Cooperative Al-H Bond Activation in DIBAL-H: Catalytic Generation of an Alumenium-Ion-Like Lewis Acid for Hydrodefluorinative Friedel-Crafts Alkylation.
Forster, Francis; Metsanen, Toni T.; Irran, Elisabeth; Hrobarik, Peter; Oestreich, Martin; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b09444

data_4126672
_publ_section_title
;
 Cooperative Al-H Bond Activation in DIBAL-H: Catalytic Generation of an
 Alumenium-Ion-Like Lewis Acid for Hydrodefluorinative Friedel-Crafts
 Alkylation.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b09444
_journal_year                    2017
_chemical_formula_moiety         'C50 H77 Al P Ru S, C24 B F20, C6 H5 F'
_chemical_formula_sum            'C80 H82 Al B F21 P Ru S'
_chemical_formula_weight         1644.35
_chemical_name_systematic
; 
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_cell_angle_alpha                95.332(2)
_cell_angle_beta                 99.221(3)
_cell_angle_gamma                104.606(3)
_cell_formula_units_Z            2
_cell_length_a                   12.6837(4)
_cell_length_b                   16.9732(4)
_cell_length_c                   18.0405(5)
_cell_measurement_reflns_used    13013
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.3740
_cell_measurement_theta_min      2.4770
_cell_volume                     3673.41(19)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5435
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_sigmaI/netI    0.0577
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25864
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         67.50
_diffrn_reflns_theta_min         2.51
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.175
_exptl_absorpt_correction_T_max  0.6684
_exptl_absorpt_correction_T_min  0.5391
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.464
_refine_diff_density_min         -1.006
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     965
_refine_ls_number_reflns         13225
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0643
_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^)+(0.0778P)^2^+19.3028P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1920
_refine_ls_wR_factor_ref         0.1996
_reflns_number_gt                11036
_reflns_number_total             13225
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja7b09444_si_002.cif
_cod_data_source_block           cu-1942
_cod_original_cell_volume        3673.40(18)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4126672