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_7109554
_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            'C51 H46 B F10 P'
_chemical_formula_weight         890.66
_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                95.861(4)
_cell_angle_beta                 100.979(3)
_cell_angle_gamma                92.959(5)
_cell_formula_units_Z            4
_cell_length_a                   11.3861(3)
_cell_length_b                   17.9307(5)
_cell_length_c                   22.6904(6)
_cell_measurement_reflns_used    12748
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      0.88
_cell_volume                     4511.9(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 0.906
_diffrn_measured_fraction_theta_max 0.906
_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  0.139
_diffrn_reflns_av_sigmaI/netI    0.1012
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            62853
_diffrn_reflns_theta_full        67.17
_diffrn_reflns_theta_max         67.17
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    1.198
_exptl_absorpt_correction_T_max  0.9649
_exptl_absorpt_correction_T_min  0.8896
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
 A disordered toluene 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 two molecule of 
 toluene per asymmetric unit (one molecule of toluene was squeezed).
;
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.065
_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     1090
_refine_ls_number_reflns         14637
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1575
_refine_ls_R_factor_gt           0.0743
_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^)+(0.1042P)^2^+0.0953P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1746
_refine_ls_wR_factor_ref         0.2114
_reflns_number_gt                7434
_reflns_number_total             14637
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc43294g.txt
_cod_data_source_block           erk7032
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7109554