#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:55:48 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178967 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/96/4119661.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4119661
loop_
_publ_author_name
'Jun Nakazawa'
'Shota Terada'
'Masaki Yamada'
'Shiro Hikichi'
_publ_contact_author_address
;
  Departmet of Material & Life Chemistry, Faculty of Engineering,
 Kanagawa University
  3-27-1 Rokkakubashi, Kanagawa-ku, Yokohama-city, 222-8686, JAPAN
;
_publ_contact_author_email       jnaka@kanagawa-u.ac.jp
_publ_contact_author_fax         +81-45-413-9770
_publ_contact_author_name        'Jun Nakazawa'
_publ_contact_author_phone       +81-45-481-5661(ext.3889)
_publ_section_title
;
 Structural Characterization and Oxidation Reactivity of a Nickel(II)
 Acylperoxo Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6010
_journal_page_last               6013
_journal_paper_doi               10.1021/ja4020277
_journal_volume                  135
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C15 H13 B Br F9 N6 Ni'
_chemical_formula_sum            'C15 H13 B Br F9 N6 Ni'
_chemical_formula_weight         597.74
_chemical_name_common            '[Ni(TPCF3,Me)Br]'
_chemical_name_systematic
;
[bromido{Hydrotris(5-methyl-3-(trifluoro)methyl-
pyrazoryl)borato}nickel(II)]
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2n 2ac'
_symmetry_space_group_name_H-M   'P c m n'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.698(5)
_cell_length_b                   13.345(7)
_cell_length_c                   17.896(10)
_cell_measurement_reflns_used    6277
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.4802
_cell_measurement_theta_min      1.93036
_cell_volume                     2077(2)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction
'CrystalClear (Rigaku Inc., 2007), SORTAV (Blessing, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details
;
scan:
    Number of images: 600
               Slice: -110.0000 - 70.0000
         Image width: 0.3000
            Exp time: 20.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 44.9410
              2theta: -20.1054
scan:
    Number of images: 600
               Slice: -110.0000 - 70.0000
         Image width: 0.3000
            Exp time: 20.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 44.9410
              2theta: -20.1054

;
_diffrn_measurement_device
;
Saturn70 (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_method       ω
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.1069
_diffrn_orient_matrix_UB_12      -0.0349
_diffrn_orient_matrix_UB_13      -0.0240
_diffrn_orient_matrix_UB_21      0.0240
_diffrn_orient_matrix_UB_22      0.0290
_diffrn_orient_matrix_UB_23      0.0648
_diffrn_orient_matrix_UB_31      -0.0102
_diffrn_orient_matrix_UB_32      -0.0486
_diffrn_orient_matrix_UB_33      0.0256
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0780
_diffrn_reflns_av_sigmaI/netI    0.1430
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2659
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.4802
_diffrn_reflns_theta_min         1.9036
_diffrn_source_current           60.0000
_diffrn_source_power             3.0000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    2.954
_exptl_absorpt_correction_T_max  0.7566
_exptl_absorpt_correction_T_min  0.4711
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;numerical (Based on real shape of the crystal) absorption
correction was parformed on CrystalClear (Rigaku Inc., 2007)
with FS_ABSCOR method.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.911
_exptl_crystal_description       block
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.118
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         2420
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0506
_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/[σ²(Fo²)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1194
_reflns_number_gt                2234
_reflns_number_total             2420
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ja4020277_si_002_2.cif
_cod_data_source_block           01
_cod_database_code               4119661
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y, z-1/2'
'x, -y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Br1 Br 0.99165(6) 0.2500 0.54825(3) 0.0435(2) Uani 1 2 d S
Ni1 Ni 0.90519(7) 0.2500 0.66857(3) 0.0254(2) Uani 1 2 d S
N4 N 1.0143(4) 0.2500 0.8213(2) 0.0247(8) Uani 1 2 d S
F2 F 0.6444(3) 0.11828(14) 0.57878(12) 0.0414(5) Uani 1 1 d .
F4 F 1.3064(2) 0.16934(15) 0.64518(13) 0.0411(5) Uani 1 1 d .
F3 F 0.5500(2) -0.02315(15) 0.61481(12) 0.0437(5) Uani 1 1 d .
F1 F 0.7918(2) -0.00915(16) 0.59243(12) 0.0444(5) Uani 1 1 d .
N2 N 0.7696(3) 0.15561(19) 0.79647(14) 0.0261(6) Uani 1 1 d .
F5 F 1.4735(3) 0.2500 0.71113(19) 0.0413(7) Uani 1 2 d S
N1 N 0.7799(3) 0.14689(18) 0.72044(15) 0.0264(6) Uani 1 1 d .
N3 N 1.0681(4) 0.2500 0.7494(2) 0.0261(8) Uani 1 2 d S
C4 C 0.6835(4) 0.0791(2) 0.82433(19) 0.0286(7) Uani 1 1 d .
C10 C 1.1087(7) 0.2500 0.9525(3) 0.0360(12) Uani 1 2 d S
H10A H 1.0221 0.2939 0.9649 0.054 Uiso 0.50 1 calc PR
H10B H 1.2018 0.2745 0.9773 0.054 Uiso 0.50 1 calc PR
H10C H 1.0864 0.1817 0.9694 0.054 Uiso 0.50 1 calc PR
C2 C 0.6942(4) 0.0663(2) 0.70213(19) 0.0280(7) Uani 1 1 d .
C9 C 1.1328(6) 0.2500 0.8702(3) 0.0310(10) Uani 1 2 d S
C7 C 1.2221(5) 0.2500 0.7553(3) 0.0289(10) Uani 1 2 d S
C5 C 0.6591(4) 0.0647(3) 0.9069(2) 0.0388(8) Uani 1 1 d .
H5A H 0.7589 0.0632 0.9323 0.058 Uiso 1 1 calc R
H5B H 0.6052 0.0012 0.9155 0.058 Uiso 1 1 calc R
H5C H 0.5974 0.1201 0.9265 0.058 Uiso 1 1 calc R
C8 C 1.2674(5) 0.2500 0.8290(3) 0.0318(11) Uani 1 2 d S
H8 H 1.3696 0.2500 0.8477 0.038 Uiso 1 2 calc SR
C3 C 0.6334(4) 0.0219(2) 0.76502(19) 0.0296(7) Uani 1 1 d .
H3 H 0.5700 -0.0360 0.7671 0.036 Uiso 1 1 calc R
C6 C 1.3257(5) 0.2500 0.6888(3) 0.0315(10) Uani 1 2 d S
C1 C 0.6702(4) 0.0387(2) 0.6226(2) 0.0326(7) Uani 1 1 d .
B1 B 0.8375(6) 0.2500 0.8349(3) 0.0266(10) Uani 1 2 d S
H1 H 0.819(6) 0.2500 0.896(3) 0.040 Uiso 1 2 d S
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'
F F 0.0171 0.0103 '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'
Br Br -0.2901 2.4595 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 Ni1 N1 87.73(15) 8_565 .
N1 Ni1 N3 92.88(11) 8_565 .
N1 Ni1 N3 92.88(11) . .
N1 Ni1 Br1 128.49(8) 8_565 .
N1 Ni1 Br1 128.49(8) . .
N3 Ni1 Br1 116.33(12) . .
C9 N4 N3 110.3(4) . .
C9 N4 B1 130.7(4) . .
N3 N4 B1 119.0(4) . .
C4 N2 N1 109.7(2) . .
C4 N2 B1 131.0(3) . .
N1 N2 B1 119.0(3) . .
C2 N1 N2 105.8(3) . .
C2 N1 Ni1 137.9(2) . .
N2 N1 Ni1 116.22(19) . .
C7 N3 N4 105.5(4) . .
C7 N3 Ni1 138.9(3) . .
N4 N3 Ni1 115.6(3) . .
N2 C4 C3 107.9(3) . .
N2 C4 C5 122.2(3) . .
C3 C4 C5 129.9(3) . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
N1 C2 C3 110.9(3) . .
N1 C2 C1 120.5(3) . .
C3 C2 C1 128.5(3) . .
N4 C9 C8 107.5(4) . .
N4 C9 C10 122.2(5) . .
C8 C9 C10 130.3(5) . .
N3 C7 C8 111.1(4) . .
N3 C7 C6 122.7(4) . .
C8 C7 C6 126.2(4) . .
C4 C5 H5A 109.5 . .
C4 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C4 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
C7 C8 C9 105.5(4) . .
C7 C8 H8 127.2 . .
C9 C8 H8 127.2 . .
C2 C3 C4 105.7(3) . .
C2 C3 H3 127.2 . .
C4 C3 H3 127.2 . .
F4 C6 F4 106.8(4) . 8_565
F4 C6 F5 107.0(3) . .
F4 C6 F5 107.0(3) 8_565 .
F4 C6 C7 112.9(3) . .
F4 C6 C7 112.9(3) 8_565 .
F5 C6 C7 109.9(4) . .
F2 C1 F3 107.3(3) . .
F2 C1 F1 105.9(3) . .
F3 C1 F1 106.2(3) . .
F2 C1 C2 112.8(3) . .
F3 C1 C2 111.2(3) . .
F1 C1 C2 113.0(3) . .
N2 B1 N2 108.5(3) . 8_565
N2 B1 N4 107.9(3) . .
N2 B1 N4 107.9(3) 8_565 .
N2 B1 H1 112.6(14) . .
N2 B1 H1 112.6(13) 8_565 .
N4 B1 H1 107(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br1 Ni1 2.2808(14) .
Ni1 N1 1.986(3) 8_565
Ni1 N1 1.986(3) .
Ni1 N3 2.025(4) .
N4 C9 1.351(6) .
N4 N3 1.370(5) .
N4 B1 1.556(7) .
F2 C1 1.338(4) .
F4 C6 1.340(4) .
F3 C1 1.340(4) .
F1 C1 1.348(4) .
N2 C4 1.361(4) .
N2 N1 1.368(4) .
N2 B1 1.552(4) .
F5 C6 1.346(6) .
N1 C2 1.349(4) .
N3 C7 1.343(6) .
C4 C3 1.378(4) .
C4 C5 1.505(5) .
C10 C9 1.488(7) .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C2 C3 1.377(4) .
C2 C1 1.486(5) .
C9 C8 1.384(7) .
C7 C8 1.377(7) .
C7 C6 1.492(7) .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C8 H8 0.9500 .
C3 H3 0.9500 .
C6 F4 1.340(4) 8_565
B1 N2 1.552(4) 8_565
B1 H1 1.10(5) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C4 N2 N1 C2 2.3(3) . .
B1 N2 N1 C2 -171.7(3) . .
C4 N2 N1 Ni1 -178.69(19) . .
B1 N2 N1 Ni1 7.3(4) . .
N1 Ni1 N1 C2 125.8(3) 8_565 .
N3 Ni1 N1 C2 -141.4(3) . .
Br1 Ni1 N1 C2 -14.0(4) . .
N1 Ni1 N1 N2 -52.8(2) 8_565 .
N3 Ni1 N1 N2 40.0(2) . .
Br1 Ni1 N1 N2 167.39(16) . .
C9 N4 N3 C7 0.000(2) . .
B1 N4 N3 C7 180.000(2) . .
C9 N4 N3 Ni1 180.000(1) . .
B1 N4 N3 Ni1 0.000(1) . .
N1 Ni1 N3 C7 -136.06(8) 8_565 .
N1 Ni1 N3 C7 136.06(8) . .
Br1 Ni1 N3 C7 0.000(2) . .
N1 Ni1 N3 N4 43.94(8) 8_565 .
N1 Ni1 N3 N4 -43.94(8) . .
Br1 Ni1 N3 N4 180.000(1) . .
N1 N2 C4 C3 -2.0(3) . .
B1 N2 C4 C3 171.1(3) . .
N1 N2 C4 C5 176.3(3) . .
B1 N2 C4 C5 -10.6(5) . .
N2 N1 C2 C3 -1.8(3) . .
Ni1 N1 C2 C3 179.5(2) . .
N2 N1 C2 C1 175.6(3) . .
Ni1 N1 C2 C1 -3.1(5) . .
N3 N4 C9 C8 0.000(2) . .
B1 N4 C9 C8 180.000(2) . .
N3 N4 C9 C10 180.000(2) . .
B1 N4 C9 C10 0.000(3) . .
N4 N3 C7 C8 0.000(2) . .
Ni1 N3 C7 C8 180.000(2) . .
N4 N3 C7 C6 180.000(2) . .
Ni1 N3 C7 C6 0.000(3) . .
N3 C7 C8 C9 0.000(2) . .
C6 C7 C8 C9 180.000(2) . .
N4 C9 C8 C7 0.000(2) . .
C10 C9 C8 C7 180.000(2) . .
N1 C2 C3 C4 0.6(4) . .
C1 C2 C3 C4 -176.5(3) . .
N2 C4 C3 C2 0.8(3) . .
C5 C4 C3 C2 -177.3(3) . .
N3 C7 C6 F4 -60.6(3) . .
C8 C7 C6 F4 119.4(3) . .
N3 C7 C6 F4 60.6(3) . 8_565
C8 C7 C6 F4 -119.4(3) . 8_565
N3 C7 C6 F5 180.000(2) . .
C8 C7 C6 F5 0.000(2) . .
N1 C2 C1 F2 -41.5(4) . .
C3 C2 C1 F2 135.4(3) . .
N1 C2 C1 F3 -162.1(3) . .
C3 C2 C1 F3 14.8(5) . .
N1 C2 C1 F1 78.6(4) . .
C3 C2 C1 F1 -104.6(4) . .
C4 N2 B1 N2 -119.6(3) . 8_565
N1 N2 B1 N2 52.9(5) . 8_565
C4 N2 B1 N4 123.8(4) . .
N1 N2 B1 N4 -63.7(4) . .
C9 N4 B1 N2 -121.5(2) . .
N3 N4 B1 N2 58.5(2) . .
C9 N4 B1 N2 121.5(2) . 8_565
N3 N4 B1 N2 -58.5(2) . 8_565
