Selective Se-for-S substitution in Cs-bearing uranyl compounds
Gurzhiy, Vladislav V.; Tyumentseva, Olga S.; Krivovichev, Sergey V.; Tananaev, Ivan G.; Journal of Solid State Chemistry 248 (2017) 126–133; doi:10.1016/j.jssc.2017.02.005

data_1560591
_publ_section_title
;
 Selective Se-for-S substitution in Cs-bearing uranyl compounds
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              126
_journal_page_last               133
_journal_paper_doi               10.1016/j.jssc.2017.02.005
_journal_volume                  248
_journal_year                    2017
_chemical_formula_moiety         '0.5(Cs4 O32 S0.98 Se5.02 U4)'
_chemical_formula_sum            'Cs2 O16 S0.49 Se2.52 U2'
_chemical_formula_weight         1212.01
_space_group_crystal_system      tetragonal
_space_group_IT_number           113
_space_group_name_Hall           'P -4 2ab'
_space_group_name_H-M_alt        'P -4 21 m'
_atom_sites_solution_hydrogens   .
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.8082(17)
_cell_length_b                   9.8082(17)
_cell_length_c                   8.1477(19)
_cell_measurement_reflns_used    3090
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.26
_cell_measurement_theta_min      2.50
_cell_volume                     783.8(3)
_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      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0655
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7910
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_min         2.937
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    31.193
_exptl_absorpt_correction_T_max  0.8192
_exptl_absorpt_correction_T_min  0.4212
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2007'
_exptl_crystal_colour            yellow-green
_exptl_crystal_density_diffrn    5.135
_exptl_crystal_density_meas      .
_exptl_crystal_description       lamina
_exptl_crystal_F_000             1031
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.037
_refine_diff_density_min         -1.107
_refine_diff_density_rms         0.191
_refine_ls_abs_structure_details
;
 Flack x determined using 355 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.012(8)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     61
_refine_ls_number_reflns         981
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0202
_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^)+(0.0186P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0420
_refine_ls_wR_factor_ref         0.0426
_reflns_Friedel_coverage         0.700
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                909
_reflns_number_total             981
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JSSC-2018-248-126.cif
_cod_data_source_block           Compound_8_4csno3_tpnew
_cod_database_code               1560591
_olex2_refinement_description
;
1. Shared sites
{Se1, S1}
{Se2, S2}
2. Uiso/Uaniso restraints and constraints
Uanis(Se1) = Uanis(S1)
Uanis(Se2) = Uanis(S2)
Uanis(O5) = Uanis(O6)
3. Others
 Sof(S1)=0.5*(1-FVAR(2))
 Sof(Se1)=0.5*FVAR(2)
 Sof(S2)=0.25*(1-FVAR(3))
 Sof(Se2)=0.25*FVAR(3)
;