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_7109555
_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            'C39 H28 B F10 P'
_chemical_formula_weight         728.39
_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                102.092(4)
_cell_angle_beta                 100.916(2)
_cell_angle_gamma                111.060(3)
_cell_formula_units_Z            2
_cell_length_a                   11.6685(2)
_cell_length_b                   13.0796(5)
_cell_length_c                   13.1348(7)
_cell_measurement_reflns_used    5472
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      0.88
_cell_volume                     1750.60(14)
_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 0.961
_diffrn_measured_fraction_theta_max 0.961
_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  0.033
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            23167
_diffrn_reflns_theta_full        67.04
_diffrn_reflns_theta_max         67.04
_diffrn_reflns_theta_min         4.24
_exptl_absorpt_coefficient_mu    1.420
_exptl_absorpt_correction_T_max  0.8711
_exptl_absorpt_correction_T_min  0.7179
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.179
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.033
_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     498
_refine_ls_number_reflns         6007
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0598P)^2^+0.4511P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1063
_refine_ls_wR_factor_ref         0.1080
_reflns_number_gt                5717
_reflns_number_total             6007
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc43294g.txt
_cod_data_source_block           erk7049
_cod_original_cell_volume        1750.60(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7109555