Synthesis and Crystal Structure of a Novel Germanate: (NH4)4[(GeO2)3(GeO1.5F3)2].0.67H2O
Tony Conradsson; Xiaodong Zou; Mike S. Dadachov; Inorganic Chemistry 39 (2000) 1716–1720; doi:10.1021/ic9911217

data_4320872
_publ_section_title
;
 Synthesis and Crystal Structure of a Novel Germanate:
 (NH4)4[(GeO2)3(GeO1.5F3)2].0.67H2O
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1716
_journal_page_last               1720
_journal_paper_doi               10.1021/ic9911217
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'F24 Ge20 H69.34 N16 O38.67'
_chemical_formula_weight         2820.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   7.0065(4)
_cell_length_b                   11.7976(6)
_cell_length_c                   19.5200(14)
_cell_measurement_temperature    293(2)
_cell_volume                     1613.52(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0536
_diffrn_reflns_av_sigmaI/netI    0.0313
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11805
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    9.324
_exptl_crystal_density_diffrn    2.903
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1347
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.139
_refine_ls_extinction_coef       0.00201(15)
_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   0.767
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         1582
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      0.763
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0223
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0514
_refine_ls_wR_factor_ref         0.0544
_reflns_number_gt                1312
_reflns_number_total             1582
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9911217.cif
_cod_data_source_block           (NH4)4[(GeO2)3(GeO1.5F3)2].0.67H2O
_cod_original_formula_sum        'H69.34 F24 Ge20 N16 O38.67'
_cod_database_code               4320872