Pentavalent and Tetravalent Uranium Selenides, Tl3Cu4USe6 and Tl2Ag2USe4: Syntheses, Characterization, and Structural Comparison to Other Layered Actinide Chalcogenide Compounds
Daniel E. Bugaris; Eun Sang Choi; Roy Copping; Per-Anders Glans; Stefan G. Minasian; Tolek Tyliszczak; Stosh A. Kozimor; David K. Shuh; James A. Ibers; Inorganic Chemistry 50 (2011) 6656–6666; doi:10.1021/ic200565n

data_4325665
_publ_section_title
;
 Pentavalent and Tetravalent Uranium Selenides, Tl3Cu4USe6 and Tl2Ag2USe4:
 Syntheses, Characterization, and Structural Comparison to Other Layered
 Actinide Chalcogenide Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6656
_journal_page_last               6666
_journal_paper_doi               10.1021/ic200565n
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'Cu4 Se6 Tl3 U'
_chemical_formula_sum            'Cu4 Se6 Tl3 U'
_chemical_formula_weight         1579.06
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.32(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.962(3)
_cell_length_b                   11.400(2)
_cell_length_c                   7.6228(15)
_cell_measurement_reflns_used    6008
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.73
_cell_volume                     1296.5(4)
_computing_cell_refinement       'APEX2 version 2009.5-1 (Bruker, 2009)'
_computing_data_collection       'APEX2 version 2009.5-1 (Bruker, 2009)'
_computing_data_reduction        'SAINT version 7.34a (Bruker, 2009)'
_computing_molecular_graphics    'CrystalMaker version 2.2.1 (Palmer, 2009)'
_computing_publication_material  'SHELXTL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type  'Bruker APEX2 CCD'
_diffrn_measurement_method       \w
_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  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            14773
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.52
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    72.808
_exptl_absorpt_correction_T_max  0.1251
_exptl_absorpt_correction_T_min  0.0170
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;

'face indexed; SADABS version 2008/1 (Sheldrick, 2008)'

;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    8.090
_exptl_crystal_description       block
_exptl_crystal_F_000             2620
_exptl_crystal_size_max          0.116
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.034
_refine_diff_density_max         4.432
_refine_diff_density_min         -2.278
_refine_diff_density_rms         0.665
_refine_ls_extinction_coef       0.00050(5)
_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   1.856
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         3036
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.856
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.000
_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+(0.0300P)^2^+0.0000sin\q/\l] 

 where P = 1.00000Fo^2^ + 0.00000Fc^2^ 

;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.0996
_reflns_number_gt                2777
_reflns_number_total             3036
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200565n_si_002_1.cif
_cod_data_source_block           Tl3Cu4USe6
_cod_database_code               4325665