Extreme Differences in Oxidation States: Synthesis and Structural Analysis of the Germanide Oxometallates A10[Ge9]2[WO4] As Well As A10+x[Ge9]2[W1-xNbxO4] with A = K and Rb Containing [Ge9]4- Polyanions
Viktor Hlukhyy; Thomas F. Fässler; Siméon Ponou; Sven Lidin; Natalia P. Ivleva; Reinhard Niessner; Inorganic Chemistry 51 (2012) 4058–4065; doi:10.1021/ic202234b

data_4328757
_publ_contact_author_address
;  Departement of Chemistry, Technische Universitaet Muenchen,
   Lichtenbergstrasse 4,
   85747 Garching, Germany
;
_publ_contact_author_email       Thomas.Faessler@lrz.tu-muenchen.de
_publ_contact_author_fax         '+49-(0) 89 289 13186'
_publ_contact_author_name        'Thomas F. Faessler'
_publ_contact_author_phone       '+49-(0) 89 289 13131'
_publ_section_title
;
 Extreme Differences in Oxidation States: Synthesis and Structural
 Analysis of the Germanide Oxometallates A10[Ge9]2[WO4] As Well As
 A10+x[Ge9]2[W1-xNbxO4] with A = K and Rb Containing [Ge9]4- Polyanions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4058
_journal_page_last               4065
_journal_paper_doi               10.1021/ic202234b
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'Ge18 K10.36 Nb0.36 O4 W0.64'
_chemical_formula_weight         1926.68
_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_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.050(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9079(10)
_cell_length_b                   15.9085(12)
_cell_length_c                   17.3829(13)
_cell_measurement_temperature    293(2)
_cell_volume                     3846.0(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Oxford XCalibur3 CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0769
_diffrn_reflns_av_sigmaI/netI    0.0610
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15358
_diffrn_reflns_theta_full        20.30
_diffrn_reflns_theta_max         20.30
_diffrn_reflns_theta_min         3.47
_exptl_absorpt_coefficient_mu    16.960
_exptl_absorpt_correction_T_max  0.0953
_exptl_absorpt_correction_T_min  0.0275
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            deep-red
_exptl_crystal_density_diffrn    3.327
_exptl_crystal_description       rod-shaped
_exptl_crystal_F_000             3468
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.980
_refine_diff_density_min         -1.957
_refine_diff_density_rms         0.267
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         3726
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0743
_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^)+(0.0972P)^2^+113.2930P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1819
_refine_ls_wR_factor_ref         0.1898
_reflns_number_gt                3251
_reflns_number_total             3726
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202234b_si_002_3.cif
_cod_data_source_block           K10.35Ge18W0.65Nb0.35O4_1b
_cod_database_code               4328757