Synthesis of a Phosphorano-Stabilized U(IV)-Carbene via One-Electron Oxidation of a U(III)-Ylide Adduct
Skye Fortier; Justin R. Walensky; Guang Wu; Trevor W. Hayton; Journal of the American Chemical Society 133 (2011) 6894–6897; doi:10.1021/ja2001133

data_4106089
_publ_contact_author_email       hayton@chem.ucsb.edu
_publ_contact_author_name        'Trevor W. Hayton'
_publ_section_title
;
 Synthesis of a Phosphorano-Stabilized U(IV)-Carbene via One-Electron
 Oxidation of a U(III)-Ylide Adduct
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6894
_journal_page_last               6897
_journal_paper_doi               10.1021/ja2001133
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C37 H68 N3 P Si6 U'
_chemical_formula_weight         992.48
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 96.242(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7155(15)
_cell_length_b                   16.2674(18)
_cell_length_c                   23.822(3)
_cell_measurement_temperature    150(2)
_cell_volume                     4898.3(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_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  0.0975
_diffrn_reflns_av_sigmaI/netI    0.0959
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            39996
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    3.519
_exptl_absorpt_correction_T_max  0.304
_exptl_absorpt_correction_T_min  0.210
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.148
_refine_diff_density_min         -1.073
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         9763
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0821
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0416P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.1017
_reflns_number_gt                6474
_reflns_number_total             9763
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2001133_si_001_1.cif
_cod_data_source_block           Complex_1
_cod_database_code               4106089