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_4111238
_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         'C22 H38 N2 Ta'
_chemical_formula_sum            'C22 H38 N2 Ta'
_chemical_formula_weight         511.49
_chemical_name_systematic
;
Ta trimethylmethylene complex 
;
_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                 118.401(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   34.649(3)
_cell_length_b                   8.3860(7)
_cell_length_c                   17.2661(15)
_cell_measurement_reflns_used    8497
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      28.9
_cell_measurement_theta_min      2.4
_cell_volume                     4413.1(7)
_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      220(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'Bruker Smart1000'
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details      606,606,244
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'cactus needle'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      0.0269677
_diffrn_orient_matrix_UB_12      -0.0600651
_diffrn_orient_matrix_UB_13      0.0409758
_diffrn_orient_matrix_UB_21      0.0035207
_diffrn_orient_matrix_UB_22      -0.0385081
_diffrn_orient_matrix_UB_23      -0.0511155
_diffrn_orient_matrix_UB_31      0.0182322
_diffrn_orient_matrix_UB_32      0.0952670
_diffrn_orient_matrix_UB_33      0.0050879
_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  0.0504
_diffrn_reflns_av_sigmaI/netI    0.0479
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15055
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.34
_diffrn_source_current           40
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0.00
_exptl_absorpt_coefficient_mu    4.988
_exptl_absorpt_correction_T_max  0.550
_exptl_absorpt_correction_T_min  0.374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_method    not-measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.245
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.434
_refine_diff_density_min         -1.629
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         4980
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0302
_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^)+(0.01P)^2^+19.7P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0742
_reflns_number_gt                4274
_reflns_number_total             4980
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja067011ysi20061102_121258.cif
_cod_data_source_block           Cp*Ta(TMM)[N(iPr)C(Me)N(iPr)]
_cod_database_code               4111238