Noninteracting, Vicinal Frustrated P/B-Lewis Pair at the Norbornane Framework: Synthesis, Characterization, and Reactions
Muhammad Sajid; Gerald Kehr; Thomas Wiegand; Hellmut Eckert; Christian Schwickert; Rainer Pöttgen; Allan Jay P. Cardenas; Timothy H. Warren; Roland Fröhlich; Constantin G. Daniliuc; Gerhard Erker; Journal of the American Chemical Society 135 (2013) 8882–8895; doi:10.1021/ja400338e

data_4119932
_publ_section_title
;
 Noninteracting, Vicinal Frustrated P/B-Lewis Pair at the Norbornane
 Framework: Synthesis, Characterization, and Reactions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8882
_journal_page_last               8895
_journal_paper_doi               10.1021/ja400338e
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C37 H32 B F10 P'
_chemical_formula_weight         708.41
_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                 90.088(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.4305(4)
_cell_length_b                   14.7348(5)
_cell_length_c                   11.0389(3)
_cell_measurement_reflns_used    4952
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      0.88
_cell_volume                     3323.14(16)
_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 0.936
_diffrn_measured_fraction_theta_max 0.936
_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  0.032
_diffrn_reflns_av_sigmaI/netI    0.0249
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            16319
_diffrn_reflns_theta_full        67.14
_diffrn_reflns_theta_max         67.14
_diffrn_reflns_theta_min         5.27
_exptl_absorpt_coefficient_mu    1.474
_exptl_absorpt_correction_T_max  0.8314
_exptl_absorpt_correction_T_min  0.5901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_description       prism
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         5559
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0562P)^2^+1.5451P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1198
_reflns_number_gt                5162
_reflns_number_total             5559
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja400338e_si_002_1.cif
_cod_data_source_block           erk6696
_cod_database_code               4119932