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_4104742
_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
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_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            'C41 H60 N2 Na2 O5 U'
_chemical_formula_weight         944.92
_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                 111.063(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.850(3)
_cell_length_b                   22.875(5)
_cell_length_c                   14.573(3)
_cell_measurement_reflns_used    509
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      24.69
_cell_measurement_theta_min      2.38
_cell_volume                     4308.5(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 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.0820
_diffrn_reflns_av_sigmaI/netI    0.0683
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24042
_diffrn_reflns_theta_full        21.96
_diffrn_reflns_theta_max         21.96
_diffrn_reflns_theta_min         1.74
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    3.829
_exptl_absorpt_correction_T_max  0.9274
_exptl_absorpt_correction_T_min  0.5147
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2000)'
_exptl_crystal_colour            brown_orange
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.458
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         5148
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0641P)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1174
_reflns_number_gt                3609
_reflns_number_total             5148
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9002525_si_007.cif
_cod_data_source_block           sg3219
_cod_depositor_comments
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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 
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_cod_database_code               4104742