(Di-2-pyridylamine-κ^2^<i>N</i>,<i>N</i>')[hydrotris(3,5-diphenylpyrazol-1-yl-κ<i>N</i>^2^)borato]nickel(II) bromide dichloromethane monosolvate
Harding, David J.; Harding, Phimphaka; Adams, Harry; Acta Crystallographica Section E 67 (2011) m477–m478; doi:10.1107/S1600536811010233

data_2229719
_publ_section_title
;
 (Di-2-pyridylamine-\k^2^<i>N</i>,<i>N</i>')[hydrotris(3,5-diphenylpyrazol-1-yl-\k<i>N</i>^2^)borato]nickel(II)
 bromide dichloromethane monosolvate
;
_journal_coeditor_code           IS2690
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m477
_journal_page_last               m478
_journal_paper_doi               10.1107/S1600536811010233
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Ni (C45 H34 B N6) (C10 H9 N3)] Br, C H2 Cl2'
_chemical_formula_moiety         'C55 H43 B N9 Ni +, Br -, C H2 Cl2'
_chemical_formula_sum            'C56 H45 B Br Cl2 N9 Ni'
_chemical_formula_weight         1064.34
_chemical_name_systematic
;
(Di-2-pyridylamine-\k^2^<i>N</i>,<i>N</i>')[hydrotris(3,5-diphenylpyrazol-
1-yl-\k<i>N</i>^2^)borato]nickel(II) bromide dichloromethane monosolvate
;
_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                91.314(6)
_cell_angle_beta                 99.245(6)
_cell_angle_gamma                101.968(6)
_cell_formula_units_Z            2
_cell_length_a                   10.3263(13)
_cell_length_b                   13.9040(16)
_cell_length_c                   17.622(2)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.60
_cell_measurement_theta_min      2.18
_cell_volume                     2438.8(5)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material  '<i>publCIF</i> (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w'
_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  0.0609
_diffrn_reflns_av_sigmaI/netI    0.0551
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            44352
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.84
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    1.376
_exptl_absorpt_correction_T_max  0.6672
_exptl_absorpt_correction_T_min  0.6159
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1997)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1092
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.32
_refine_diff_density_max         1.403
_refine_diff_density_min         -1.664
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         11127
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0545
_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/[\s^2^(Fo^2^)+(0.1045P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1509
_refine_ls_wR_factor_ref         0.1608
_reflns_number_gt                9003
_reflns_number_total             11127
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            is2690.cif
_cod_data_source_block           I
_cod_database_code               2229719
_cod_database_fobs_code          2229719