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_4320556
_publ_section_title
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 Preparation, Structure, and Reactivity of Ge-Containing Heterometallic
 Cube Derivatives of [M3E4(H2O)9]4+ (M = Mo, W; E = S, Se)
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_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 H148 Ge Mo6 O70 S16'
_chemical_formula_weight         3102.93
_chemical_name_systematic
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?
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_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.984(2)
_cell_angle_beta                 104.680(2)
_cell_angle_gamma                118.056(2)
_cell_formula_units_Z            1
_cell_length_a                   13.5499(10)
_cell_length_b                   14.0334(10)
_cell_length_c                   18.4296(13)
_cell_measurement_reflns_used    13084
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.75
_cell_measurement_theta_min      2.22
_cell_volume                     2930.8(4)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.859
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_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  0.0214
_diffrn_reflns_av_sigmaI/netI    0.0529
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18952
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.86
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.259
_exptl_absorpt_correction_T_max  0.647
_exptl_absorpt_correction_T_min  0.573
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.224
_refine_diff_density_min         -1.488
_refine_diff_density_rms         0.148
_refine_ls_extinction_coef       0.00012(15)
_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   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     876
_refine_ls_number_reflns         13214
_refine_ls_number_restraints     647
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0595
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+23.4752P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1372
_refine_ls_wR_factor_ref         0.1438
_reflns_number_gt                10685
_reflns_number_total             13214
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010256l_1.cif
_cod_data_source_block           ags23
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+23.4752P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+23.4752P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4320556