Syntheses and Characterization of Nine Quaternary Uranium Chalcogenides Among the Compounds A2M3UQ6 (A = K, Rb, Cs; M = Pd, Pt; Q = S, Se)
George N. Oh; Eun Sang Choi; James A. Ibers; Inorganic Chemistry 51 (2012) 4224–4230; doi:10.1021/ic2027048

data_4328810
_publ_contact_author_address
;
Department of Chemistry
Northwestern University
Evanston, IL 60208-3113
;
_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
;
 Syntheses and Characterization of Nine Quaternary Uranium Chalcogenides
 Among the Compounds A2M3UQ6 (A = K, Rb, Cs; M = Pd, Pt; Q = S, Se)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4224
_journal_page_last               4230
_journal_paper_doi               10.1021/ic2027048
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'Cs2 Pd3 S6 U'
_chemical_formula_weight         1015.41
_chemical_name_systematic
; 
 Dicaesium tripalladium(II) uranium(IV) sulfide
;
_space_group_IT_number           69
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-F 2 2'
_symmetry_space_group_name_H-M   'F m m m'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.7874(4)
_cell_length_b                   15.0077(4)
_cell_length_c                   16.9773(7)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.315
_cell_measurement_theta_min      2.397
_cell_volume                     2493.73(16)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Crystalmaker (Palmer, 2009)'
_computing_publication_material  'SHELXL (Sheldrick, 2008a)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008a)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008a)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Bruker APEXII 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0257
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1393
_diffrn_reflns_theta_full        28.70
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         2.40
_exptl_absorpt_coefficient_mu    23.910
_exptl_absorpt_correction_T_max  0.3056
_exptl_absorpt_correction_T_min  0.1127
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2008c)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    5.409
_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_F_000             3488
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.721
_refine_diff_density_min         -2.029
_refine_diff_density_rms         0.318
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.269
_refine_ls_matrix_type           full
_refine_ls_number_parameters     39
_refine_ls_number_reflns         1393
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.269
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0247
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 calc 1/[\s^2^(Fo^2^)+(0.0293Fo^2^)^2^] 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0626
_refine_ls_wR_factor_ref         0.0629
_reflns_number_gt                1330
_reflns_number_total             1393
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2027048_si_002_4.cif
_cod_data_source_block           csupds
_cod_database_code               4328810