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_4080191
_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            'C43 H115 N6 Se Si12 U2'
_chemical_formula_weight         1608.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.827(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.600(6)
_cell_length_b                   21.067(11)
_cell_length_c                   28.140(14)
_cell_measurement_temperature    100(2)
_cell_volume                     6876(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'ccd 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  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0893
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            29181
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.21
_exptl_absorpt_coefficient_mu    5.475
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3202
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.970
_refine_diff_density_min         -1.936
_refine_diff_density_rms         0.210
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.022(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1033
_refine_ls_number_reflns         25135
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+50.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1232
_refine_ls_wR_factor_ref         0.1282
_reflns_number_gt                21092
_reflns_number_total             25135
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om301004q_si_002.cif
_cod_data_source_block           Complex_3
_cod_original_sg_symbol_H-M      P(2)1
_cod_database_code               4080191