A redetermination of chlorido[hydridotris(3-<i>tert</i>-butyl-5-methylpyrazolyl)borato]nickel(II)
Adam D. Beitelman; Gregory M. Ferrence; Acta Crystallographica Section E 63 (2007) m2520–m2521; doi:10.1107/S1600536807043814

data_2215465
_publ_section_title
;
 A redetermination of
 chlorido[hydridotris(3-<i>tert</i>-butyl-5-methylpyrazolyl)borato]nickel(II)
;
_journal_coeditor_code           FI2040
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2520
_journal_page_last               m2521
_journal_paper_doi               10.1107/S1600536807043814
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Ni Cl(C24 H40 B N6)]'
_chemical_formula_moiety         'C24 H40 B1 Cl1 N6 Ni1'
_chemical_formula_sum            'C24 H40 B Cl N6 Ni'
_chemical_formula_weight         517.59
_chemical_name_systematic
chlorido[hydridotris(3-tert-butyl-5-methylpyrazolyl)borato]nickel(II)
_space_group_IT_number           160
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 -2"'
_symmetry_space_group_name_H-M   'R 3 m :H'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   15.8900(4)
_cell_length_b                   15.8900(4)
_cell_length_c                   9.4584(5)
_cell_measurement_reflns_used    5297
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.34
_cell_measurement_theta_min      2.56
_cell_volume                     2068.22(13)
_computing_cell_refinement       'SMART (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material
'<i>WinGX</i> (Farrugia, 1999) and <i>publCIF</i> (Westrip, 2007)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4349
_diffrn_reflns_theta_full        26.34
_diffrn_reflns_theta_max         26.34
_diffrn_reflns_theta_min         3.66
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.823
_exptl_absorpt_correction_T_max  0.7845
_exptl_absorpt_correction_T_min  0.6818
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.226
_refine_diff_density_min         -0.143
_refine_ls_abs_structure_details 'Flack (1983), 444 Friedel pairs'
_refine_ls_abs_structure_Flack   0.033(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     69
_refine_ls_number_reflns         964
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_gt           0.0175
_refine_ls_shift/su_max          <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0143P)^2^+0.6826P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0448
_reflns_number_gt                964
_reflns_number_total             964
_reflns_threshold_expression     I>>2\s(I)
_cod_data_source_file            fi2040.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'R 3 m'
_cod_database_code               2215465
_cod_database_fobs_code          2215465