High-Temperature, High-Pressure Hydrothermal Synthesis, Crystal Structure, and Solid-State NMR Spectroscopy of Cs2(UO2)(Si2O6) and Variable-Temperature Powder X-ray Diffraction Study of the Hydrate Phase Cs2(UO2)(Si2O6).0.5H2O
Chih-Shan Chen; Ray-Kuang Chiang; Hsien-Ming Kao; Kwang-Hwa Lii; Inorganic Chemistry 44 (2005) 3914–3918; doi:10.1021/ic0500199

data_4308901
_publ_section_title
;
High-Temperature, High-Pressure Hydrothermal Synthesis, Crystal Structure,
and Solid-State NMR Spectroscopy of Cs2(UO2)(Si2O6) and
Variable-Temperature Powder X-ray Diffraction Study of the Hydrate Phase
Cs2(UO2)(Si2O6).0.5H2O
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3914
_journal_page_last               3918
_journal_paper_doi               10.1021/ic0500199
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         Cs2(UO2)(Si2O6)
_chemical_formula_sum            'Cs2 O8 Si2 U'
_chemical_formula_weight         688.03
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           73
_symmetry_space_group_name_Hall  '-I 2b 2c'
_symmetry_space_group_name_H-M   'I b c 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            16
_cell_length_a                   15.1372(10)
_cell_length_b                   15.2949(10)
_cell_length_c                   16.4010(11)
_cell_measurement_temperature    293(2)
_cell_volume                     3797.2(4)
_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 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Siemens Smart CCD'
_diffrn_measurement_method       'omega scans with narrow frames'
_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  0.0548
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11278
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    24.919
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.329
_exptl_absorpt_correction_type
;
SADABS program (All reflections with I>5sigma are used to 
create an absorption curve by trying to make equivalent 
reflections have the same intensity.) 
;
_exptl_crystal_colour            yellow-green
_exptl_crystal_density_diffrn    4.814
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polygon
_exptl_crystal_F_000             4704
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.529
_refine_diff_density_min         -1.156
_refine_diff_density_rms         0.321
_refine_ls_extinction_coef       0.000572(17)
_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   1.285
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         2279
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.285
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0147P)^2^+167.3439P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0829
_reflns_number_gt                2036
_reflns_number_total             2279
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0500199si20050106_075531.cif
_cod_data_source_block           csu16
_cod_original_cell_volume        3797.2(8)
_cod_database_code               4308901