High temperature synthesis of two open-framework uranyl silicates with ten-ring channels: Cs2(UO2)2Si8O19 and Rb2(UO2)2Si5O13
Babo, Jean-Marie; Albrecht-Schmitt, Thomas E.; Journal of Solid State Chemistry 197 (2013) 186–190; doi:10.1016/j.jssc.2012.07.048

data_1562793
_publ_section_title
;
 High temperature synthesis of two open-framework uranyl silicates with
 ten-ring channels: Cs2(UO2)2Si8O19 and Rb2(UO2)2Si5O13
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              186
_journal_page_last               190
_journal_paper_doi               10.1016/j.jssc.2012.07.048
_journal_volume                  197
_journal_year                    2013
_chemical_formula_moiety         Cs2(UO2)2Si8O19
_chemical_formula_sum            'Cl0 Cs0.62 O7.08 Si2.46 Te0 U0.62'
_chemical_formula_weight         412.345
_chemical_name_common            'cesium uranyl silicate'
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n m a'
_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            26
_cell_length_a                   14.1955(2)
_cell_length_b                   14.6274(2)
_cell_length_c                   23.0639(4)
_cell_measurement_temperature    296(2)
_cell_volume                     4789.06(13)
_computing_cell_refinement       'smart saint'
_computing_data_collection       smart
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXP-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXCIF-97 (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0495
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            69253
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    17.003
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    3.702
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             4720
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.035
_refine_diff_density_max         2.137
_refine_diff_density_min         -1.467
_refine_diff_density_rms         0.200
_refine_ls_extinction_coef       0.000023(4)
_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   0.991
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         5648
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0236P)^2^+29.6774P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0571
_refine_ls_wR_factor_ref         0.0666
_reflns_number_gt                3863
_reflns_number_total             5648
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2013-197-186.cif
_cod_data_source_block           Cs2(UO2)2Si8O19
_cod_original_sg_symbol_H-M      pnma
_cod_database_code               1562793