P-C Bond Activation Chemistry: Evidence for 1,1-Carboboration Reactions Proceeding with Phosphorus-Carbon Bond Cleavage
Olga Ekkert; Gerald Kehr; Roland Fröhlich; Gerhard Erker; Journal of the American Chemical Society 133 (2011) 4610–4616; doi:10.1021/ja1110283

data_4105836
_publ_section_title
;
 P-C Bond Activation Chemistry: Evidence for 1,1-Carboboration Reactions
 Proceeding with Phosphorus-Carbon Bond Cleavage
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4610
_journal_page_last               4616
_journal_paper_doi               10.1021/ja1110283
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C45 H22 B Cl2 F15 P2'
_chemical_formula_weight         991.28
_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                95.231(2)
_cell_angle_beta                 102.492(2)
_cell_angle_gamma                104.305(2)
_cell_formula_units_Z            2
_cell_length_a                   9.7976(2)
_cell_length_b                   10.8460(4)
_cell_length_c                   21.1870(7)
_cell_measurement_reflns_used    6155
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      0.88
_cell_volume                     2104.94(12)
_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 0.918
_diffrn_measured_fraction_theta_max 0.918
_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  0.110
_diffrn_reflns_av_sigmaI/netI    0.0658
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25965
_diffrn_reflns_theta_full        67.32
_diffrn_reflns_theta_max         67.32
_diffrn_reflns_theta_min         4.26
_exptl_absorpt_coefficient_mu    3.023
_exptl_absorpt_correction_T_max  0.8887
_exptl_absorpt_correction_T_min  0.7520
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_description       plate
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.698
_refine_diff_density_min         -0.822
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     596
_refine_ls_number_reflns         6932
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1257
_refine_ls_R_factor_gt           0.0769
_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^)+(0.0976P)^2^+3.9162P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1866
_refine_ls_wR_factor_ref         0.2242
_reflns_number_gt                4337
_reflns_number_total             6932
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1110283_si_004.cif
_cod_data_source_block           erk5624
_cod_original_cell_volume        2104.94(11)
_cod_database_code               4105836