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_4111237
_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         'C23 H43 N2 Ta, C24 B F20'
_chemical_formula_sum            'C47 H43 B F20 N2 Ta'
_chemical_formula_weight         1207.59
_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 & ZCIF'
_cell_angle_alpha                90.00
_cell_angle_beta                 108.280(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.039(2)
_cell_length_b                   16.2703(18)
_cell_length_c                   18.251(2)
_cell_measurement_reflns_used    7854
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.7
_cell_measurement_theta_min      2.3
_cell_volume                     4804.4(9)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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      0.0371296
_diffrn_orient_matrix_UB_12      -0.0164383
_diffrn_orient_matrix_UB_13      0.0521659
_diffrn_orient_matrix_UB_21      -0.0456155
_diffrn_orient_matrix_UB_22      0.0108645
_diffrn_orient_matrix_UB_23      0.0223163
_diffrn_orient_matrix_UB_31      -0.0190048
_diffrn_orient_matrix_UB_32      -0.0582198
_diffrn_orient_matrix_UB_33      -0.0105219
_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  0.0239
_diffrn_reflns_av_sigmaI/netI    0.0162
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            62540
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.52
_diffrn_source_current           30
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0.08
_exptl_absorpt_coefficient_mu    2.401
_exptl_absorpt_correction_T_max  0.421
_exptl_absorpt_correction_T_min  0.330
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            brownish
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             2388
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.36
_refine_diff_density_max         2.988
_refine_diff_density_min         -1.642
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         11016
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0350
_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^)+(0.03P)^2^+9.85P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0837
_reflns_number_gt                9328
_reflns_number_total             11016
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja067011ysi20061102_121247.cif
_cod_data_source_block           {Cp*Ta(Np)[N(iPr)C(Me)N(iPr)]}[B(C6F5)4]
_cod_original_cell_volume        4804.3(10)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4111237