Reaction of strongly electrophilic alkenylboranes with phosphanylalkynes: rare examples of intermolecular 1,1-alkenylboration reactions
Olga Ekkert; Ottmar Tuschewitzki; Constantin G. Daniliuc; Gerald Kehr; Gerhard Erker; Chem.Commun. 49 (2013) 6992–; doi:10.1039/c3cc43294g

data_7109557
_publ_section_title
;
 Reaction of strongly electrophilic alkenylboranes with phosphanylalkynes:
 rare examples of intermolecular 1,1-alkenylboration reactions
;
_journal_name_full               Chem.Commun.
_journal_page_first              6992
_journal_paper_doi               10.1039/c3cc43294g
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C41.5 H25 B Cl F10 P'
_chemical_formula_weight         790.84
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 106.575(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8469(4)
_cell_length_b                   18.4534(4)
_cell_length_c                   14.8031(7)
_cell_measurement_reflns_used    6055
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      0.88
_cell_volume                     3625.3(2)
_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 (Sheldrick, 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 0.970
_diffrn_measured_fraction_theta_max 0.970
_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  0.043
_diffrn_reflns_av_sigmaI/netI    0.0271
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27693
_diffrn_reflns_theta_full        67.01
_diffrn_reflns_theta_max         67.01
_diffrn_reflns_theta_min         3.93
_exptl_absorpt_coefficient_mu    2.084
_exptl_absorpt_correction_T_max  0.9030
_exptl_absorpt_correction_T_min  0.6030
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1604
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
 A disordered half dichloromethane molecule was found in the asymmetrical 
 unit and could not be satisfactorily refined. The program SQUEEZE (A. L.
 Spek J. Appl. Cryst., 2003, 36, 7-13) was therefore used to remove 
 mathematically the effect of the solvent.
 The quoted formula and derived parameters are based on one half molecule
 of dichloromethane per asymmetric unit.  
;
_refine_diff_density_max         0.245
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.033
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         6278
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0412P)^2^+1.2492P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1038
_reflns_number_gt                5284
_reflns_number_total             6278
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc43294g.txt
_cod_data_source_block           erk7077
_cod_original_sg_symbol_H-M      P21/n
_cod_original_formula_sum        'C41.50 H25 B Cl F10 P'
_cod_database_code               7109557