High-Temperature, High-Pressure Hydrothermal Synthesis and Characterization of a Salt-Inclusion Mixed-Valence Uranium(V,VI) Silicate: [Na9F2][(UVO2)(UVIO2)2(Si2O7)2]
Yu-Chih Chang; Wen-Jung Chang; Sophie Boudin; Kwang-Hwa Lii; Inorganic Chemistry 52 (2013) 7230–7235; doi:10.1021/ic400854j

data_4335252
_publ_section_title
;
 High-Temperature, High-Pressure Hydrothermal Synthesis and
 Characterization of a Salt-Inclusion Mixed-Valence Uranium(V,VI)
 Silicate: [Na9F2][(UVO2)(UVIO2)2(Si2O7)2]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7230
_journal_page_last               7235
_journal_paper_doi               10.1021/ic400854j
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'F2 Na9 O20 Si4 U3'
_chemical_formula_weight         1391.36
_chemical_name_systematic
; 
 ? 
;
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_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.75(3)
_cell_angle_beta                 96.09(3)
_cell_angle_gamma                90.90(3)
_cell_formula_units_Z            1
_cell_length_a                   5.7889(12)
_cell_length_b                   7.4227(15)
_cell_length_c                   12.092(2)
_cell_measurement_temperature    296(2)
_cell_volume                     516.53(17)
_computing_molecular_graphics    Diamond
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_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  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0387
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3630
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    23.994
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.478
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS program'
_exptl_crystal_colour            olve-green
_exptl_crystal_density_diffrn    4.473
_exptl_crystal_description       plate
_exptl_crystal_F_000             609
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.213
_refine_diff_density_min         -1.584
_refine_diff_density_rms         0.253
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         1771
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0241
_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^)+(0.0223P)^2^+2.7642P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0602
_refine_ls_wR_factor_ref         0.0612
_reflns_number_gt                1673
_reflns_number_total             1771
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400854j_si_002.cif
_cod_data_source_block           nafusio
_cod_original_cell_volume        516.53(18)
_cod_database_code               4335252