Sulfur-Bridged Sandwich Cubane-Type Molybdenum-Antimony Cluster. Synthesis, X-ray Structure, and 121Sb Mössbauer Spectra of [(H2O)9Mo3S4SbS4Mo3(H2O)9](CH3C6H4SO3)8.24H2O
Genta Sakane; Kouichi Hashimoto; Masashi Takahashi; Masuo Takeda; Takashi Shibahara; Inorganic Chemistry 37 (1998) 4231–4234; doi:10.1021/ic971628m

data_4322950
_publ_contact_author
;
Prof. Takashi Shibahara
Departtment of Chemistry,
Okayama University of Science
1-1 Ridai-cho, Okayama 700-0005, Japan
;
_publ_contact_author_email       shiba@chem.ous.ac.jp
_publ_contact_author_fax         '+81 86 256 9443'
_publ_contact_author_phone       '+81 86 256 9443'
_publ_section_title
;
 Sulfur-Bridged Sandwich Cubane-Type Molybdenum-Antimony Cluster.
 Synthesis, X-ray Structure, and 121Sb M\"ossbauer Spectra of
 [(H2O)9Mo3S4SbS4Mo3(H2O)9](CH3C6H4SO3)8.24H2O
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4231
_journal_page_last               4234
_journal_paper_doi               10.1021/ic971628m
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C56 H140 Mo6 O66 S16 Sb'
_chemical_formula_weight         3080.03
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             'Tue Apr  7 21:55:35 1998'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                105.26(2)
_cell_angle_beta                 119.71(1)
_cell_angle_gamma                72.48(3)
_cell_formula_units_Z            1
_cell_length_a                   14.468(3)
_cell_length_b                   18.531(5)
_cell_length_c                   13.713(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298.2
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      10.0
_cell_volume                     3016.1(17)
_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      298.2
_diffrn_measurement_device_type  'Mac Science MXC-18'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.07570
_diffrn_orient_matrix_UB_12      -0.00870
_diffrn_orient_matrix_UB_13      -0.03546
_diffrn_orient_matrix_UB_21      -0.02062
_diffrn_orient_matrix_UB_22      0.02703
_diffrn_orient_matrix_UB_23      -0.06434
_diffrn_orient_matrix_UB_31      0.02112
_diffrn_orient_matrix_UB_32      -0.04958
_diffrn_orient_matrix_UB_33      0.04230
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.011
_diffrn_reflns_av_sigmaI/netI    0.024
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8300
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         0.00
_diffrn_reflns_theta_min         0.00
_diffrn_standards_decay_%        -25.63
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.192
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.794
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   '(Walker & Stuart, 1983)'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       unknown
_exptl_crystal_F_000             1563.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.73
_refine_diff_density_min         -0.36
_refine_ls_extinction_coef       0.0008(5)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_ref   1.332
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     649
_refine_ls_number_reflns         6593
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0000
_refine_ls_R_factor_gt           0.0000
_refine_ls_shift/su_max          0.0040
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00240|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0000
_refine_ls_wR_factor_ref         0.0747
_reflns_number_gt                0
_reflns_number_total             7898
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ic971628m.cif
_cod_data_source_block           '[(H2O)9Mo3S4SbS4Mo3(H2O)9](CH3C6H4SO3)8.24H2O'
_cod_original_cell_volume        3016(1)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C56 H140 Mo6 O66 S16 Sb '
_cod_database_code               4322950