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_4114803
_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            'C32 H20 B F10 Ta'
_chemical_formula_weight         786.24
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 108.2173(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.5920(6)
_cell_length_b                   11.5277(6)
_cell_length_c                   19.4942(9)
_cell_measurement_reflns_used    6039
_cell_measurement_temperature    193(2)
_cell_volume                     2687.9(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0474
_diffrn_reflns_av_sigmaI/netI    0.0542
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            13116
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    4.182
_exptl_absorpt_correction_T_max  0.7875
_exptl_absorpt_correction_T_min  0.5542
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            yellow-oran
_exptl_crystal_density_diffrn    1.943
_exptl_crystal_description       prism
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.249
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         5501
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0384P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0769
_reflns_number_gt                4404
_reflns_number_total             5501
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja025547n_s2_3.cif
_cod_data_source_block           5-(Ph,Ph)
_cod_database_code               4114803