A New Mode of Reactivity for Pyridine N-Oxide: C-H Activation with Uranium(IV) and Thorium(IV) Bis(alkyl) Complexes
Jaime A. Pool; Brian L. Scott; Jaqueline L. Kiplinger; Journal of the American Chemical Society 127 (2005) 1338–1339; doi:10.1021/ja044153o

data_4111406
_publ_contact_author             'Jaqueline L. Kiplinger'
_publ_contact_author_email       kiplinger@lanl.gov
_publ_section_title
;
 A New Mode of Reactivity for Pyridine N-Oxide: C-H Activation with
 Uranium(IV) and Thorium(IV) Bis(alkyl) Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1338
_journal_page_last               1339
_journal_paper_doi               10.1021/ja044153o
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C28 H41 N O Th'
_chemical_formula_weight         639.66
_chemical_name_systematic
; 
 ? 
;
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_symmetry_space_group_name_Hall  '-P 2yn'
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_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                 91.050(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.379(3)
_cell_length_b                   15.315(3)
_cell_length_c                   13.674(3)
_cell_measurement_temperature    203(2)
_cell_volume                     2591.9(10)
_computing_cell_refinement       'SAINT 4.05 (Bruker, 1996)'
_computing_data_collection       'SMART 4.210 (Bruker, 1996)'
_computing_data_reduction        'SAINT 4.05 (Bruker, 1996)'
_computing_molecular_graphics    'SHELXTL 5.10 (Bruker, 1997)'
_computing_publication_material  'SHELXTL 5.10 (Bruker, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.910
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type  'Bruker P4 with SMART 1k CCD'
_diffrn_measurement_method       '\f 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  0.0189
_diffrn_reflns_av_sigmaI/netI    0.0194
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
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_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17421
_diffrn_reflns_theta_full        27.90
_diffrn_reflns_theta_max         27.90
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        '< 2'
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    5.772
_exptl_absorpt_correction_T_max  0.6553
_exptl_absorpt_correction_T_min  0.2596
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.345
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.462
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         5636
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.462
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0282
_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^)+(0.0425P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0846
_reflns_number_gt                4790
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_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja044153osi20041110_110707_1.cif
_cod_data_source_block           ccd834
_cod_original_cell_volume        2592.0(10)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4111406