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_4111234
_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_absolute_configuration ad
_chemical_formula_moiety         'C23 H43 Cl N2 Ta'
_chemical_formula_sum            'C23 H43 Cl N2 Ta'
_chemical_formula_weight         563.99
_chemical_name_systematic
;
Tantalum methyl neopentyl
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.1356(14)
_cell_length_b                   14.719(2)
_cell_length_c                   18.008(3)
_cell_measurement_reflns_used    6528
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      29.4
_cell_measurement_theta_min      2.3
_cell_volume                     2421.5(6)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      606,606,606,1206
_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      0.0054081
_diffrn_orient_matrix_UB_12      -0.0624356
_diffrn_orient_matrix_UB_13      -0.0217735
_diffrn_orient_matrix_UB_21      -0.1046073
_diffrn_orient_matrix_UB_22      0.0048583
_diffrn_orient_matrix_UB_23      -0.0159115
_diffrn_orient_matrix_UB_31      0.0318452
_diffrn_orient_matrix_UB_32      0.0263640
_diffrn_orient_matrix_UB_33      -0.0485494
_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  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0271
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25765
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.26
_diffrn_source_current           20
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0.00
_exptl_absorpt_coefficient_mu    4.660
_exptl_absorpt_correction_T_max  0.642
_exptl_absorpt_correction_T_min  0.518
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_method    not-measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             1140
_exptl_crystal_id                'Sita/Epshteyn AE570 crystal no. 7'
_exptl_crystal_size_max          0.205
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.095
_refine_diff_density_max         2.541
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details '(Flack, 1983)'
_refine_ls_abs_structure_Flack   0.479(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         5540
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0257
_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^)+(0.025P)^2^+5.12P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0594
_reflns_Friedel_coverage         0.762
_reflns_number_gt                5338
_reflns_number_total             5540
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja067011ysi20061102_121208.cif
_cod_data_source_block           Cp*Ta(Np)(Cl)[N(iPr)C(Me)N(iPr)]
_cod_database_code               4111234