Chalcogen Atom Transfer to Uranium(III): Synthesis and Characterization of [(R2N)3U]2(μ-E) and [(R2N)3U]2(μ-η2:η2-S2) (R = SiMe3; E = S, Se, Te)
Brown, Jessie L.; Wu, Guang; Hayton, Trevor W.; Organometallics 32 (2013) 1193–; doi:10.1021/om301004q

data_4080190
_publ_section_title
;
 Chalcogen Atom Transfer to Uranium(III): Synthesis and Characterization
 of [(R2N)3U]2(\m-E) and [(R2N)3U]2(\m-\h2:\h2-S2) (R = SiMe3; E = S, Se,
 Te)
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1193
_journal_paper_doi               10.1021/om301004q
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C36 H108 N6 S2 Si12 U2'
_chemical_formula_weight         1502.54
_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_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.123(3)
_cell_angle_beta                 97.622(3)
_cell_angle_gamma                118.498(2)
_cell_formula_units_Z            2
_cell_length_a                   11.6382(4)
_cell_length_b                   11.6617(4)
_cell_length_c                   27.9827(11)
_cell_measurement_temperature    100(2)
_cell_volume                     3286.2(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'ccd area detector'
_diffrn_measurement_method       'omega scan'
_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  0.0704
_diffrn_reflns_av_sigmaI/netI    0.0897
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            31404
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         0.74
_exptl_absorpt_coefficient_mu    5.233
_exptl_absorpt_correction_T_max  0.6227
_exptl_absorpt_correction_T_min  0.4209
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.073
_refine_diff_density_min         -2.036
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         13422
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0328
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+0.0100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0682
_reflns_number_gt                9843
_reflns_number_total             13422
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om301004q_si_002.cif
_cod_data_source_block           Complex_2
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4080190