Synthesis and Structure of the [(UO2)S4]6- Anion: A Cation-Stabilized Uranyl Sulfide
Matthew D. Ward; Jordan M. Klingsporn; James A. Ibers; Inorganic Chemistry 52 (2013) 10220–10222; doi:10.1021/ic401382g

data_4335958
_publ_contact_author_address
'Department of Chemistry, Northwestern University, Evanston, IL, United States'
_publ_contact_author_email       ibers@chem.northwestern.edu
_publ_contact_author_fax         '+1 847 491 2976'
_publ_contact_author_name        'James A. Ibers '
_publ_contact_author_phone       "'+1 847 491 5449"
_publ_section_title
;
 Synthesis and Structure of the [(UO2)S4]6- Anion: A Cation-Stabilized
 Uranyl Sulfide
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10220
_journal_page_last               10222
_journal_paper_doi               10.1021/ic401382g
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'O2 S4 U, 2(Ba), 2(Na)'
_chemical_formula_sum            'Ba2 Na2 O2 S4 U'
_chemical_formula_weight         718.93
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                81.3250(10)
_cell_angle_beta                 67.1010(10)
_cell_angle_gamma                72.5420(10)
_cell_formula_units_Z            1
_cell_length_a                   6.3325(2)
_cell_length_b                   6.7148(2)
_cell_length_c                   6.7530(2)
_cell_measurement_reflns_used    5892
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.20
_cell_measurement_theta_min      3.18
_cell_volume                     252.144(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008a)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008a)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0141
_diffrn_reflns_av_sigmaI/netI    0.0136
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6706
_diffrn_reflns_theta_full        33.20
_diffrn_reflns_theta_max         33.20
_diffrn_reflns_theta_min         3.18
_exptl_absorpt_coefficient_mu    24.599
_exptl_absorpt_correction_T_max  0.1656
_exptl_absorpt_correction_T_min  0.0891
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed, SADABS (Sheldrick, 2008b)'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    4.735
_exptl_crystal_description       Prism
_exptl_crystal_F_000             306
_exptl_crystal_size_max          0.173
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.149
_refine_diff_density_max         1.422
_refine_diff_density_min         -1.955
_refine_diff_density_rms         0.213
_refine_ls_extinction_coef       0.0690(11)
_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   1.436
_refine_ls_matrix_type           full
_refine_ls_number_parameters     53
_refine_ls_number_reflns         1927
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.436
_refine_ls_R_factor_all          0.0134
_refine_ls_R_factor_gt           0.0134
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc 
 [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ 
   [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0161P)^2^+0.0000sin\q/\l] 
 where P = 1.00000Fo^2^ + 0.00000Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0354
_refine_ls_wR_factor_ref         0.0354
_reflns_number_gt                1927
_reflns_number_total             1927
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401382g_si_001.cif
_cod_data_source_block           Na2Ba2UO2S4
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4335958