Synthesis, Structures, and Redox Properties of Octa(μ3-sulfido)hexarhenium(III) Complexes Having Terminal Pyridine Ligands
Takashi Yoshimura; Keisuke Umakoshi; Yoichi Sasaki; A. Geoffrey Sykes; Inorganic Chemistry 38 (1999) 5557–5564; doi:10.1021/ic9907922

data_4322441
_publ_contact_author_address
;
            Pr Yoichi Sasaki
    Division of Chemistry
    Graduate School of Science
    Hokkaido University
    Kita-ku, Sapporo 060-0810
    Japan
;
_publ_contact_author_email       ysasaki@science.hokudai.ac.jp
_publ_contact_author_fax         +81-11-706-3447
_publ_contact_author_name        ' Sasaki, Yoichi '
_publ_contact_author_phone       +81-11-706-3817
_publ_section_title
;
 Synthesis, Structures, and Redox Properties of
 Octa(\m3-sulfido)hexarhenium(III) Complexes Having Terminal Pyridine
 Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5557
_journal_page_last               5564
_journal_paper_doi               10.1021/ic9907922
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C31 H51 Cl3 N4 Re6 S8'
_chemical_formula_weight         1959.85
_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'
_cell_angle_alpha                90
_cell_angle_beta                 108.94(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.156(5)
_cell_length_b                   19.760(5)
_cell_length_c                   18.895(4)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      14.8
_cell_measurement_theta_min      12.1
_cell_volume                     5706(3)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device_type  'Rigaku AFC5R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.01177
_diffrn_orient_matrix_UB_12      -0.04921
_diffrn_orient_matrix_UB_13      -0.01108
_diffrn_orient_matrix_UB_21      -0.04626
_diffrn_orient_matrix_UB_22      0.00117
_diffrn_orient_matrix_UB_23      0.02458
_diffrn_orient_matrix_UB_31      -0.04477
_diffrn_orient_matrix_UB_32      0.01175
_diffrn_orient_matrix_UB_33      -0.04903
_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  0.068
_diffrn_reflns_av_sigmaI/netI    0.112
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13543
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.06
_diffrn_standards_decay_%        1.40
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    13.304
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.328
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'North, Phillips & Mathews, 1968'
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    2.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             3576.00
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.16
_refine_diff_density_min         -1.06
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.617
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     384
_refine_ls_number_reflns         6675
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.3860
_refine_ls_shift/su_mean         0.0560
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00063|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0735
_reflns_number_gt                6675
_reflns_number_total             13090
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ic9907922_3.cif
_cod_data_source_block           (Bu4N)[mer-{Re6S8Cl3(py)3}]
_cod_original_cell_volume        5705(2)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C31 H51 Cl3 N4 S8 Re6 '
_cod_database_code               4322441