ansa-Cyclopentadienyl-Arene Tantalum Complexes: Structure and Reactivity of Neutral, Cationic, and Dicationic Derivatives
Otten, Edwin; Meetsma, Auke; Hessen, Bart; Organometallics 31 (2012) 6071–; doi:10.1021/om300421m

data_4079057
_publ_section_related_literature
;
;
_publ_section_title
;
 ansa-Cyclopentadienyl-Arene Tantalum Complexes: Structure and Reactivity
 of Neutral, Cationic, and Dicationic Derivatives
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              6071
_journal_paper_doi               10.1021/om300421m
_journal_volume                  31
_journal_year                    2012
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C21 H28 Ta, C24 B F20'
_chemical_formula_sum            'C45 H28 B F20 Ta'
_chemical_formula_weight         1140.44
_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             '2007-05-07  11:43:12'
_audit_creation_method
;
 PLATON <TABLE ACC> option    (version :: 250307)
 SHELXL97-2 & Manual Editing
;
_audit_update_record
;
?

2012-07-31 # Formatted by publCIF
;
_cell_angle_alpha                90
_cell_angle_beta                 97.749(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.801(5)
_cell_length_b                   14.004(7)
_cell_length_c                   26.883(14)
_cell_measurement_reflns_used    3430
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      23.57
_cell_measurement_theta_min      2.59
_cell_volume                     4029(3)
_computing_cell_refinement       'SAINT-Plus, (Bruker, 2006)'
_computing_data_collection       'SMART, (Bruker, 2006)'
_computing_data_reduction        'SAINT-Plus, (Bruker, 2006)'
_computing_molecular_graphics
;
 PLATON (Spek, 2003)
 PLUTO (Meetsma, 2007)
;
_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 0.997
_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  0.2121
_diffrn_reflns_av_sigmaI/netI    0.1665
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            25898
_diffrn_reflns_reduction_process
;
 Intensity data were corrected for Lorentz and polarization
  effects, decay and absorption and reduced to F~o~^2^
  using SAINT-Plus & SADABS (Bruker, 2006).
;
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         2.59
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.856
_exptl_absorpt_correction_T_max  0.8704
_exptl_absorpt_correction_T_min  0.2367
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, (Bruker, 2006))'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.880
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platlet
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.739
_refine_diff_density_min         -3.298
_refine_diff_density_rms         0.206
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.924
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         6867
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.924
_refine_ls_R_factor_all          0.1254
_refine_ls_R_factor_gt           0.0678
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0756P)^2^+0.0P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1465
_refine_ls_wR_factor_ref         0.1732
_reflns_number_gt                3792
_reflns_number_total             6867
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om300421m_si_003.cif
_cod_data_source_block           DATNAM
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4079057
_vrn_publ_code_frame_time_sec    30.0
_vrn_publ_code_meas_time_hour    17.7