Synthesis and Chemistry of Zwitterionic Tantala-3-boratacyclopentenes: Olefin-like Reactivity of a Borataalkene Ligand
Kevin S. Cook; Warren E. Piers; Robert McDonald; Journal of the American Chemical Society 124 (2002) 5411–5418; doi:10.1021/ja025547n

data_4114801
_publ_section_title
;
 Synthesis and Chemistry of Zwitterionic Tantala-3-boratacyclopentenes:
 Olefin-like Reactivity of a Borataalkene Ligand
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5411
_journal_page_last               5418
_journal_paper_doi               10.1021/ja025547n
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C29 H22 B F10 Ta'
_chemical_formula_weight         752.23
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6947(6)
_cell_length_b                   12.0858(8)
_cell_length_c                   21.2732(14)
_cell_measurement_reflns_used    5529
_cell_measurement_temperature    193(2)
_cell_volume                     2492.5(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_av_sigmaI/netI    0.0966
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            12482
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    4.504
_exptl_absorpt_correction_T_max  0.9010
_exptl_absorpt_correction_T_min  0.6644
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.005
_exptl_crystal_description       plate
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.516
_refine_diff_density_min         -0.917
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.020(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.863
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         5098
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.863
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.224
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0038P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0531
_refine_ls_wR_factor_ref         0.0564
_reflns_number_gt                4022
_reflns_number_total             5098
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja025547n_s2_1.cif
_cod_data_source_block           2b
_cod_database_code               4114801