#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/23/2222312.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2222312
loop_
_publ_author_name
'Harding, David J.'
'Harding, Phimphaka'
'Adams, Harry'
_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       φ
_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/[σ²(Fo²)+(0.0169P)²] where P=(Fo²+2Fc²)/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>2σ(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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br Br1 0.6667 0.3333 0.732391(16) 0.02249(14) Uani d S 1 . .
Ni Ni1 0.6667 0.3333 0.61068(2) 0.01335(14) Uani d S 1 . .
N N1 0.75319(18) 0.26622(19) 0.55312(10) 0.0127(4) Uani d . 1 . .
N N2 0.75175(19) 0.29001(19) 0.48407(10) 0.0128(4) Uani d . 1 . .
B B1 0.6667 0.3333 0.4567(3) 0.0139(10) Uani d S 1 . .
H H1B 0.6667 0.3333 0.3983 0.017 Uiso d SR 1 . .
C C1 0.8082(2) 0.2003(2) 0.55910(12) 0.0146(5) Uani d . 1 . .
C C2 0.8419(3) 0.1815(3) 0.49355(13) 0.0166(6) Uani d . 1 . .
H H2 0.8812 0.1373 0.4829 0.020 Uiso calc R 1 . .
C C3 0.8064(2) 0.2405(2) 0.44716(12) 0.0136(5) Uani d . 1 . .
C C4 0.8224(3) 0.2532(3) 0.37198(14) 0.0135(5) Uani d . 1 . .
C C5 0.7922(2) 0.1509(2) 0.33065(13) 0.0173(6) Uani d . 1 . .
H H5 0.7601 0.0738 0.3515 0.021 Uiso calc R 1 . .
C C6 0.8094(3) 0.1632(3) 0.25990(16) 0.0182(7) Uani d . 1 . .
H H6 0.7890 0.0942 0.2325 0.022 Uiso calc R 1 . .
C C7 0.8557(2) 0.2743(3) 0.22844(13) 0.0201(6) Uani d . 1 . .
H H7 0.8668 0.2814 0.1797 0.024 Uiso calc R 1 . .
C C8 0.8860(3) 0.3759(3) 0.26839(13) 0.0215(6) Uani d . 1 . .
H H8 0.9179 0.4525 0.2469 0.026 Uiso calc R 1 . .
C C9 0.8698(3) 0.3652(3) 0.33951(14) 0.0190(6) Uani d . 1 . .
H H9 0.8913 0.4350 0.3665 0.023 Uiso calc R 1 . .
C C10 0.8239(2) 0.1510(3) 0.62468(13) 0.0163(6) Uani d . 1 . .
C C11 0.8460(2) 0.2131(3) 0.68680(14) 0.0185(6) Uani d . 1 . .
H H11 0.8564 0.2919 0.6872 0.022 Uiso calc R 1 . .
C C12 0.8530(3) 0.1605(3) 0.74866(17) 0.0230(7) Uani d . 1 . .
H H12 0.8650 0.2023 0.7912 0.028 Uiso calc R 1 . .
C C13 0.8422(3) 0.0472(3) 0.74807(16) 0.0269(7) Uani d . 1 . .
H H13 0.8468 0.0113 0.7901 0.032 Uiso calc R 1 . .
C C14 0.8246(3) -0.0137(3) 0.68574(15) 0.0234(7) Uani d . 1 . .
H H14 0.8191 -0.0904 0.6849 0.028 Uiso calc R 1 . .
C C15 0.8150(3) 0.0381(3) 0.62476(16) 0.0209(6) Uani d . 1 . .
H H15 0.8022 -0.0041 0.5824 0.025 Uiso calc R 1 . .
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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'
Br Br -0.2901 2.4595 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Ni1 N1 . 3_665 93.11(8) y
N1 Ni1 N1 . 2_655 93.11(8) ?
N1 Ni1 N1 3_665 2_655 93.11(8) ?
N1 Ni1 Br1 . . 123.04(6) y
N1 Ni1 Br1 3_665 . 123.04(6) ?
N1 Ni1 Br1 2_655 . 123.04(6) ?
C1 N1 N2 . . 106.99(19) ?
C1 N1 Ni1 . . 141.45(17) ?
N2 N1 Ni1 . . 111.47(15) ?
C3 N2 N1 . . 109.82(19) ?
C3 N2 B1 . . 127.6(2) ?
N1 N2 B1 . . 120.3(2) ?
N2 B1 N2 . 3_665 108.89(19) ?
N2 B1 N2 . 2_655 108.89(19) ?
N2 B1 N2 3_665 2_655 108.89(19) ?
N2 B1 H1B . . 110.0 ?
N2 B1 H1B 3_665 . 110.0 ?
N2 B1 H1B 2_655 . 110.0 ?
N1 C1 C2 . . 109.5(2) ?
N1 C1 C10 . . 124.6(2) ?
C2 C1 C10 . . 125.8(2) ?
C3 C2 C1 . . 106.1(2) ?
C3 C2 H2 . . 127.0 ?
C1 C2 H2 . . 127.0 ?
N2 C3 C2 . . 107.6(2) ?
N2 C3 C4 . . 122.9(2) ?
C2 C3 C4 . . 129.5(2) ?
C9 C4 C5 . . 118.4(2) ?
C9 C4 C3 . . 121.7(3) ?
C5 C4 C3 . . 119.9(2) ?
C6 C5 C4 . . 119.9(3) ?
C6 C5 H5 . . 120.0 ?
C4 C5 H5 . . 120.0 ?
C7 C6 C5 . . 121.0(3) ?
C7 C6 H6 . . 119.5 ?
C5 C6 H6 . . 119.5 ?
C6 C7 C8 . . 119.7(2) ?
C6 C7 H7 . . 120.1 ?
C8 C7 H7 . . 120.1 ?
C9 C8 C7 . . 119.9(3) ?
C9 C8 H8 . . 120.0 ?
C7 C8 H8 . . 120.0 ?
C8 C9 C4 . . 120.9(3) ?
C8 C9 H9 . . 119.5 ?
C4 C9 H9 . . 119.5 ?
C11 C10 C15 . . 118.8(3) ?
C11 C10 C1 . . 121.9(3) ?
C15 C10 C1 . . 119.2(2) ?
C10 C11 C12 . . 120.4(3) ?
C10 C11 H11 . . 119.8 ?
C12 C11 H11 . . 119.8 ?
C13 C12 C11 . . 120.1(3) ?
C13 C12 H12 . . 120.0 ?
C11 C12 H12 . . 120.0 ?
C14 C13 C12 . . 119.8(3) ?
C14 C13 H13 . . 120.1 ?
C12 C13 H13 . . 120.1 ?
C15 C14 C13 . . 119.7(3) ?
C15 C14 H14 . . 120.2 ?
C13 C14 H14 . . 120.2 ?
C14 C15 C10 . . 121.1(3) ?
C14 C15 H15 . . 119.4 ?
C10 C15 H15 . . 119.4 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 Br1 . 2.3523(6) y
Ni1 N1 . 2.041(2) y
Ni1 N1 3_665 2.041(2) ?
Ni1 N1 2_655 2.041(2) ?
N1 C1 . 1.350(3) n
N1 N2 . 1.371(3) n
N2 C3 . 1.360(3) n
N2 B1 . 1.544(3) ?
B1 N2 3_665 1.544(3) ?
B1 N2 2_655 1.544(3) ?
B1 H1B . 1.1278 ?
C1 C2 . 1.398(4) n
C1 C10 . 1.475(3) ?
C2 C3 . 1.388(3) n
C2 H2 . 0.9500 ?
C3 C4 . 1.465(4) ?
C4 C9 . 1.397(4) ?
C4 C5 . 1.415(4) ?
C5 C6 . 1.381(4) ?
C5 H5 . 0.9500 ?
C6 C7 . 1.380(4) ?
C6 H6 . 0.9500 ?
C7 C8 . 1.392(4) ?
C7 H7 . 0.9500 ?
C8 C9 . 1.387(4) ?
C8 H8 . 0.9500 ?
C9 H9 . 0.9500 ?
C10 C11 . 1.389(4) ?
C10 C15 . 1.394(4) ?
C11 C12 . 1.397(4) ?
C11 H11 . 0.9500 ?
C12 C13 . 1.390(5) ?
C12 H12 . 0.9500 ?
C13 C14 . 1.391(5) ?
C13 H13 . 0.9500 ?
C14 C15 . 1.388(4) ?
C14 H14 . 0.9500 ?
C15 H15 . 0.9500 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C5 H5 Cg1 6_654 0.95 2.73 3.589(3) 151
