Electronic Control of Frustrated Lewis Pair Behavior: Chemistry of a Geminal Alkylidene-Bridged Per-pentafluorophenylated P/B Pair
Rosorius, Christoph; Kehr, Gerald; Fröhlich, Roland; Grimme, Stefan; Erker, Gerhard; Organometallics 30 (2011) 4211–; doi:10.1021/om200569k

data_4065113
_publ_section_title
;
 Electronic Control of Frustrated Lewis Pair Behavior: Chemistry of a
 Geminal Alkylidene-Bridged Per-pentafluorophenylated P/B Pair
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4211
_journal_paper_doi               10.1021/om200569k
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C35.5 H11 B Cl F20 P'
_chemical_formula_weight         894.67
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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            16
_cell_length_a                   33.3804(8)
_cell_length_b                   40.8995(9)
_cell_length_c                   9.9755(4)
_cell_measurement_reflns_used    4680
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      0.88
_cell_volume                     13619.0(7)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 2003)'
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.041
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            14647
_diffrn_reflns_theta_full        66.73
_diffrn_reflns_theta_max         66.73
_diffrn_reflns_theta_min         4.32
_exptl_absorpt_coefficient_mu    2.740
_exptl_absorpt_correction_T_max  0.7713
_exptl_absorpt_correction_T_min  0.4473
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewksi & Minor, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.745
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             7056
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.47(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         5675
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0487P)^2^+27.1590P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.0940
_reflns_number_gt                5458
_reflns_number_total             5675
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200569k_si_003.cif
_cod_data_source_block           erk5877
_cod_original_sg_symbol_H-M      Fdd2
_cod_original_formula_sum        'C35.50 H11 B Cl F20 P'
_cod_database_code               4065113