Reactions of Modified Intermolecular Frustrated P/B Lewis Pairs with Dihydrogen, Ethene, and Carbon Dioxide
Harhausen, Marcel; Fröhlich, Roland; Kehr, Gerald; Erker, Gerhard; Organometallics 31 (2012) 2801–; doi:10.1021/om201076f

data_4077934
_publ_section_title
;
 Reactions of Modified Intermolecular Frustrated P/B Lewis Pairs with
 Dihydrogen, Ethene, and Carbon Dioxide
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              2801
_journal_paper_doi               10.1021/om201076f
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C51 H51 B F15 P'
_chemical_formula_weight         990.70
_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   'at B and P from difmap, others geom'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                71.304(2)
_cell_angle_beta                 70.488(2)
_cell_angle_gamma                70.734(2)
_cell_formula_units_Z            2
_cell_length_a                   12.6283(5)
_cell_length_b                   13.1720(5)
_cell_length_c                   16.6906(8)
_cell_measurement_reflns_used    7526
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      0.88
_cell_volume                     2400.31(18)
_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 0.964
_diffrn_measured_fraction_theta_max 0.964
_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  0.065
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30346
_diffrn_reflns_theta_full        67.49
_diffrn_reflns_theta_max         67.49
_diffrn_reflns_theta_min         3.66
_exptl_absorpt_coefficient_mu    1.334
_exptl_absorpt_correction_T_max  0.8563
_exptl_absorpt_correction_T_min  0.7762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.201
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         8313
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0537
_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^)+(0.0486P)^2^+1.3966P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1236
_refine_ls_wR_factor_ref         0.1371
_reflns_number_gt                6216
_reflns_number_total             8313
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201076f_si_002.cif
_cod_data_source_block           erk5479
_cod_original_cell_volume        2400.31(17)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4077934