Preparation, Structure, and Reactivity of Ge-Containing Heterometallic Cube Derivatives of [M3E4(H2O)9]4+ (M = Mo, W; E = S, Se)
Mi-Sook Seo; Vladimir P. Fedin; Maxim N. Sokolov; Rita Hernandez-Molina; Achim Sokolowski; Mark R. J. Elsegood; William Clegg; A. Geoffrey Sykes; Inorganic Chemistry 40 (2001) 6115–6122; doi:10.1021/ic010256l

data_4320558
_publ_section_title
;
 Preparation, Structure, and Reactivity of Ge-Containing Heterometallic
 Cube Derivatives of [M3E4(H2O)9]4+ (M = Mo, W; E = S, Se)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6115
_journal_page_last               6122
_journal_paper_doi               10.1021/ic010256l
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C56 H108 Ge Mo6 O50 S8 Se8'
_chemical_formula_weight         3117.81
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   'geom except H2O-H coords freely refined'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.437(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.3558(5)
_cell_length_b                   34.0069(13)
_cell_length_c                   11.9249(5)
_cell_measurement_reflns_used    11925
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      2.48
_cell_volume                     5006.1(3)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device_type  'Bruker SMART CCD difractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.0530
_diffrn_reflns_av_sigmaI/netI    0.1097
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            32370
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.38
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.189
_exptl_absorpt_correction_T_max  0.885
_exptl_absorpt_correction_T_min  0.348
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.068
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3056
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.145
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.139
_refine_ls_extinction_coef       0.00025(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.873
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     666
_refine_ls_number_reflns         11466
_refine_ls_number_restraints     403
_refine_ls_restrained_S_all      0.863
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0269P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0762
_reflns_number_gt                6992
_reflns_number_total             11466
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010256l_3.cif
_cod_data_source_block           ags35
_cod_database_code               4320558