A three-dimensional open-framework germanate containing four-, five- and six-coordinated germanium
Sun, Kai; Dadachov, Mike S.; Conradsson, Tony; Zou, Xiaodong; Acta Crystallographica Section C 56 (2000) 1092–1094; doi:10.1107/S0108270100009057

data_2011343
_publ_section_title
;
 A three-dimensional open-framework germanate containing four-, five-
 and six-coordinated germanium
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1092
_journal_page_last               1094
_journal_paper_doi               10.1107/S0108270100009057
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac          '(C2 H8 N2 )(C2 H10 N2 )2 [H4 Ge9 O22 ]'
_chemical_formula_moiety         'C6 H32 Ge9 N6 O22'
_chemical_formula_sum            'C6 H32 Ge9 N6 O22'
_chemical_formula_weight         1193.68
_chemical_name_common            '[(H2NC2H4NH2)(H3NC2H4NH3)2][Ge9O18(OH)4]'
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.695(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.1958(15)
_cell_length_b                   9.9753(10)
_cell_length_c                   13.1655(19)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.98
_cell_measurement_theta_min      2.86
_cell_volume                     1338.9(3)
_computing_cell_refinement       'CELL (Stoe & Cie, 1997b)'
_computing_data_collection       'EXPOSE (Stoe & Cie, 1997b)'
_computing_data_reduction        'INTEGRATE (Stoe & Cie, 1997b)'
_computing_molecular_graphics    'DIAMOND (Bergerhoff, 1996)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.0
_diffrn_measured_fraction_theta_full .987
_diffrn_measured_fraction_theta_max .987
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       '\f-oscill., \f-incr. = 1.5\%; 133 exposures'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0581
_diffrn_reflns_av_sigmaI/netI    .0450
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10190
_diffrn_reflns_theta_full        25.98
_diffrn_reflns_theta_max         25.98
_diffrn_reflns_theta_min         2.86
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    10.059
_exptl_absorpt_correction_T_max  .7212
_exptl_absorpt_correction_T_min  .5769
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(XRED; Stoe & Cie, 1997a)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.961
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1148
_exptl_crystal_size_max          .060
_exptl_crystal_size_mid          .040
_exptl_crystal_size_min          .038
_refine_diff_density_max         .799
_refine_diff_density_min         -.626
_refine_ls_extinction_coef       .00047(18)
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   .958
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         2598
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      .958
_refine_ls_R_factor_all          .0406
_refine_ls_R_factor_gt           .0268
_refine_ls_shift/su_max          .041
_refine_ls_shift/su_mean         .002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0315P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .0579
_reflns_number_gt                2077
_reflns_number_total             2598
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            os1114.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2011343