Reduced Uranium Complexes: Synthetic and DFT Study of the Role of π Ligation in the Stabilization of Uranium Species in a Formal Low-Valent State
Ilia Korobkov; Serge Gorelsky; Sandro Gambarotta; Journal of the American Chemical Society 131 (2009) 10406–10420; doi:10.1021/ja9002525

data_4104743
_publ_section_title
;
 Reduced Uranium Complexes: Synthetic and DFT Study of the Role of \p
 Ligation in the Stabilization of Uranium Species in a Formal Low-Valent
 State
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10406
_journal_page_last               10420
_journal_paper_doi               10.1021/ja9002525
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C80 H113 Li N4 O4 U'
_chemical_formula_weight         1439.71
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 104.170(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.448(5)
_cell_length_b                   40.927(15)
_cell_length_c                   14.033(5)
_cell_measurement_reflns_used    1840
_cell_measurement_temperature    206(2)
_cell_measurement_theta_max      21.85
_cell_measurement_theta_min      2.46
_cell_volume                     7489(5)
_computing_cell_refinement       'SMART, Bruker (2000)'
_computing_data_collection       'SMART, Bruker (2000)'
_computing_data_reduction        'XPREP, Bruker (2000)'
_computing_molecular_graphics    'SHELXTL, Bruker (2000)'
_computing_publication_material  'SHELXTL, Bruker (2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      206(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       'phi and omega 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  0.0714
_diffrn_reflns_av_sigmaI/netI    0.0725
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            61066
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.58
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    2.217
_exptl_absorpt_correction_T_max  0.7321
_exptl_absorpt_correction_T_min  0.5109
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2000)'
_exptl_crystal_colour            dk_brown
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_description       block
_exptl_crystal_F_000             2992
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.273
_refine_diff_density_min         -2.214
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     831
_refine_ls_number_reflns         15277
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0917
_refine_ls_R_factor_gt           0.0570
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+5.8372P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1056
_reflns_number_gt                11242
_reflns_number_total             15277
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9002525_si_008.cif
_cod_data_source_block           sg2270
_cod_database_code               4104743