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_4326563
_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         'C25 H32 B N9 Ni O2 S, C2 H3 N'
_chemical_formula_sum            'C27 H35 B N10 Ni O2 S'
_chemical_formula_weight         633.23
_chemical_name_common            '[Ni(TpMe,Me)(SPh-NO2)(MeCN)2]MeCN'
_chemical_name_systematic
;
 [{Hydrotris(3,5-dimethylpyrazoryl)borato}{4-methoxythiophenolato}
(diacetonitrile)nickel(II)] acetonitrile
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2010-03-6
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.167(20)
_cell_angle_beta                 98.872(23)
_cell_angle_gamma                107.454(25)
_cell_formula_units_Z            2
_cell_length_a                   10.687(10)
_cell_length_b                   12.383(7)
_cell_length_c                   12.968(3)
_cell_measurement_reflns_used    236
_cell_measurement_temperature    113
_cell_measurement_theta_max      30.0348
_cell_measurement_theta_min      1.5909
_cell_measurement_wavelength     0.71073
_cell_volume                     1615.3(18)
_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
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.874
_diffrn_measured_fraction_theta_max 0.739
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -115.0000 - 65.0000
         Image width: 0.5000
            Exp time: 30.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 54.7963
              2theta: -25.1763
scan:
    Number of images: 360
               Slice: -115.0000 - 65.0000
         Image width: 0.5000
            Exp time: 30.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 54.7963
              2theta: -25.1763
scan:
    Number of images: 360
               Slice: -115.0000 - 65.0000
         Image width: 0.5000
            Exp time: 30.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 54.7963
              2theta: -25.1763

;
_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      0.0138
_diffrn_orient_matrix_UB_12      0.0979
_diffrn_orient_matrix_UB_13      0.0105
_diffrn_orient_matrix_UB_21      -0.0668
_diffrn_orient_matrix_UB_22      0.0311
_diffrn_orient_matrix_UB_23      0.0419
_diffrn_orient_matrix_UB_31      0.0378
_diffrn_orient_matrix_UB_32      0.0003
_diffrn_orient_matrix_UB_33      0.0684
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710747
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_sigmaI/netI    0.2072
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7048
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.12
_diffrn_reflns_theta_min         1.59
_diffrn_source_current           60.0000
_diffrn_source_power             3.0000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.706
_exptl_absorpt_correction_T_max  0.9349
_exptl_absorpt_correction_T_min  0.8951
_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    1.302
_exptl_crystal_description       block
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.1500
_exptl_crystal_size_mid          0.1500
_exptl_crystal_size_min          0.1000
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         7048
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0414P)^2^+0.1000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1120
_refine_ls_wR_factor_ref         0.1108
_reflns_number_gt                4240
_reflns_number_total             7048
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic201555f_si_001_1.cif
_cod_data_source_block           1a_prime_[Ni(TpMe,Me)(SPh-NO2)(MeCN)2]MeCN
_cod_original_cell_volume        1615.4(18)
_cod_database_code               4326563