Carbon-Carbon Bond Activation by 1,1-Carboboration of Internal Alkynes
Chao Chen; Gerald Kehr; Roland Fröhlich; Gerhard Erker; Journal of the American Chemical Society 132 (2010) 13594–13595; doi:10.1021/ja106365j

data_4103178
_publ_section_title
;
 Carbon-Carbon Bond Activation by 1,1-Carboboration of Internal Alkynes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13594
_journal_page_last               13595
_journal_paper_doi               10.1021/ja106365j
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C53 H37 B F15 P'
_chemical_formula_weight         1000.61
_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                70.022(4)
_cell_angle_beta                 70.262(4)
_cell_angle_gamma                69.078(2)
_cell_formula_units_Z            2
_cell_length_a                   12.2855(5)
_cell_length_b                   12.4303(6)
_cell_length_c                   18.0373(8)
_cell_measurement_reflns_used    7061
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      0.88
_cell_volume                     2343.94(19)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP (BrukerAXS, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrcik, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'Nonius KappaCCD APEXII'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.085
_diffrn_reflns_av_sigmaI/netI    0.0476
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29028
_diffrn_reflns_theta_full        67.71
_diffrn_reflns_theta_max         67.71
_diffrn_reflns_theta_min         3.97
_exptl_absorpt_coefficient_mu    1.381
_exptl_absorpt_correction_T_max  0.9598
_exptl_absorpt_correction_T_min  0.7241
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewksi & Minor, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         7920
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0583
_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^)+(0.0609P)^2^+1.8617P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1392
_refine_ls_wR_factor_ref         0.1598
_reflns_number_gt                5522
_reflns_number_total             7920
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja106365j_si_003.cif
_cod_data_source_block           erk5463
_cod_original_cell_volume        2343.94(18)
_cod_database_code               4103178