Synthesis of Thermally Stable Extra-Large Pore Crystalline Materials: A Uranyl Germanate with 12-Ring Channels
Chia-Hui Lin; Ray-Kuang Chiang; Kwang-Hwa Lii; Journal of the American Chemical Society 131 (2009) 2068–2069; doi:10.1021/ja8084143

data_4103912
_publ_contact_author
;
Kwang-Hwa Lii
Department of Chemistry
National Central University
Jhongli, Taiwan 320
;
_publ_contact_author_email
;
liikh@cc.ncu.edu.tw
;
_publ_section_title
;
 Synthesis of Thermally Stable Extra-Large Pore Crystalline Materials: A
 Uranyl Germanate with 12-Ring Channels
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2068
_journal_page_last               2069
_journal_paper_doi               10.1021/ja8084143
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         Cs6[(UO2)3(Ge2O7)2].4H2O
_chemical_formula_sum            'Cs6 Ge4 H8 O24 U3'
_chemical_formula_weight         2193.97
_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'
_atom_sites_solution_hydrogens   -
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.941(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.6417(4)
_cell_length_b                   10.3281(6)
_cell_length_c                   18.8545(11)
_cell_measurement_temperature    296(2)
_cell_volume                     1486.12(15)
_computing_cell_refinement       'Bruker SHELXTL'
_computing_data_collection       'Bruker SHELXTL'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    Diamond
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0256
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12951
_diffrn_reflns_theta_full        28.42
_diffrn_reflns_theta_max         28.42
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    27.600
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.450
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    4.903
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1868
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.905
_refine_diff_density_min         -1.241
_refine_diff_density_rms         0.203
_refine_ls_extinction_coef       0.00073(3)
_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   1.063
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         3704
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0232
_refine_ls_R_factor_gt           0.0197
_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^)+(0.0104P)^2^+5.6424P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0400
_refine_ls_wR_factor_ref         0.0410
_reflns_number_gt                3370
_reflns_number_total             3704
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8084143_si_001.cif
_cod_data_source_block           csu326b
_cod_original_cell_volume        1486.12(14)
_cod_database_code               4103912