Structural Characterization and Oxidation Reactivity of a Nickel(II) Acylperoxo Complex
Jun Nakazawa; Shota Terada; Masaki Yamada; Shiro Hikichi; Journal of the American Chemical Society 135 (2013) 6010–6013; doi:10.1021/ja4020277

data_4119662
_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         'C22 H17 B Cl F9 N6 Ni O2, C3.5 H4'
_chemical_formula_sum            'C25.5 H21 B Cl F9 N6 Ni O2'
_chemical_formula_weight         719.45
_chemical_name_common            '[Ni(TP CF3Me)mCBA] 0.5Toluene'
_chemical_name_systematic
;
[(3-Chlorobenzoato){Hydrotris(5-methyl-3-(trifluoro)methyl-
pyrazoryl)borato}nickel(II)] 0.5 toluene
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 94.212(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.350(3)
_cell_length_b                   8.5172(17)
_cell_length_c                   26.064(5)
_cell_measurement_reflns_used    8396
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.4839
_cell_measurement_theta_min      1.6665
_cell_volume                     2955.6(11)
_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      113.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 20.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 44.8163
              2theta: -20.1904
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 20.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 44.8163
              2theta: -20.1904

;
_diffrn_measurement_device
;
Saturn70 (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_method       \w
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0631
_diffrn_orient_matrix_UB_12      -0.0265
_diffrn_orient_matrix_UB_13      -0.0310
_diffrn_orient_matrix_UB_21      0.0632
_diffrn_orient_matrix_UB_22      -0.0512
_diffrn_orient_matrix_UB_23      -0.0847
_diffrn_orient_matrix_UB_31      0.0005
_diffrn_orient_matrix_UB_32      -0.0328
_diffrn_orient_matrix_UB_33      0.0202
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_av_sigmaI/netI    0.1571
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7160
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.6665
_diffrn_source_current           60.0000
_diffrn_source_power             3.0000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.840
_exptl_absorpt_correction_T_max  0.9032
_exptl_absorpt_correction_T_min  0.8471
_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            Green
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_description       Block
_exptl_crystal_F_000             1452
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.1500
_refine_diff_density_max         0.764
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         6712
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.188
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0658
_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^)+(0.0001P)^2^+3.6509P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1584
_refine_ls_wR_factor_ref         0.1613
_reflns_number_gt                5777
_reflns_number_total             6712
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja4020277_si_002_3.cif
_cod_data_source_block           02
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C25.50 H21 B Cl F9 N6 Ni O2'
_cod_database_code               4119662