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_4344049
_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, 8(H2 O), 1.80(H4 N), 4.20(Cs)
;
_chemical_formula_sum            'Cs4.2 Ge6 H29.2 N1.8 O32'
_chemical_formula_weight         1560.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.2960(10)
_cell_angle_beta                 97.1230(10)
_cell_angle_gamma                90.8290(10)
_cell_formula_units_Z            1
_cell_length_a                   7.8960(8)
_cell_length_b                   10.2383(11)
_cell_length_c                   10.4517(11)
_cell_measurement_reflns_used    7514
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      30.618
_cell_measurement_theta_min      2.600
_cell_volume                     838.30(15)
_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  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEX II'
_diffrn_measurement_method       \w
_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  0.0162
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9278
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         2.60
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.912
_exptl_absorpt_correction_T_max  0.5044
_exptl_absorpt_correction_T_min  0.1995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.091
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             721
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.019
_refine_diff_density_min         -1.063
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       0.00124(17)
_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   1.151
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         4438
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0202
_refine_ls_R_factor_gt           0.0189
_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^)+(0.0186P)^2^+0.8675P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0459
_refine_ls_wR_factor_ref         0.0464
_reflns_number_gt                4246
_reflns_number_total             4438
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic5b01293_si_003.cif
_cod_data_source_block           b
_cod_depositor_comments
'Adding full bibliography for 4344048--4344049.cif.'
_cod_original_formula_sum        'Cs4.20 Ge6 H29.20 N1.80 O32'
_cod_database_code               4344049