C-H Bond Activation by Radical Ion Pairs Derived from R3P/Al(C6F5)3 Frustrated Lewis Pairs and N2O
Gabriel Ménard; Jillian A. Hatnean; Hugh J. Cowley; Alan J. Lough; Jeremy M. Rawson; Douglas W. Stephan; Journal of the American Chemical Society 135 (2013) 6446–6449; doi:10.1021/ja402964h

data_4119709
_publ_section_title
;
 C-H Bond Activation by Radical Ion Pairs Derived from R3P/Al(C6F5)3
 Frustrated Lewis Pairs and N2O
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6446
_journal_page_last               6449
_journal_paper_doi               10.1021/ja402964h
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C81 H33.5 Al2 Br F31.5 O P'
_chemical_formula_weight         1785.92
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 99.212(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8953(10)
_cell_length_b                   14.9435(10)
_cell_length_c                   35.121(3)
_cell_measurement_reflns_used    7774
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      20.04
_cell_measurement_theta_min      2.35
_cell_volume                     7198.6(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1480
_diffrn_reflns_av_sigmaI/netI    0.2070
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            67147
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    0.749
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_F_000             3548
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.645
_refine_diff_density_min         -1.459
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1036
_refine_ls_number_reflns         12324
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.2446
_refine_ls_R_factor_gt           0.0864
_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^)+(0.1445P)^2^+1.5429P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2190
_refine_ls_wR_factor_ref         0.2949
_reflns_number_gt                4797
_reflns_number_total             12324
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja402964h_si_002_3.cif
_cod_data_source_block           gm081_0m
_cod_original_cell_volume        7198.7(9)
_cod_original_formula_sum        'C81 H33.50 Al2 Br F31.50 O P'
_cod_database_code               4119709