Synthesis, Structure, and Properties of Alkaline-earth-substituted Tungstogermanate: [K2.5(H2O)1.5]2H3[Ca2(GeW11O39)(H2O)5]2·7H2O
Wang, Jingping; Han, Ruijuan; Du, Xiaodi; Niu, Jingyang; Chemistry Letters 37 (2008) 110–; doi:10.1246/cl.2008.110

data_8000180
_publ_section_title
;
 Synthesis, Structure, and Properties of Alkaline-earth-substituted
 Tungstogermanate: [K2.5(H2O)1.5]2H3[Ca2(GeW11O39)(H2O)5]2&#x00B7;7H2O
;
_journal_issue                   1
_journal_name_full               'Chemistry Letters'
_journal_page_first              110
_journal_paper_doi               10.1246/cl.2008.110
_journal_volume                  37
_journal_year                    2008
_chemical_formula_sum            'Ca4 Ge2 H43 K5 O98 W22'
_chemical_formula_weight         6157.04
_space_group_IT_number           15
_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                 113.268(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   41.05(5)
_cell_length_b                   13.854(17)
_cell_length_c                   19.29(2)
_cell_measurement_temperature    293(2)
_cell_volume                     10078(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.920
_diffrn_measured_fraction_theta_max 0.920
_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  0.1126
_diffrn_reflns_av_sigmaI/netI    0.1407
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22409
_diffrn_reflns_theta_full        25.16
_diffrn_reflns_theta_max         25.16
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    26.108
_exptl_absorpt_correction_T_max  0.2022
_exptl_absorpt_correction_T_min  0.1112
_exptl_crystal_density_diffrn    4.059
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             10776
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         3.991
_refine_diff_density_min         -2.042
_refine_diff_density_rms         0.456
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.907
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     600
_refine_ls_number_reflns         8318
_refine_ls_number_restraints     300
_refine_ls_restrained_S_all      0.890
_refine_ls_R_factor_all          0.1280
_refine_ls_R_factor_gt           0.0651
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0562P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1276
_refine_ls_wR_factor_ref         0.1467
_reflns_number_gt                4728
_reflns_number_total             8318
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            37-110sup1.cif
_cod_data_source_block           njy1
_cod_original_cell_volume        10075(22)
_cod_original_formula_sum        'H43 Ca4 Ge2 K5 O98 W22'
_cod_database_code               8000180