Facile Access to Pentavalent Uranium Organometallics: One-Electron Oxidation of Uranium(IV) Imido Complexes with Copper(I) Salts
Christopher R. Graves; Brian L. Scott; David E. Morris; Jaqueline L. Kiplinger; Journal of the American Chemical Society 129 (2007) 11914–11915; doi:10.1021/ja074889w

data_4109969
_publ_contact_author_address
;
Los Alamos National Laboratory
Los Alamos, NM 87545
USA
;
_publ_contact_author_email       kiplinger@lanl.gov
_publ_contact_author_fax         '+1 505 667 9905'
_publ_contact_author_name        'Jaqueline L. Kiplinger'
_publ_contact_author_phone       '+1 505 665 9553'
_publ_section_title
;
 Facile Access to Pentavalent Uranium Organometallics: One-Electron
 Oxidation of Uranium(IV) Imido Complexes with Copper(I) Salts
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11914
_journal_page_last               11915
_journal_paper_doi               10.1021/ja074889w
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C32 H47 I N U'
_chemical_formula_weight         810.64
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.5588(9)
_cell_length_b                   18.7054(10)
_cell_length_c                   19.5958(10)
_cell_measurement_temperature    141(2)
_cell_volume                     6069.6(6)
_computing_cell_refinement       'SAINT+, v. 7.06 (Bruker AXS, 2001)'
_computing_data_collection       'APEX II, v. 1.08 (Bruker AXS, 2003)'
_computing_data_reduction        'SAINT+, v. 7.06 (Bruker AXS, 2001)'
_computing_molecular_graphics    'SHELXTL, v. 6.10, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.10, (Bruker AXS, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      141(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       '\w scans'
_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  0.0874
_diffrn_reflns_av_sigmaI/netI    0.0630
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            61796
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.36
_diffrn_reflns_theta_min         1.50
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.386
_exptl_absorpt_correction_T_max  0.7843
_exptl_absorpt_correction_T_min  0.3616
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.774
_exptl_crystal_description       'multifaceted rod'
_exptl_crystal_F_000             3128
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.814
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.138
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.529(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         11113
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0231P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0662
_refine_ls_wR_factor_ref         0.0708
_reflns_number_gt                9573
_reflns_number_total             11113
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja074889wsi20070817_025549_3.cif
_cod_data_source_block           apx405
_cod_database_code               4109969