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_4328755
_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 O4 Rb10 W'
_chemical_formula_weight         2409.17
_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                 90.078(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.3230(7)
_cell_length_b                   15.9060(9)
_cell_length_c                   17.8634(9)
_cell_measurement_temperature    150(2)
_cell_volume                     4069.7(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1504
_diffrn_reflns_av_sigmaI/netI    0.1929
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14274
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    27.773
_exptl_absorpt_correction_T_max  0.2930
_exptl_absorpt_correction_T_min  0.1268
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            ruby-red
_exptl_crystal_density_diffrn    3.932
_exptl_crystal_description       rod-shaped
_exptl_crystal_F_000             4208
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         4.580
_refine_diff_density_min         -2.450
_refine_diff_density_rms         0.535
_refine_ls_extinction_coef       0.00023(11)
_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   1.011
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         7157
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1634
_refine_ls_R_factor_gt           0.1177
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1627P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2757
_refine_ls_wR_factor_ref         0.3015
_reflns_number_gt                4318
_reflns_number_total             7157
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202234b_si_002_1.cif
_cod_data_source_block           Rb10Ge18WO4_4b
_cod_database_code               4328755