2_666
N6 Co1 N4 93.51(6) . 2_666
N2 Co1 N4 87.51(7) 2_666 2_666
N2 Co1 N4 92.49(7) . 2_666
N4 Co1 N4 180.000(1) . 2_666
C2 N1 N2 109.81(17) . .
C2 N1 B1 130.34(17) . .
N2 N1 B1 119.77(16) . .
C4 N2 N1 107.11(17) . .
C4 N2 Co1 135.49(15) . .
N1 N2 Co1 117.21(12) . .
C12 N3 N4 109.77(18) . .
C12 N3 B1 130.91(18) . .
N4 N3 B1 119.32(15) . .
C14 N4 N3 106.62(16) . .
C14 N4 Co1 135.84(15) . .
N3 N4 Co1 117.40(12) . .
C7 N5 N6 109.36(16) . .
C7 N5 B1 130.40(17) . .
N6 N5 B1 120.24(15) . .
C9 N6 N5 106.52(16) . .
C9 N6 Co1 136.44(14) . .
N5 N6 Co1 117.01(12) . .
C2 C1 H1A 109.5 . .
C2 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
C2 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
N1 C2 C3 107.52(19) . .
N1 C2 C1 123.5(2) . .
C3 C2 C1 129.0(2) . .
C2 C3 C4 105.8(2) . .
C2 C3 H3 127.1 . .
C4 C3 H3 127.1 . .
N2 C4 C3 109.7(2) . .
N2 C4 C5 122.7(2) . .
C3 C4 C5 127.6(2) . .
C4 C5 H5A 109.5 . .
C4 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C4 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
C7 C6 H6A 109.5 . .
C7 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C7 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
N5 C7 C8 108.00(18) . .
N5 C7 C6 123.3(2) . .
C8 C7 C6 128.7(2) . .
C7 C8 C9 106.19(19) . .
C7 C8 H8 126.9 . .
C9 C8 H8 126.9 . .
N6 C9 C8 109.93(19) . .
N6 C9 C10 122.5(2) . .
C8 C9 C10 127.6(2) . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C12 C11 H11A 109.5 . .
C12 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C12 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
N3 C12 C13 107.5(2) . .
N3 C12 C11 123.4(2) . .
C13 C12 C11 129.2(2) . .
C12 C13 C14 106.4(2) . .
C12 C13 H13 126.8 . .
C14 C13 H13 126.8 . .
N4 C14 C13 109.8(2) . .
N4 C14 C15 122.4(2) . .
C13 C14 C15 127.8(2) . .
C14 C15 H15A 109.5 . .
C14 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C14 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
N1 B1 N5 109.81(16) . .
N1 B1 N3 108.57(16) . .
N5 B1 N3 109.67(17) . .
N1 B1 H1 107.3 . .
N5 B1 H1 111.2 . .
N3 B1 H1 110.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N6 2.1334(16) 2_666
Co1 N6 2.1334(16) .
Co1 N2 2.1465(17) 2_666
Co1 N2 2.1465(17) .
Co1 N4 2.1509(17) .
Co1 N4 2.1509(17) 2_666
N1 C2 1.340(3) .
N1 N2 1.375(2) .
N1 B1 1.544(3) .
N2 C4 1.321(3) .
N3 C12 1.347(3) .
N3 N4 1.374(2) .
N3 B1 1.550(3) .
N4 C14 1.324(3) .
N5 C7 1.351(3) .
N5 N6 1.375(2) .
N5 B1 1.548(3) .
N6 C9 1.333(3) .
C1 C2 1.494(3) .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
C2 C3 1.384(3) .
C3 C4 1.397(3) .
C3 H3 0.9300 .
C4 C5 1.506(3) .
C5 H5A 0.9600 .
C5 H5B 0.9600 .
C5 H5C 0.9600 .
C6 C7 1.496(3) .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C6 H6C 0.9600 .
C7 C8 1.365(3) .
C8 C9 1.389(3) .
C8 H8 0.9300 .
C9 C10 1.495(3) .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
C11 C12 1.498(3) .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C12 C13 1.366(4) .
C13 C14 1.392(3) .
C13 H13 0.9300 .
C14 C15 1.500(3) .
C15 H15A 0.9600 .
C15 H15B 0.9600 .
C15 H15C 0.9600 .
B1 H1 1.1005 .
