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_4104741
_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            'C50.42 H82.28 Cl1.58 Li N2 O8.43 U'
_chemical_formula_weight         1152.16
_chemical_name_systematic
; 
 ? 
;
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
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_cell_angle_beta                 92.600(5)
_cell_angle_gamma                94.776(5)
_cell_formula_units_Z            2
_cell_length_a                   11.302(3)
_cell_length_b                   12.323(3)
_cell_length_c                   20.387(5)
_cell_measurement_reflns_used    967
_cell_measurement_temperature    208(2)
_cell_measurement_theta_max      21.88
_cell_measurement_theta_min      2.87
_cell_volume                     2805.4(12)
_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      208(2)
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.929
_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  0.0576
_diffrn_reflns_av_sigmaI/netI    0.1000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            30188
_diffrn_reflns_theta_full        28.45
_diffrn_reflns_theta_max         28.45
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    3.017
_exptl_absorpt_correction_T_max  0.6604
_exptl_absorpt_correction_T_min  0.5837
_exptl_absorpt_correction_type   multi-scan
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_exptl_crystal_description       block
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.20
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_exptl_crystal_size_min          0.15
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_refine_diff_density_min         -0.608
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         13149
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0644
_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^)+(0.0748P)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1441
_refine_ls_wR_factor_ref         0.1551
_reflns_number_gt                9716
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_reflns_threshold_expression     >2sigma(I)
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