Comparison of the Redox Chemistry of Primary and Secondary Amides of U(IV): Isolation of a U(VI) Bis(imido) Complex or a Homoleptic U(VI) Amido Complex
Lani A. Seaman; Skye Fortier; Guang Wu; Trevor W. Hayton; Inorganic Chemistry 50 (2011) 636–646; doi:10.1021/ic101847b

data_4324240
_publ_contact_author_email       hayton@chem.ucsb.edu
_publ_contact_author_name        'Trevor W. Hayton'
_publ_section_title
;
 Comparison of the Redox Chemistry of Primary and Secondary Amides of
 U(IV): Isolation of a U(VI) Bis(imido) Complex or a Homoleptic U(VI)
 Amido Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              636
_journal_page_last               646
_journal_paper_doi               10.1021/ic101847b
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C30 H60 N6 U'
_chemical_formula_weight         742.87
_chemical_name_systematic
; 
 Uranium(VI) Piperidide 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 100.896(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3860(13)
_cell_length_b                   17.154(2)
_cell_length_c                   17.858(2)
_cell_measurement_temperature    150(2)
_cell_volume                     3124.2(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scan'
_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  0.0932
_diffrn_reflns_av_sigmaI/netI    0.0736
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25724
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    5.223
_exptl_absorpt_correction_T_max  0.360
_exptl_absorpt_correction_T_min  0.198
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'psi scan'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_description       block
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.235
_refine_diff_density_min         -1.371
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         6295
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0364
_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^)+(0.0317P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0865
_reflns_number_gt                4418
_reflns_number_total             6295
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101847b_si_002_6.cif
_cod_data_source_block           Complex_6
_cod_original_cell_volume        3124.4(7)
_cod_database_code               4324240