Synthesis and characterization of a twin Cubane-type molybdenum-rhodium-sulfur cluster, [{Mo3RhCp*S4(H2O)7(O)}2]8+. X-ray structure of [{Mo3RhCpS4(H2O7O}2](CH3C6H4SO3)(8).14H2O.
Akashi, Haruo; Isobe, Kiyoshi; Shibahara, Takashi; Inorganic Chemistry 44 (2005) 3494–3498; doi:10.1021/ic048733y

data_4340411
_publ_section_title
;
 Synthesis and characterization of a twin Cubane-type
 molybdenum-rhodium-sulfur cluster, [{Mo3RhCp*S4(H2O)7(O)}2]8+.
 X-ray structure of [{Mo3RhCpS4(H2O7O}2](CH3C6H4SO3)(8).14H2O.
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   10
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3494
_journal_page_last               3498
_journal_paper_doi               10.1021/ic048733y
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C76 H142 Mo6 O54 Rh2 S16'
_chemical_formula_sum            'C76 H142 Mo6 O54 Rh2 S16'
_chemical_formula_weight         3214.34
_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'
_cell_angle_alpha                63.704(3)
_cell_angle_beta                 78.688(2)
_cell_angle_gamma                81.038(2)
_cell_formula_units_Z            1
_cell_length_a                   12.2631(8)
_cell_length_b                   15.911(1)
_cell_length_c                   17.389(3)
_cell_measurement_reflns_used    7019
_cell_measurement_temperature    93.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     2973.5(6)
_computing_cell_refinement       CRYSTALCLEAR
_computing_data_collection       CRYSTALCLEAR
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.6.0'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 7.32
_diffrn_measured_fraction_theta_full 0.9960
_diffrn_measured_fraction_theta_max 0.9861
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.073
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33644
_diffrn_reflns_theta_full        25.75
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    1.249
_exptl_absorpt_correction_T_max  0.939
_exptl_absorpt_correction_T_min  0.695
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1628.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.61
_refine_diff_density_min         -3.49
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     737
_refine_ls_number_reflns         11328
_refine_ls_R_factor_gt           0.0610
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0010Fo^2^ + 1.0000\s(Fo^2^) + 0.5000]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1630
_reflns_number_gt                7661
_reflns_number_total             13440
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic048733ysi20040923_125311.cif
_cod_data_source_block           010214B
_cod_depositor_comments
;

2025-01-22
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         1607.17
_cod_original_formula_moiety         'C38 H71 Mo3 O27 Rh1 S8'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        2973.5(5)
_cod_original_formula_sum        'C38 H71 Mo3 O27 Rh1 S8'
_cod_database_code               4340411