Sulfur-Bridged Early-Late Heterobimetallics Synthesized by Incorporation of Titanium, Vanadium, and Molybdenum into Bis(hydrosulfido) Templates of Group 9 Metals
Shigeki Kuwata; Tatsuya Nagano; Akihiro Matsubayashi; Youichi Ishii; Masanobu Hidai; Inorganic Chemistry 41 (2002) 4324–4330; doi:10.1021/ic020105y

data_4318385
_publ_contact_author_address
;
     Department of Chemistry and Biotechnology, Graduate School of 
Engineering, The University of Tokyo, Hongo, Bunkyo-ku, Tokyo 
113-8656, JAPAN
;
_publ_contact_author_email       ishii@chembio.t.u-tokyo.ac.jp
_publ_contact_author_fax         +81-3-5841-7265
_publ_contact_author_name        'Youichi ISHII'
_publ_contact_author_phone       +81-3-5841-7264
_publ_section_title
;
 Sulfur-Bridged Early-Late Heterobimetallics Synthesized by Incorporation
 of Titanium, Vanadium, and Molybdenum into Bis(hydrosulfido) Templates of
 Group 9 Metals
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4324
_journal_page_last               4330
_journal_paper_doi               10.1021/ic020105y
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'C17 H26 Ir Mo O4 P S2 '
_chemical_formula_sum            'C17 H26 Ir Mo O4 P S2'
_chemical_formula_weight         677.64
_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             'Tue Nov 14 20:16:27 2000'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 97.24(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.562(4)
_cell_length_b                   13.406(4)
_cell_length_c                   20.309(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294.2
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      19.8
_cell_volume                     2312.5(13)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    'DIRDIF92 (PATTY)'
_diffrn_ambient_temperature      294.2
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.10656
_diffrn_orient_matrix_UB_12      0.03104
_diffrn_orient_matrix_UB_13      -0.00135
_diffrn_orient_matrix_UB_21      0.04172
_diffrn_orient_matrix_UB_22      0.04657
_diffrn_orient_matrix_UB_23      0.03649
_diffrn_orient_matrix_UB_31      0.02766
_diffrn_orient_matrix_UB_32      0.04931
_diffrn_orient_matrix_UB_33      -0.03362
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.056
_diffrn_reflns_av_sigmaI/netI    0.040
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            5670
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.53
_diffrn_standards_decay_%        0.05
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.573
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.759
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            darkred
_exptl_crystal_density_diffrn    1.946
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1304.00
_exptl_crystal_size_max          0.900
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.300
_refine_diff_density_max         1.13
_refine_diff_density_min         -0.82
_refine_ls_extinction_coef       0.0036(1)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_ref   1.820
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     236
_refine_ls_number_reflns         4219
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.0060
_refine_ls_shift/su_mean         0.0010
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00006|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0313
_refine_ls_wR_factor_ref         0.0313
_reflns_number_gt                4219
_reflns_number_total             5321
_reflns_observed_criterion       >3.0sigma(I)
_cod_data_source_file            ic020105y_5.cif
_cod_data_source_block           Cp*IrP(m-SH)2Mo(CO)4](6b)
_cod_original_cell_volume        2312(1)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C17 H26 Ir Mo O4 P S2 '
_cod_database_code               4318385