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_4119933
_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 H34 B F10 P'
_chemical_formula_weight         710.42
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.5236(5)
_cell_length_b                   18.1897(6)
_cell_length_c                   20.2976(3)
_cell_measurement_reflns_used    5828
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      0.88
_cell_volume                     6469.8(3)
_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 0.971
_diffrn_measured_fraction_theta_max 0.971
_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  0.056
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33268
_diffrn_reflns_theta_full        67.22
_diffrn_reflns_theta_max         67.22
_diffrn_reflns_theta_min         4.12
_exptl_absorpt_coefficient_mu    1.515
_exptl_absorpt_correction_T_max  0.9560
_exptl_absorpt_correction_T_min  0.7033
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_description       needle
_exptl_crystal_F_000             2928
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.230
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         5632
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0457P)^2^+4.5707P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1149
_reflns_number_gt                4485
_reflns_number_total             5632
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja400338e_si_002_2.cif
_cod_data_source_block           erk6547
_cod_database_code               4119933