Preparation of Cationic Dinuclear Hydrido Complexes of Ruthenium, Rhodium, and Iridium with Bridging Thiolato Ligands and Their Reactions with Nitrosobenzene
Takafumi Iwasa; Hitoshi Shimada; Atsushi Takami; Hiroyuki Matsuzaka; Youichi Ishii; Masanobu Hidai; Inorganic Chemistry 38 (1999) 2851–2859; doi:10.1021/ic981274e

data_4322075
_publ_contact_author
;
    Masanobu Hidai
  Department of Chemistry and Biotechnology, Graduate School of Engineering,
  The University of Tokyo, Hongo, Bunkyo-Ku, Tokyo 113-8656, Japan
;
_publ_contact_author_fax         ' +81-3-5800-6945 '
_publ_contact_author_phone       ' +81-3-3812-2111 ext 7261 '
_publ_section_title
;
 Preparation of Cationic Dinuclear Hydrido Complexes of Ruthenium,
 Rhodium, and Iridium with Bridging Thiolato Ligands and Their Reactions
 with Nitrosobenzene
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2851
_journal_page_last               2859
_journal_paper_doi               10.1021/ic981274e
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C56 H69 B Ir2 N O S2'
_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'
_audit_creation_date             'Fri Jun  5 12:26:02 1998'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 90.91(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4.00
_cell_length_a                   11.031(5)
_cell_length_b                   24.316(5)
_cell_length_c                   19.226(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    23.0
_cell_measurement_theta_max      39.94
_cell_measurement_theta_min      36.41
_cell_volume                     5156(3)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan: PROCESS (MSC)'
_computing_publication_material  'teXsan: FINISH (MSC)'
_computing_structure_refinement  'teXsan: LS (MSC)'
_diffrn_ambient_temperature      23.0
_diffrn_measurement_device       AFC7R
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_orient_matrix_UB_11      0.00066
_diffrn_orient_matrix_UB_12      -0.02086
_diffrn_orient_matrix_UB_13      0.04483
_diffrn_orient_matrix_UB_21      -0.00031
_diffrn_orient_matrix_UB_22      0.03544
_diffrn_orient_matrix_UB_23      0.02638
_diffrn_orient_matrix_UB_31      -0.09066
_diffrn_orient_matrix_UB_32      -0.00027
_diffrn_orient_matrix_UB_33      -0.00059
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  5.06
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9826
_diffrn_reflns_theta_max         25.0105
_diffrn_reflns_theta_min         2.515
_diffrn_standards_decay_%        -0.33
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu_cm 52.903
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.509
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            darkbrown
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2444.00
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.350
_refine_diff_density_max         -1.08880
_refine_diff_density_min         1.17420
_refine_ls_extinction_coef       0.94785
_refine_ls_extinction_method     Zachariasen_type_2_Gaussian_isotropic
_refine_ls_goodness_of_fit_obs   1.830
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         5336
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0380
_refine_ls_shift/esd_max         0.0620
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0260
_cod_data_source_file            ic981274e_6.cif
_cod_data_source_block
'[Cp*Ir(-PhNO)(-SPri)2IrCp*][BPh4](Compound10b)'
_cod_depositor_comments
;
 Changing the values of the _geom_angle_atom_site_label_1,
 _geom_angle_atom_site_label_2, _geom_angle_atom_site_label_3,
 _geom_bond_atom_site_label_1 and _geom_bond_atom_site_label_2
 data items to match the _atom_site_label data item values.

 Antanas Vaitkus,
 2017-01-29
;
_cod_original_cell_volume        5156(2)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C56 H69 Ir2 S2 B N O'
_cod_database_code               4322075