Vanadogermanate Cluster Anions
T. Whitfield; X. Wang; A. J. Jacobson; Inorganic Chemistry 42 (2003) 3728–3733; doi:10.1021/ic0206185

data_4313740
_publ_section_title
;
 Vanadogermanate Cluster Anions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3728
_journal_page_last               3733
_journal_paper_doi               10.1021/ic0206185
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'Cs8 Ge4 H9.5 O50.75 V16'
_chemical_formula_weight         2990.26
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 101.3760(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   44.513(2)
_cell_length_b                   12.7632(7)
_cell_length_c                   22.9233(12)
_cell_measurement_temperature    293(2)
_cell_volume                     12767.5(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.910
_diffrn_measured_fraction_theta_max 0.910
_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  0.0859
_diffrn_reflns_av_sigmaI/netI    0.0844
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_h_min       -59
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            39019
_diffrn_reflns_theta_full        28.48
_diffrn_reflns_theta_max         28.48
_diffrn_reflns_theta_min         0.93
_exptl_absorpt_coefficient_mu    8.660
_exptl_crystal_density_diffrn    3.111
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             10812
_refine_diff_density_max         2.499
_refine_diff_density_min         -2.439
_refine_diff_density_rms         0.315
_refine_ls_extinction_coef       0.000058(10)
_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   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     792
_refine_ls_number_reflns         14692
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1280
_refine_ls_R_factor_gt           0.0788
_refine_ls_shift/su_max          0.916
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0922P)^2^+346.1017P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1839
_refine_ls_wR_factor_ref         0.2119
_reflns_number_gt                9692
_reflns_number_total             14692
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0206185_1.cif
_cod_data_source_block           sad
_cod_original_cell_volume        12767.7(12)
_cod_original_formula_sum        'H9.50 Cs8 Ge4 O50.75 V16'
_cod_database_code               4313740