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_4080189
_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            'C40 H118 N6 O S Si12 U2'
_chemical_formula_weight         1544.60
_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                 90.026(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5726(10)
_cell_length_b                   21.379(2)
_cell_length_c                   28.376(3)
_cell_measurement_temperature    100(2)
_cell_volume                     7020.5(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0555
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            77675
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.19
_exptl_absorpt_coefficient_mu    4.873
_exptl_absorpt_correction_T_max  0.6963
_exptl_absorpt_correction_T_min  0.4914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3104
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         6.727
_refine_diff_density_min         -6.657
_refine_diff_density_rms         0.386
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.087(8)
_refine_ls_extinction_coef       0.00021(3)
_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   1.214
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     919
_refine_ls_number_reflns         34650
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.214
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0907
_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 w=1/[\s^2^(Fo^2^)+(0.0010P)^2^+403.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2119
_refine_ls_wR_factor_ref         0.2133
_reflns_number_gt                33143
_reflns_number_total             34650
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om301004q_si_002.cif
_cod_data_source_block           Complex_1
_cod_original_cell_volume        7020.8(11)
_cod_original_sg_symbol_H-M      P(2)1
_cod_database_code               4080189