[Tris(3,5-diphenylpyrazolyl)hydroborato]nickel(II) bromide
Harding, David J.; Harding, Phimphaka; Adams, Harry; Acta Crystallographica Section E 65 (2009) m773–; doi:10.1107/S1600536809021606

data_2222312
_publ_section_title
;
 [Tris(3,5-diphenylpyrazolyl)hydroborato]nickel(II) bromide
;
_journal_coeditor_code           HB2976
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m773
_journal_paper_doi               10.1107/S1600536809021606
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Ni Br (C45 H34 B N6)]'
_chemical_formula_moiety         'C45 H34 B Br N6 Ni'
_chemical_formula_sum            'C45 H34 B Br N6 Ni'
_chemical_formula_weight         808.21
_chemical_name_systematic
;
[Tris(3,5-diphenylpyrazolyl)hydroborato]nickel(II) bromide
;
_space_group_IT_number           146
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   12.8227(8)
_cell_length_b                   12.8227(8)
_cell_length_c                   19.327(3)
_cell_measurement_reflns_used    2851
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.61
_cell_measurement_theta_min      2.79
_cell_volume                     2752.0(5)
_computing_cell_refinement       'SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       \f
_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  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0556
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            5609
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.661
_exptl_absorpt_correction_T_max  0.722
_exptl_absorpt_correction_T_min  0.691
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1997)'
_exptl_crystal_colour            purple--pink
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1242
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.294
_refine_ls_abs_structure_details 'Flack (1983), 670 Friedel pairs'
_refine_ls_abs_structure_Flack   0.020(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2075
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0278
_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/[\s^2^(Fo^2^)+(0.0169P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0617
_refine_ls_wR_factor_ref         0.0629
_reflns_number_gt                1943
_reflns_number_total             2075
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb2976.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               2222312
_cod_database_fobs_code          2222312