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_7122499
_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         '0.5(Cs4 Na2 O28 Si8 U4)'
_chemical_formula_sum            'Cs2 Na O14 Si4 U2'
_chemical_formula_weight         1101.23
_space_group_crystal_system      orthorhombic
_space_group_IT_number           65
_space_group_name_Hall           '-C 2 2'
_space_group_name_H-M_alt        'C m m m'
_symmetry_space_group_name_Hall  '-C 2 2'
_symmetry_space_group_name_H-M   'C m m m'
_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            2
_cell_length_a                   8.3837(3)
_cell_length_b                   11.4748(4)
_cell_length_c                   7.4900(3)
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      36.27
_cell_measurement_theta_min      2.72
_cell_volume                     720.55(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      300.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0321
_diffrn_reflns_av_unetI/netI     0.0097
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            30032
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.499
_diffrn_reflns_theta_min         2.719
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    27.860
_exptl_absorpt_correction_T_max  0.2740
_exptl_absorpt_correction_T_min  0.1591
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1264 before and 0.0499 after correction.
The Ratio of minimum to maximum transmission is 0.5807.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    5.076
_exptl_crystal_description       tablet
_exptl_crystal_F_000             946
_exptl_crystal_size_max          0.054
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.011
_refine_diff_density_max         1.734
_refine_diff_density_min         -1.905
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.207
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     49
_refine_ls_number_reflns         770
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.207
_refine_ls_R_factor_all          0.0110
_refine_ls_R_factor_gt           0.0110
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0022P)^2^+7.1511P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0284
_refine_ls_wR_factor_ref         0.0284
_reflns_Friedel_coverage         0.000
_reflns_number_gt                769
_reflns_number_total             770
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc07789d2.cif
_cod_data_source_block           Cs2Na(UO)2Si4O12
_cod_depositor_comments
'Adding full bibliography for 7122499--7122503.cif.'
_cod_database_code               7122499
_shelx_estimated_absorpt_t_max   0.749
_shelx_estimated_absorpt_t_min   0.315
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O1) = Uanis(O2)
2. Others
 Sof(O2)=1-FVAR(1)
 Sof(O1)=FVAR(1)
 Fixed Sof: O3(0.25) O4(0.25) O5(0.25)
;
_shelx_res_checksum              5503
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'