Potassium, Cesium, and Ammonium Peroxogermanates with Inorganic Hexanuclear Peroxo Bridged Germanium Anion Isolated from Aqueous Solution.
Medvedev, Alexander G.; Mikhaylov, Alexey A.; Churakov, Andrei V.; Vener, Mikhail V.; Tripol'skaya, Tatiana A.; Cohen, Shmuel; Lev, Ovadia; Prikhodchenko, Petr V.; Inorganic chemistry 54 (2015) 8058–8065; doi:10.1021/acs.inorgchem.5b01293

data_4344048
_publ_section_title
;
 Potassium, Cesium, and Ammonium Peroxogermanates with Inorganic
 Hexanuclear Peroxo Bridged Germanium Anion Isolated from Aqueous
 Solution.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8058
_journal_page_last               8065
_journal_paper_doi               10.1021/acs.inorgchem.5b01293
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'Ge6 H6 O24, 14(H2 O), 6(K)'
_chemical_formula_sum            'Ge6 H34 K6 O38'
_chemical_formula_weight         1312.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 107.188(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.9695(13)
_cell_length_b                   12.7455(16)
_cell_length_c                   14.6041(19)
_cell_measurement_reflns_used    9909
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      30.501
_cell_measurement_theta_min      2.164
_cell_volume                     1772.8(4)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       '<i>APEX2</i> (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX II'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19201
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.999
_diffrn_reflns_theta_min         2.670
_exptl_absorpt_coefficient_mu    5.848
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4698
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.459
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       0.00110(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         4714
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0181
_refine_ls_R_factor_gt           0.0169
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0195P)^2^+1.6805P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0421
_refine_ls_wR_factor_ref         0.0426
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4533
_reflns_number_total             4714
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01293_si_002.cif
_cod_data_source_block           b
_cod_depositor_comments
'Adding full bibliography for 4344048--4344049.cif.'
_cod_database_code               4344048
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.234
_shelx_estimated_absorpt_t_max   0.388
_shelx_res_checksum              89805
_shelx_hkl_checksum              7450