First Cubane-like Polysulfidomolybdate: Synthesis and Crystal Structure of Cs6[Mo4S23.6]
Yuri V. Mironov; Anna S. Gardberg; James A. Ibers; Inorganic Chemistry 41 (2002) 1333–1334; doi:10.1021/ic011020k

data_4317657
_publ_section_title
;
 First Cubane-like Polysulfidomolybdate: Synthesis and Crystal Structure
 of Cs6[Mo4S23.6]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1333
_journal_page_last               1334
_journal_paper_doi               10.1021/ic011020k
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'Cs6 Mo4 S23.64'
_chemical_formula_weight         1939.12
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           216
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'F -4 2 3'
_symmetry_space_group_name_H-M   'F -4 3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.8436(7)
_cell_length_b                   15.8436(7)
_cell_length_c                   15.8436(7)
_cell_measurement_temperature    153(2)
_cell_volume                     3977.1(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_sigmaI/netI    0.0070
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12183
_diffrn_reflns_theta_full        28.17
_diffrn_reflns_theta_max         28.17
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    7.89
_exptl_crystal_density_diffrn    3.239
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3505
_refine_diff_density_max         1.177
_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.138
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         541
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0339P)^2^+106.3063P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0865
_reflns_number_gt                524
_reflns_number_total             541
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic011020k.cif
_cod_data_source_block           dis
_cod_database_code               4317657