Transition-Metal-Promoted or -Catalyzed Exocyclic Alkyne Insertion via Zirconacyclopentene with Carborane Auxiliary: Formation of Symmetric or Unsymmetric Benzocarboranes
Shikuo Ren; Zaozao Qiu; Zuowei Xie; Journal of the American Chemical Society 134 (2012) 3242–3254; doi:10.1021/ja211485t

data_4117470
_publ_section_title
;
 Transition-Metal-Promoted or -Catalyzed Exocyclic Alkyne Insertion via
 Zirconacyclopentene with Carborane Auxiliary: Formation of Symmetric or
 Unsymmetric Benzocarboranes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3242
_journal_page_last               3254
_journal_paper_doi               10.1021/ja211485t
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C17 H28 B10'
_chemical_formula_weight         340.49
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                79.451(3)
_cell_angle_beta                 81.489(3)
_cell_angle_gamma                81.424(3)
_cell_formula_units_Z            4
_cell_length_a                   9.7263(15)
_cell_length_b                   14.740(2)
_cell_length_c                   14.927(2)
_cell_measurement_temperature    293(2)
_cell_volume                     2064.2(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0709
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11471
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    0.054
_exptl_absorpt_correction_T_max  0.9840
_exptl_absorpt_correction_T_min  0.9735
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_description       block
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         7425
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1151
_refine_ls_R_factor_gt           0.0706
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1145P)^2^+0.2976P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1909
_refine_ls_wR_factor_ref         0.2312
_reflns_number_gt                4377
_reflns_number_total             7425
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja211485t_si_001_1.cif
_cod_data_source_block           3e
_cod_original_cell_volume        2064.1(5)
_cod_database_code               4117470