Polycationic Ligands in Gold Catalysis: Synthesis and Applications of Extremely π-Acidic Catalysts
Javier Carreras; Gopinadhanpillai Gopakumar; Liangu Gu; Ana Gimeno; Pawel Linowski; Jekaterina Petuškova; Walter Thiel; Manuel Alcarazo; Journal of the American Chemical Society 135 (2013) 18815–18823; doi:10.1021/ja411146x

data_4121365
_publ_section_title
;
 Polycationic Ligands in Gold Catalysis: Synthesis and Applications of
 Extremely \p-Acidic Catalysts
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18815
_journal_page_last               18823
_journal_paper_doi               10.1021/ja411146x
_journal_volume                  135
_journal_year                    2013
_chemical_compound_source        dichloromethane/diethylether
_chemical_formula_moiety         'C36 H61 N4 P, 2(B F4)'
_chemical_formula_sum            'C36 H61 B2 F8 N4 P'
_chemical_formula_weight         754.48
_chemical_name_systematic
;
 PTA-PB-166-03_7279
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      60
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                PTA-PB-166-03
_audit_creation_date             2011-03-10
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   45.8483(14)
_cell_length_b                   11.6679(3)
_cell_length_c                   15.3567(5)
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    100
_cell_measurement_theta_max      64.3646
_cell_measurement_theta_min      3.8565
_cell_volume                     8215.1(4)
_computing_cell_refinement       'SAINT software (Bruker AXS, 2004)'
_computing_data_collection       'PROTEUM2 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT software (Bruker AXS, 2004)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2005)'
_computing_structure_refinement  'SHELXL-97 (G. M. Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (G. M. Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 66.67
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker AXS X8 Proteum'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  'focusing multilayer optic'
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_type           Cu-K\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1118
_diffrn_reflns_av_sigmaI/netI    0.0394
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            205006
_diffrn_reflns_theta_full        67.48
_diffrn_reflns_theta_max         67.48
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    1.160
_exptl_absorpt_correction_T_max  0.95524
_exptl_absorpt_correction_T_min  0.50794
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_description       plate
_exptl_crystal_F_000             3216
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.51
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       0.00099(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   2.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         7325
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.065
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0794
_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^)+(0.0111P)^2^+4.8321P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1689
_refine_ls_wR_factor_ref         0.1718
_reflns_number_gt                6324
_reflns_number_total             7325
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja411146x_si_007.cif
_cod_data_source_block           7279
_cod_original_sg_symbol_Hall     '-p 2n 2ab'
_cod_database_code               4121365