Structure and Reactivity of the β-Agostic [ansa-Cp-arene]Ta(nPr) Cation: Ambivalent Behavior Induced by Intramolecular Arene Coordination
Edwin Otten; Auke Meetsma; Bart Hessen; Journal of the American Chemical Society 129 (2007) 10100–10101; doi:10.1021/ja073956j

data_4109797
_publ_contact_author_address
;
   Crystal Structure Center, Chemical Physics,
   Zernike Institute for Advanced Materials,
   University of Groningen,
   Nijenborgh 4,
   NL-9747 AG Groningen, The Netherlands.
;
_publ_contact_author_email       A.Meetsma@rug.nl
_publ_contact_author_fax         '+31 50 3634441'
_publ_contact_author_name
;
   Drs. A. Meetsma
;
_publ_contact_author_phone       '+31 50 3634368'
_publ_section_title
;
 Structure and Reactivity of the \b-Agostic [ansa-Cp-arene]Ta(nPr) Cation:
 Ambivalent Behavior Induced by Intramolecular Arene Coordination
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10100
_journal_page_last               10101
_journal_paper_doi               10.1021/ja073956j
_journal_volume                  129
_journal_year                    2007
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C22 H31 Ta'
_chemical_formula_sum            'C22 H31 Ta'
_chemical_formula_weight         476.44
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   direct
_audit_creation_date             '2006-06-09  08:11:48'
_audit_creation_method
;
 PLATON <TABLE ACC> option    (version ::  40506)
 SHELXL97-2 & Manual Editing 
;
_audit_update_record
;
 ?
;
_cell_angle_alpha                90
_cell_angle_beta                 107.539(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9609(7)
_cell_length_b                   12.4178(8)
_cell_length_c                   14.4607(9)
_cell_measurement_reflns_used    9732
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      29.64
_cell_measurement_theta_min      2.21
_cell_volume                     1876.7(2)
_computing_cell_refinement       'SAINTPLUS, Version 6.02A, (Bruker, 2000)'
_computing_data_collection       'SMART, Version 5.624, (Bruker, 2001)'
_computing_data_reduction        'XPREP, Version 5.1/NT, (Bruker, 2000)'
_computing_molecular_graphics
;
 PLUTO (Meetsma, 2006) 
 PLATON (Spek, 2003)
;
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
 DIRDIF-99 (Beurskens et al., 1999)
;
_diffrn_ambient_temperature      295(1)
_diffrn_detector_area_resol_mean 66.06
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type
;
  Bruker Smart Apex; CCD area detector 
;
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_detector
;
  CCD area-detector
;
_diffrn_radiation_monochromator  'parallel mounted graphite'
_diffrn_radiation_source         'fine focus sealed Siemens Mo tube '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16347
_diffrn_reflns_reduction_process
;
 Intensity data were corrected for Lorentz and polarization
  effects, decay and absorption and reduced to F~o~^2^
  using SAINT (Bruker, 2000) and SADABS (Sheldrick, 2001)
;
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.63
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.855
_exptl_absorpt_correction_T_max  0.2924
_exptl_absorpt_correction_T_min  0.1666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Sheldrick, Bruker, 2001))'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.21
_refine_diff_density_max         2.057
_refine_diff_density_min         -1.042
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         4627
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0156P)^2^+2.9597P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0554
_refine_ls_wR_factor_ref         0.0565
_reflns_number_gt                4225
_reflns_number_total             4627
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja073956jsi20070717_081752.cif
_cod_data_source_block           DATNAM
_cod_original_cell_volume        1876.8(2)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4109797
_vrn_publ_code_frame_time_sec    10.0
_vrn_publ_code_meas_time_hour    8.1