Facile synthesis of electrophilic vinyl boranes: reactions of alkynyl-borates and diazonium salts
Xiaoxi Zhao; Liyuan Liang; Douglas W. Stephan; Chem.Commun. 48 (2012) 10189–; doi:10.1039/c2cc35553a

data_7108444
_publ_section_title
;
 Facile synthesis of electrophilic vinyl boranes: reactions of
 alkynyl-borates and diazonium salts
;
_journal_name_full               Chem.Commun.
_journal_page_first              10189
_journal_paper_doi               10.1039/c2cc35553a
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C35 H13 B Cl2 F18 O'
_chemical_formula_weight         873.16
_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                 105.050(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.2093(4)
_cell_length_b                   13.0466(4)
_cell_length_c                   22.3254(7)
_cell_measurement_temperature    150(2)
_cell_volume                     3434.23(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0515
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            36446
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.318
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.7062
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.543
_refine_diff_density_min         -0.941
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         6049
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0669
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1142P)^2^+7.9218P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1887
_refine_ls_wR_factor_ref         0.2139
_reflns_number_gt                4407
_reflns_number_total             6049
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc35553a.txt
_cod_data_source_block           ll007_0m
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7108444