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_4109800
_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         'C19.73 H25.38 Br0.09 O Ta, C24 B F20'
_chemical_formula_sum            'C43.73 H25.38 B Br0.09 F20 O Ta'
_chemical_formula_weight         1145.71
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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     heavy
_atom_sites_solution_secondary   direct
_audit_creation_date             '2007-02-07  08:53:39'
_audit_creation_method
;
 PLATON <TABLE ACC> option    (version ::  30107)
 SHELXL97-2 & Manual Editing
;
_audit_update_record
;
?

2007-07-17 # Formatted by publCIF
;
_cell_angle_alpha                90
_cell_angle_beta                 94.5624(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8967(8)
_cell_length_b                   15.2744(8)
_cell_length_c                   17.686(1)
_cell_measurement_reflns_used    5644
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      29.21
_cell_measurement_theta_min      2.67
_cell_volume                     4011.5(4)
_computing_cell_refinement       'SAINTPLUS, Version 6.45, (Bruker, 2006)'
_computing_data_collection       'SMART, Version 5.632, (Bruker, 2005)'
_computing_data_reduction        'SAINTPLUS, Version 6.45, (Bruker, 2006)'
_computing_molecular_graphics
;
 PLUTO (Meetsma, 2007)
 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      100(1)
_diffrn_detector_area_resol_mean 66.06
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33050
_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, 2006) and SADABS (Sheldrick, 2006)
;
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.67
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.96
_exptl_absorpt_correction_T_max  0.5699
_exptl_absorpt_correction_T_min  0.4466
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, (Sheldrick, 2006))'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.897
_exptl_crystal_description       block
_exptl_crystal_F_000             2227.6
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_refine_diff_density_max         2.356
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         8828
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0442P)^2^+1.43P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0777
_refine_ls_wR_factor_ref         0.0820
_reflns_number_gt                7297
_reflns_number_total             8828
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja073956jsi20070717_081844.cif
_cod_data_source_block           DATNAM
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4109800
_vrn_publ_code_frame_time_sec    10.0
_vrn_publ_code_meas_time_hour    7.7