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_4111409
_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            'C32 H41 N O Th'
_chemical_formula_weight         687.70
_chemical_name_systematic
; 
 ? 
;
_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                 93.6720(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4583(4)
_cell_length_b                   23.2441(8)
_cell_length_c                   11.4942(4)
_cell_measurement_temperature    200(2)
_cell_volume                     2788.43(17)
_computing_cell_refinement       'SAINT+ V7.06A (Bruker 2003)'
_computing_data_collection       'APEX II, V1.0-8 (Bruker 2003)'
_computing_data_reduction        'SAINT+ V7.06A (Bruker 2003)'
_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, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       '\w 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  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0300
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            27423
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.96
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        '< 2'
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.372
_exptl_absorpt_correction_T_max  0.5650
_exptl_absorpt_correction_T_min  0.4130
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_description       'parallelpiped fragment'
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.994
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         6861
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0231
_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^)+(0.0323P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0595
_refine_ls_wR_factor_ref         0.0614
_reflns_number_gt                5676
_reflns_number_total             6861
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja044153osi20041110_110707_4.cif
_cod_data_source_block           apx030
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4111409