Dioxygen Activation and Substrate Oxygenation by a p-Nitrothiophenolatonickel Complex: Unique Effects of an Acetonitrile Solvent and the p-Nitro Group of the Ligand
Jun Nakazawa; Hiroyuki Ogiwara; Yusuke Kashiwazaki; Akiyoshi Ishii; Naoki Imamura; Yuya Samejima; Shiro Hikichi; Inorganic Chemistry 50 (2011) 9933–9935; doi:10.1021/ic201555f

data_4326565
_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
;
 Dioxygen Activation and Substrate Oxygenation by a
 p-Nitrothiophenolatonickel Complex: Unique Effects of an Acetonitrile
 Solvent and the p-Nitro Group of the Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9933
_journal_page_last               9935
_journal_paper_doi               10.1021/ic201555f
_journal_volume                  50
_journal_year                    2011
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         '2(C21 H26 B N7 Ni O2 S),(C7 H8)'
_chemical_formula_sum            'C49 H60 B2 N14 Ni2 O4 S2'
_chemical_formula_weight         1112.32
_chemical_name_common            '[Ni(TPMe,Me)(SPh-NO2)]'
_chemical_name_systematic
;
 [{Hydrotris(3,5-dimethylpyrazoryl)borato}{4-nitrothiophenolato}nickel(II)]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2009-08-25
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.0000(0)
_cell_angle_beta                 96.7699(36)
_cell_angle_gamma                90.0000(0)
_cell_formula_units_Z            2
_cell_length_a                   12.7330(7)
_cell_length_b                   15.1098(8)
_cell_length_c                   13.6871(9)
_cell_measurement_reflns_used    7740
_cell_measurement_temperature    113
_cell_measurement_theta_max      30.4322
_cell_measurement_theta_min      1.3477
_cell_volume                     2614.9(3)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_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    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      113
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -115.0000 - 65.0000
         Image width: 0.5000
            Exp time: 20.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 54.9317
              2theta: -24.8257
scan:
    Number of images: 360
               Slice: -115.0000 - 65.0000
         Image width: 0.5000
            Exp time: 20.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 54.9317
              2theta: -24.8257
scan:
    Number of images: 360
               Slice: -115.0000 - 65.0000
         Image width: 0.5000
            Exp time: 20.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 54.9317
              2theta: -24.8257

;
_diffrn_measurement_device
;
Saturn724 (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       \w
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0182
_diffrn_orient_matrix_UB_12      0.0757
_diffrn_orient_matrix_UB_13      0.0140
_diffrn_orient_matrix_UB_21      -0.0177
_diffrn_orient_matrix_UB_22      0.0157
_diffrn_orient_matrix_UB_23      -0.0618
_diffrn_orient_matrix_UB_31      -0.0664
_diffrn_orient_matrix_UB_32      0.0205
_diffrn_orient_matrix_UB_33      0.0242
_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  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0274
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7552
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         30.4322
_diffrn_reflns_theta_min         1.61
_diffrn_source_current           60.0000
_diffrn_source_power             3.0000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.858
_exptl_absorpt_correction_T_max  0.9249
_exptl_absorpt_correction_T_min  0.8142
_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    1.413
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          0.5000
_exptl_crystal_size_mid          0.1500
_exptl_crystal_size_min          0.1000
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.216
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         7291
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.216
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0431P)^2^+2.1749P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1097
_reflns_number_gt                6831
_reflns_number_total             7291
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic201555f_si_001_3.cif
_cod_data_source_block           1a_Ni(TpMe,Me)(SPh-NO2)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4326565