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_4104739
_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            'C46 H65 Cl2 Li N2 O3 U'
_chemical_formula_weight         1009.87
_chemical_name_systematic
; 
 ? 
;
_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                70.233(6)
_cell_angle_beta                 80.328(8)
_cell_angle_gamma                67.287(6)
_cell_formula_units_Z            2
_cell_length_a                   10.944(4)
_cell_length_b                   12.922(5)
_cell_length_c                   18.617(9)
_cell_measurement_reflns_used    206
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      23.46
_cell_measurement_theta_min      2.37
_cell_volume                     2283.4(16)
_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      213(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.0787
_diffrn_reflns_av_sigmaI/netI    0.1262
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13823
_diffrn_reflns_theta_full        23.46
_diffrn_reflns_theta_max         23.46
_diffrn_reflns_theta_min         2.37
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    3.711
_exptl_absorpt_correction_T_max  0.8362
_exptl_absorpt_correction_T_min  0.6060
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2000)'
_exptl_crystal_colour            lt_brown
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.607
_refine_diff_density_min         -1.460
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         6578
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.1151
_refine_ls_R_factor_gt           0.0717
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0782P)^2^+5.1125P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1497
_refine_ls_wR_factor_ref         0.1682
_reflns_number_gt                4742
_reflns_number_total             6578
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9002525_si_004.cif
_cod_data_source_block           sg2821a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/a' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4104739