(C~4~N~2~H~12~)[(GeO~2~)~3~(BO~1.5~F)~2~], a layered borogermanate containing three- and nine-membered rings
Li, Yang-feng; Zou, Xiaodong; Acta Crystallographica Section C 59 (2003) m471–m472; doi:10.1107/S0108270103021747

data_2013720
_publ_section_title
;
 (C~4~N~2~H~12~)[(GeO~2~)~3~(BO~1.5~F)~2~], a layered borogermanate
 containing three- and nine-membered rings
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m471
_journal_page_last               m472
_journal_paper_doi               10.1107/S0108270103021747
_journal_volume                  59
_journal_year                    2003
_chemical_formula_moiety         'B2 F2 Ge3 O9, C4 H12 N2'
_chemical_formula_sum            'C4 H12 B2 F2 Ge3 N2 O9'
_chemical_formula_weight         509.54
_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            4
_cell_length_a                   6.9776(14)
_cell_length_b                   11.779(2)
_cell_length_c                   15.997(3)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.90
_cell_measurement_theta_min      3.39
_cell_volume                     1314.8(4)
_computing_cell_refinement       'CELL (Stoe & Cie, 1997)'
_computing_data_collection       'EXPOSURE (Stoe & Cie, 1997)'
_computing_data_reduction        'INTEGRATE (Stoe & Cie, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2000)'
_computing_publication_material  SHELXL97
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       '\f-oscill., \f-incr.=1.4\%; 129 exposure'
_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  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0200
_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       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8492
_diffrn_reflns_theta_full        25.90
_diffrn_reflns_theta_max         25.90
_diffrn_reflns_theta_min         3.39
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    6.888
_exptl_absorpt_correction_T_max  0.5579
_exptl_absorpt_correction_T_min  0.4436
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(XRED; Stoe & Cie, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.574
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.401
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         1278
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0192
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0299P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0442
_refine_ls_wR_factor_ref         0.0455
_reflns_number_gt                1092
_reflns_number_total             1278
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tr1066.cif
_cod_data_source_block           I
_cod_database_code               2013720
_cod_database_fobs_code          2013720