High-Oxidation-State Neutral and Cationic Tantalum(IV) Alkyl Complexes That Are Stable toward β-Hydrogen and β-Methyl Eliminations
Albert Epshteyn; Peter Y. Zavalij; Lawrence R. Sita; Journal of the American Chemical Society 128 (2006) 16052–16053; doi:10.1021/ja067011y

data_4111229
_publ_section_title
;
 High-Oxidation-State Neutral and Cationic Tantalum(IV) Alkyl Complexes
 That Are Stable toward \b-Hydrogen and \b-Methyl Eliminations
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16052
_journal_page_last               16053
_journal_paper_doi               10.1021/ja067011y
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C26 H50 N2 Ta'
_chemical_formula_sum            'C26 H50 N2 Ta'
_chemical_formula_weight         571.63
_chemical_name_systematic        ?
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 & ZCIF'
_cell_angle_alpha                90.00
_cell_angle_beta                 100.2780(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   36.0392(11)
_cell_length_b                   8.7448(3)
_cell_length_c                   17.3910(5)
_cell_measurement_reflns_used    6853
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      29.3
_cell_measurement_theta_min      2.3
_cell_volume                     5392.9(3)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'XSHEL (Bruker, 1999)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'Bruker Smart1000'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      606,606,606,50,1206,50
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      -0.0263948
_diffrn_orient_matrix_UB_12      -0.0378515
_diffrn_orient_matrix_UB_13      -0.0029282
_diffrn_orient_matrix_UB_21      0.0009179
_diffrn_orient_matrix_UB_22      0.0291179
_diffrn_orient_matrix_UB_23      0.0559092
_diffrn_orient_matrix_UB_31      -0.0098797
_diffrn_orient_matrix_UB_32      0.1038996
_diffrn_orient_matrix_UB_33      -0.0167408
_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  0.0186
_diffrn_reflns_av_sigmaI/netI    0.0116
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            34475
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.63
_diffrn_source_current           30
_diffrn_source_voltage           50
_diffrn_standards_decay_%        -0.23
_exptl_absorpt_coefficient_mu    4.090
_exptl_absorpt_correction_T_max  0.325
_exptl_absorpt_correction_T_min  0.233
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             2344
_exptl_crystal_id                'Sita/Epshteyn AE532'
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.325
_exptl_crystal_size_min          0.275
_refine_diff_density_max         0.731
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         6178
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0158
_refine_ls_R_factor_gt           0.0142
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.019P)^2^+6.86P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0357
_refine_ls_wR_factor_ref         0.0363
_reflns_number_gt                5792
_reflns_number_total             6178
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja067011ysi20061102_121031.cif
_cod_data_source_block           Cp*Ta(i-Bu)2[N(iPr)C(Me)N(iPr)]
_cod_database_code               4111229