Synthesis and Characterization of a Novel Organically Templated Open Framework Zirconogermanate with Three- and Seven-Membered Rings
Zhicheng Liu; Linhong Weng; Zhenxia Chen; Dongyuan Zhao; Inorganic Chemistry 42 (2003) 5960–5965; doi:10.1021/ic0343612

data_4314243
_publ_section_title
;
 Synthesis and Characterization of a Novel Organically Templated Open
 Framework Zirconogermanate with Three- and Seven-Membered Rings
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5960
_journal_page_last               5965
_journal_paper_doi               10.1021/ic0343612
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C2 H12 Ge3 N2 O10 Zr'
_chemical_formula_sum            'C2 H12 Ge3 N2 O10 Zr'
_chemical_formula_weight         533.13
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_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                 104.826(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.299(3)
_cell_length_b                   7.7649(19)
_cell_length_c                   13.835(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1173.4(5)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics
;
DS Viewerpro (Accelrys, 2002)
;
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Nonius KappaCCDr'
_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  0.0205
_diffrn_reflns_av_sigmaI/netI    0.0544
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            2760
_diffrn_reflns_theta_full        27.11
_diffrn_reflns_theta_max         27.11
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    8.524
_exptl_absorpt_correction_T_max  0.6752
_exptl_absorpt_correction_T_min  0.2805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.018
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangle plate'
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.819
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.020(10)
_refine_ls_extinction_coef       0.00069(10)
_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   0.928
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         2133
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0263
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0077P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0529
_refine_ls_wR_factor_ref         0.0537
_reflns_number_gt                1803
_reflns_number_total             2133
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0343612si20030403_053357.cif
_cod_data_source_block           FDZG-3
_cod_database_code               4314243