Rerefinement of the crystal structure of trichloridosulfonium(IV) hexachloridouranate(V), (SCl~3~)[UCl~6~]
Deubner, Holger Lars; Ivlev, Sergei I.; Kraus, Florian; IUCrData 5 (2020) x200960–; doi:10.1107/S2414314620009608

data_1558815
_publ_section_title
;
 Rerefinement of the crystal structure of trichloridosulfonium(IV)
 hexachloridouranate(V), (SCl~3~)[UCl~6~]
;
_journal_coeditor_code           WM4134
_journal_issue                   7
_journal_name_full               IUCrData
_journal_page_first              x200960
_journal_paper_doi               10.1107/S2414314620009608
_journal_volume                  5
_journal_year                    2020
_chemical_formula_iupac          '(S Cl3) [U Cl6]'
_chemical_formula_moiety         'SCl3 +, U Cl6 -'
_chemical_formula_sum            'Cl9 S U'
_chemical_formula_weight         589.14
_chemical_name_common
'Trichloridosulfonium(IV) hexachloridouranate(V)'
_chemical_name_systematic
;
Trichloridosulfonium(IV) hexachloridouranate(V)
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_primary     other
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.534(2)
_cell_length_b                   10.545(2)
_cell_length_c                   11.217(2)
_cell_measurement_reflns_used    23552
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      58.94
_cell_measurement_theta_min      3.55
_cell_volume                     1246.0(4)
_computing_cell_refinement
;
X-AREA (Stoe, 2016)
;
_computing_data_collection
;
X-AREA (Stoe, 2016)
;
_computing_data_reduction
;
X-AREA (Stoe, 2016)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2019)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015)
;
_computing_structure_solution    'coordinates from an isotypic structure'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18340
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.174
_diffrn_reflns_theta_min         2.651
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    15.067
_exptl_absorpt_correction_T_max  0.0903
_exptl_absorpt_correction_T_min  0.0363
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(X-Red32; Stoe 2016)
;
_exptl_crystal_colour            'dark yellow'
_exptl_crystal_density_diffrn    3.141
_exptl_crystal_description       block
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.533
_refine_diff_density_min         -1.010
_refine_ls_abs_structure_details
;
 Refined as an inversion twin
;
_refine_ls_abs_structure_Flack   0.186(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         3364
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0201
_refine_ls_R_factor_gt           0.0194
_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^)+(0.0148P)^2^+3.5607P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0432
_refine_ls_wR_factor_ref         0.0434
_reflns_number_gt                3304
_reflns_number_total             3364
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm4134sup1.cif
_cod_data_source_block           I
_cod_database_code               1558815
_shelx_hkl_checksum              12958
_shelx_res_checksum              92138
_cod_database_fobs_code 1558815