The U5+ compound Ba9Ag10U4S24: Synthesis, structure, and electronic properties
Mesbah, Adel; Stojko, Wojciech; Lebègue, Sébastien; Malliakas, Christos D.; Frazer, Laszlo; Ibers, James A.; Journal of Solid State Chemistry 221 (2015) 398–404; doi:10.1016/j.jssc.2014.10.014

data_1562161
_publ_section_title
;
 The U5+ compound Ba9Ag10U4S24: Synthesis, structure, and electronic
 properties
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              398
_journal_page_last               404
_journal_paper_doi               10.1016/j.jssc.2014.10.014
_journal_volume                  221
_journal_year                    2015
_chemical_formula_sum            'Ag10 Ba9 S24 U4'
_chemical_formula_weight         4036.32
_space_group_crystal_system      tetragonal
_space_group_IT_number           108
_space_group_name_Hall           'I 4 -2c'
_space_group_name_H-M_alt        'I 4 c m'
_atom_sites_solution_hydrogens   .
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9189(6)
_cell_length_b                   13.9189(6)
_cell_length_c                   23.7641(11)
_cell_measurement_reflns_used    9937
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      60.896
_cell_measurement_theta_min      6.783
_cell_volume                     4604.0(4)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'bruker apex II'
_diffrn_measurement_method       ' omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            45064
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.548
_diffrn_reflns_theta_min         1.696
_exptl_absorpt_coefficient_mu    26.796
_exptl_absorpt_correction_T_max  0.342
_exptl_absorpt_correction_T_min  0.218
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed (SADABS; Sheldrick), 2008'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    5.823
_exptl_crystal_description       block
_exptl_crystal_F_000             6904
_exptl_crystal_size_max          0.067
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.041
_refine_diff_density_max         3.828
_refine_diff_density_min         -2.860
_refine_diff_density_rms         0.261
_refine_ls_abs_structure_details
;
 Flack x determined using 1629 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.001(4)
_refine_ls_extinction_coef       0.000095(4)
_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   1.610
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         3714
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.609
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0227
_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^)+(0.0100P)^2^]
 where P=(1.0000Fo^2^+0.0000Fc^2^)
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0447
_refine_ls_wR_factor_ref         0.0454
_reflns_Friedel_coverage         0.953
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                3492
_reflns_number_total             3714
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JSSC-2015-221-398.cif
_cod_data_source_block           1
_cod_original_cell_volume        4604.0(5)
_cod_database_code               1562161
_shelx_estimated_absorpt_t_min   0.267
_shelx_estimated_absorpt_t_max   0.406
_shelxl_version_number           2013-2
_shelx_res_checksum              6993
_shelx_hkl_checksum              53443