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_4110163
_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            'C10 H30 N5 O Ta'
_chemical_formula_weight         417.34
_chemical_name_common            Tantalum
_chemical_name_systematic
; 
Tantalum tetra(dimethyl)amide Hydroamide
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.079(6)
_cell_length_b                   12.092(4)
_cell_length_c                   16.206(5)
_cell_measurement_temperature    173(2)
_cell_volume                     3346.9(19)
_computing_cell_refinement       'SMART, Bruker (2000)'
_computing_data_collection       'SMART, Bruker (2000)'
_computing_data_reduction        'SHELXS-97 (Sheldrick, 1990)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL, Bruker (2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       multi-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  0.0596
_diffrn_reflns_av_sigmaI/netI    0.0501
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32990
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    6.565
_exptl_absorpt_correction_T_max  0.2702
_exptl_absorpt_correction_T_min  0.1893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2000)'
_exptl_crystal_colour            fragment
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_description       yellow
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.27
_refine_diff_density_max         3.786
_refine_diff_density_min         -2.130
_refine_diff_density_rms         0.291
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.07(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         7935
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.057
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0141P)^2^+49.3765P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.1229
_reflns_number_gt                6740
_reflns_number_total             7935
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja075076asi20070709_042547.cif
_cod_data_source_block           cp1
_cod_database_code               4110163