Moderate supercritical synthesis as a facile route to mixed-valent uranium(iv,v) and (v,vi) silicates.
Pace, Kristen A.; Klepov, Vladislav V.; Morrison, Gregory; Zur Loye, Hans-Conrad; Chemical communications (Cambridge, England) 54 (2018) 13794–13797; doi:10.1039/c8cc07789d

data_7122500
_publ_section_title
;
 Moderate supercritical synthesis as a facile route to mixed-valent
 uranium(iv,v) and (v,vi) silicates.
;
_journal_issue                   98
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              13794
_journal_page_last               13797
_journal_paper_doi               10.1039/c8cc07789d
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         '0.25(Cs8 Na4 O44 Si8 U8)'
_chemical_formula_sum            'Cs2 Na O11 Si2 U2'
_chemical_formula_weight         997.05
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_audit_creation_date             2018-06-26
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2018-06-26 deposited with the CCDC.
2018-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8327(3)
_cell_length_b                   7.4187(2)
_cell_length_c                   11.5783(3)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      36.31
_cell_measurement_theta_min      2.95
_cell_volume                     1188.17(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      300.01
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23469
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.138
_diffrn_reflns_theta_min         3.579
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    33.548
_exptl_absorpt_correction_T_max  0.2740
_exptl_absorpt_correction_T_min  0.1251
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1494 before and 0.0507 after correction.
The Ratio of minimum to maximum transmission is 0.4566.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    5.574
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1684
_exptl_crystal_size_max          0.055
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.029
_refine_diff_density_max         1.424
_refine_diff_density_min         -1.400
_refine_diff_density_rms         0.192
_refine_ls_extinction_coef       0.00156(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         2247
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.0166
_refine_ls_R_factor_gt           0.0155
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0105P)^2^+3.5539P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0351
_refine_ls_wR_factor_ref         0.0355
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2146
_reflns_number_total             2247
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc07789d2.cif
_cod_data_source_block           Cs2Na[(UO2)2(Si2O7)]
_cod_depositor_comments
'Adding full bibliography for 7122499--7122503.cif.'
_cod_database_code               7122500
_shelx_estimated_absorpt_t_max   0.443
_shelx_estimated_absorpt_t_min   0.260
_olex2_refinement_description
;
;
_shelx_res_checksum              67588
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'