Synthesis, Reactivity, and DFT Studies of Tantalum Complexes Incorporating Diamido-N-heterocyclic Carbene Ligands. Facile Endocyclic C-H Bond Activation
Liam P. Spencer; Chad Beddie; Michael B. Hall; Michael D. Fryzuk; Journal of the American Chemical Society 128 (2006) 12531–12543; doi:10.1021/ja063282x

data_4110903
_publ_section_title
;
 Synthesis, Reactivity, and DFT Studies of Tantalum Complexes
 Incorporating Diamido-N-heterocyclic Carbene Ligands. Facile Endocyclic
 C-H Bond Activation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12531
_journal_page_last               12543
_journal_paper_doi               10.1021/ja063282x
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C35 H53 N4 Ta'
_chemical_formula_sum            'C35 H53 N4 Ta'
_chemical_formula_weight         710.76
_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                 104.6490(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.67930(10)
_cell_length_b                   22.4522(3)
_cell_length_c                   16.0990(2)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.839
_cell_measurement_theta_min      2.355
_cell_volume                     3384.93(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            49582
_diffrn_reflns_theta_full        27.92
_diffrn_reflns_theta_max         27.92
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    3.275
_exptl_absorpt_correction_T_max  0.8698
_exptl_absorpt_correction_T_min  0.6647
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_description       Irregular
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         8005
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0181
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0199P)^2^+0.0225P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0394
_refine_ls_wR_factor_ref         0.0406
_reflns_number_gt                6682
_reflns_number_total             8005
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja063282xsi20060510_051642.cif
_cod_data_source_block           mf625_0m
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4110903