Reaction of Ta(NMe2)5 with O2: Formation of Aminoxy and Unusual (Aminomethyl)amide Oxo Complexes and Theoretical Studies of the Mechanistic Pathways
Shu-Jian Chen; Xin-Hao Zhang; Xianghua Yu; He Qiu; Glenn P. A. Yap; Ilia A. Guzei; Zhenyang Lin; Yun-Dong Wu; Zi-Ling Xue; Journal of the American Chemical Society 129 (2007) 14408–14421; doi:10.1021/ja075076a

data_4110165
_publ_contact_author_address
;
Department of Chemistry
University of Wisconsin-Madison
1101 University Ave
Madison, WI  53706
USA
;
_publ_contact_author_email       iguzei@chem.wisc.edu
_publ_contact_author_fax         608-262-0381
_publ_contact_author_name
;
Guzei, Ilia A. 
;
_publ_contact_author_phone       608-263-4694
_publ_section_title
;
 Reaction of Ta(NMe2)5 with O2: Formation of Aminoxy and Unusual
 (Aminomethyl)amide Oxo Complexes and Theoretical Studies of the
 Mechanistic Pathways
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14408
_journal_page_last               14421
_journal_paper_doi               10.1021/ja075076a
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C16 H46 N8 O2 Ta2'
_chemical_formula_weight         744.51
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 107.534(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.435(6)
_cell_length_b                   13.712(8)
_cell_length_c                   8.616(5)
_cell_measurement_reflns_used    998
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.04
_cell_measurement_theta_min      2.39
_cell_volume                     1288.2(13)
_computing_cell_refinement       'SHELXTL, Sheldrick (2001)'
_computing_data_collection       'SMART, Bruker (2002)'
_computing_data_reduction        'SHELXTL, Sheldrick (2001)'
_computing_molecular_graphics    'SHELXTL, Sheldrick (2001)'
_computing_publication_material  'SHELXTL, Sheldrick (2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 836.6
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'Bruker AXS APEX diffractometer'
_diffrn_measurement_method       \w
_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  0.0529
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7190
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.21
_diffrn_reflns_theta_min         2.39
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    8.514
_exptl_absorpt_correction_T_max  0.7270
_exptl_absorpt_correction_T_min  0.2808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick (2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.920
_exptl_crystal_description       plate
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.691
_refine_diff_density_min         -3.269
_refine_diff_density_rms         0.231
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         1565
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0566
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0817P)^2^+55.9479P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1576
_refine_ls_wR_factor_ref         0.1591
_reflns_number_gt                1546
_reflns_number_total             1565
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja075076asi20070709_042618.cif
_cod_data_source_block           benx004
_cod_original_cell_volume        1288.1(12)
_cod_database_code               4110165