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_4322073
_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
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_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            'C33 H49 F3 N O4 Ru2 S3'
_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'
_audit_creation_date             'Fri Jun  5 12:28:39 1998'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 95.48(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4.00
_cell_length_a                   14.802(3)
_cell_length_b                   12.929(4)
_cell_length_c                   19.735(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    23.0
_cell_measurement_theta_max      38.93
_cell_measurement_theta_min      28.35
_cell_volume                     3759.5(15)
_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)'
_computing_structure_solution    'DIRDIF92 (PATTY)'
_diffrn_ambient_temperature      23.0
_diffrn_measurement_device       AFC7R
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_orient_matrix_UB_11      -0.05658
_diffrn_orient_matrix_UB_12      0.01964
_diffrn_orient_matrix_UB_13      -0.02890
_diffrn_orient_matrix_UB_21      -0.03147
_diffrn_orient_matrix_UB_22      0.01240
_diffrn_orient_matrix_UB_23      0.04190
_diffrn_orient_matrix_UB_31      0.02035
_diffrn_orient_matrix_UB_32      0.07377
_diffrn_orient_matrix_UB_33      0.00065
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  3.11
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9373
_diffrn_reflns_theta_max         27.4946
_diffrn_reflns_theta_min         2.60
_diffrn_standards_decay_%        -0.75
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu_cm 10.210
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.932
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            darkbrown
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1796.00
_exptl_crystal_size_max          0.900
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         -0.61080
_refine_diff_density_min         0.48340
_refine_ls_extinction_coef       0.15270
_refine_ls_extinction_method     Zachariasen_type_2_Gaussian_isotropic
_refine_ls_goodness_of_fit_obs   1.530
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         5119
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0420
_refine_ls_shift/esd_max         0.4210
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0300
_cod_data_source_file            ic981274e_4.cif
_cod_data_source_block           '[Cp*Ru(-PhNO)(-SPri)2RuCp*][OTf](Compound8)'
_cod_original_cell_volume        3759(1)
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C33 H49 Ru2 S3 F3 N O4'
_cod_database_code               4322073
_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
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