Syntheses and Structures of Mixed-Metal Sulfido Clusters Containing Incomplete Cubane-Type M2M'S4 and Cubane-Type M2M'2S4 Cores (M = Mo, W; M' = Rh, Ir)
Tomotake Ikada; Shigeki Kuwata; Yasushi Mizobe; Masanobu Hidai; Inorganic Chemistry 38 (1999) 64–69; doi:10.1021/ic981035r

data_4321729
_publ_contact_author
;
    Masanobu Hidai
 Department of Chemstry and Biotechnology, Graduate Scool of Engineering, Th
e University of Tokyo, Hongo, Tokyo 113-8656, Japan
;
_publ_contact_author_email       ' hidai@chembio.t.u-tokyo.ac.jp '
_publ_contact_author_fax         ' 81-3-5800-6945 '
_publ_contact_author_phone       ' 81-3-5800-6945 '
_publ_section_title
;
 Syntheses and Structures of Mixed-Metal Sulfido Clusters Containing
 Incomplete Cubane-Type M2M'S4 and Cubane-Type M2M'2S4 Cores (M = Mo, W;
 M' = Rh, Ir)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              64
_journal_page_last               69
_journal_paper_doi               10.1021/ic981035r
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C48 H54 Cl5 Ir N2 P2 S8 W2'
_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             'Sat Aug 22 15:42:50 1998'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 96.34(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4.00
_cell_length_a                   10.521(4)
_cell_length_b                   32.325(5)
_cell_length_c                   17.277(3)
_cell_measurement_reflns_used    18
_cell_measurement_temperature    23.0
_cell_measurement_theta_max      28.77
_cell_measurement_theta_min      20.03
_cell_volume                     5840(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)'
_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      0.02197
_diffrn_orient_matrix_UB_12      0.01686
_diffrn_orient_matrix_UB_13      0.04814
_diffrn_orient_matrix_UB_21      -0.00438
_diffrn_orient_matrix_UB_22      -0.02541
_diffrn_orient_matrix_UB_23      0.03261
_diffrn_orient_matrix_UB_31      0.09297
_diffrn_orient_matrix_UB_32      -0.00518
_diffrn_orient_matrix_UB_33      -0.00323
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  14.58
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11098
_diffrn_reflns_theta_max         24.9948
_diffrn_standards_decay_%        1.21
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu_cm 68.182
_exptl_absorpt_correction_T_max  0.905
_exptl_absorpt_correction_T_min  0.419
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.950
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3296.00
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_exptl_crystal_size_min          0.200
_refine_diff_density_max         -1.51230
_refine_diff_density_min         2.05490
_refine_ls_extinction_coef       0.58740
_refine_ls_extinction_method     Zachariasen_type_2_Gaussian_isotropic
_refine_ls_goodness_of_fit_obs   1.900
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         4472
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0710
_refine_ls_shift/esd_max         0.0330
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0680
_cod_data_source_file            ic981035r_1.cif
_cod_data_source_block           '[Ir(PPh3)2blabla'
_cod_original_cell_volume        5839(2)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C48 H54 N2 P2 S8 Ir W2 Cl5'
_cod_database_code               4321729