U(IV) Chalcogenolates Synthesized via Oxidation of Uranium Metal by Dichalcogenides
Andrew J. Gaunt; Brian L. Scott; Mary P. Neu; Inorganic Chemistry 45 (2006) 7401–7407; doi:10.1021/ic060560k

data_4345996
_publ_section_title
;
 U(IV) Chalcogenolates Synthesized via Oxidation of Uranium Metal by
 Dichalcogenides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7401
_journal_page_last               7407
_journal_paper_doi               10.1021/ic060560k
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C56 H52 N4 S8 U2'
_chemical_formula_weight         1513.56
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.0352(19)
_cell_length_b                   20.0352(19)
_cell_length_c                   13.988(3)
_cell_measurement_temperature    203(1)
_cell_volume                     5614.9(14)
_computing_cell_refinement       'Bruker SAINT (v. 5.00, Bruker 1998)'
_computing_data_collection       'Siemens SMART (v. 4.202, Siemens 1996)'
_computing_data_reduction        'Bruker SAINT (v. 5.00, Bruker 1998)'
_computing_molecular_graphics    'Bruker AXS SHEXTL (v. 5.10)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      141(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker P4 with 1k CCD'
_diffrn_measurement_method       '\f 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  0.0214
_diffrn_reflns_av_sigmaI/netI    0.0137
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17602
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.41
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        '< 2'
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.099
_exptl_absorpt_correction_T_max  0.3472
_exptl_absorpt_correction_T_min  0.2175
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2912
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         3.133
_refine_diff_density_min         -0.750
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.803
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         2574
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.803
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0394
_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 w=1/[\s^2^(Fo^2^)+(0.0686P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1365
_refine_ls_wR_factor_ref         0.1502
_reflns_number_gt                2074
_reflns_number_total             2574
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060560ksi20060614_012839.cif
_cod_data_source_block           ccd843
_cod_original_cell_volume        5615.0(13)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4345996