An unusual bis-heteroscorpionate complex with anomalous ligands: [tris(3,4-dibromo-5-phenylpyrazolyl)hydroborato][hydrotris(3-neopentylpyrazolyl)borato]nickel(II)
Trofimenko, Swiatoslaw; Jové, Fernando; Yap, Glenn P. A.; Acta Crystallographica Section C 72 (2016) 802–805; doi:10.1107/S2053229616001376

data_2020600
_publ_section_title
;
 An unusual bis-heteroscorpionate complex with anomalous ligands:
 [tris(3,4-dibromo-5-phenylpyrazolyl)hydroborato][hydrotris(3-neopentylpyrazolyl)borato]nickel(II)
;
_journal_coeditor_code           FO3001
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              802
_journal_page_last               805
_journal_paper_doi               10.1107/S2053229616001376
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          '[Ni (C27 H16 B1 Br6 N6) (C24 H40 B N6)]'
_chemical_formula_sum            'C51 H56 B2 Br6 N12 Ni'
_chemical_formula_weight         1396.86
_chemical_name_systematic
'[Hydrotris(3,4-dibromo-5-phenyl-pyrazolyl)borato-\k<i>N</i>^2^][hydrotris(3-neopentylpyrazolyl-\k<i>N</i>^2^)lborato]nickel(II)'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                69.299(6)
_cell_angle_beta                 74.191(6)
_cell_angle_gamma                89.546(6)
_cell_formula_units_Z            4
_cell_length_a                   12.833(5)
_cell_length_b                   21.295(8)
_cell_length_c                   22.787(9)
_cell_measurement_reflns_used    1016
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.50
_cell_measurement_theta_min      2.60
_cell_volume                     5578(4)
_computing_cell_refinement
;
SHELXTL (Sheldrick, 2008)
;
_computing_data_collection
;
SMART (Bruker, 2002)
;
_computing_data_reduction
;
SHELXTL (Sheldrick, 2008)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
Mercury (Bruno <i>et al.</i>,  2002)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXL97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 836.6
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            62529
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.275
_diffrn_reflns_theta_min         1.141
_exptl_absorpt_coefficient_mu    4.693
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6142
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2003)
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2776
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.301
_refine_diff_density_min         -0.818
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1327
_refine_ls_number_reflns         25046
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0425P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0945
_reflns_number_gt                18299
_reflns_number_total             25046
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fo3001sup1.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2020600.cif.'
_cod_database_code               2020600
_cod_database_fobs_code          2020600
_shelx_estimated_absorpt_t_min   0.255
_shelx_estimated_absorpt_t_max   0.454
_shelx_hkl_checksum              54231
_shelx_res_checksum              99855