Facile Reduction of a Uranyl(VI) β-Ketoiminate Complex to U(IV) Upon Oxo Silylation
Jessie L. Brown; Charles C. Mokhtarzadeh; Jeremie M. Lever; Guang Wu; Trevor W. Hayton; Inorganic Chemistry 50 (2011) 5105–5112; doi:10.1021/ic200387n

data_4325238
_publ_section_title
;
 Facile Reduction of a Uranyl(VI) \b-Ketoiminate Complex to U(IV) Upon Oxo
 Silylation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5105
_journal_page_last               5112
_journal_paper_doi               10.1021/ic200387n
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C24 H33 I5 O2 P Si2 U'
_chemical_formula_weight         1313.18
_chemical_name_systematic
; 
 Triphenylmonoiodophosphonium Uranium(V) tetraiodo-bistrimethylsilyloxide  
;
_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                103.327(12)
_cell_angle_beta                 90.511(13)
_cell_angle_gamma                101.222(12)
_cell_formula_units_Z            2
_cell_length_a                   9.452(7)
_cell_length_b                   9.961(8)
_cell_length_c                   20.940(16)
_cell_measurement_temperature    150(2)
_cell_volume                     1879(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_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  0.1135
_diffrn_reflns_av_sigmaI/netI    0.0970
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            15723
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.00
_exptl_absorpt_coefficient_mu    8.553
_exptl_absorpt_correction_T_max  0.481
_exptl_absorpt_correction_T_min  0.212
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'psi scan'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.321
_exptl_crystal_description       block
_exptl_crystal_F_000             1186
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.346
_refine_diff_density_min         -4.005
_refine_diff_density_rms         0.335
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         7383
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0671P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1216
_refine_ls_wR_factor_ref         0.1346
_reflns_number_gt                5626
_reflns_number_total             7383
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200387n_si_001_2.cif
_cod_data_source_block           Complex_2
_cod_database_code               4325238