Quantitative Assessment of the Lewis Acidity of Silylium Ions
Großekappenberg, Henning; Reißmann, Matti; Schmidtmann, Marc; Müller, Thomas; Organometallics 34 (2015) 4952–; doi:10.1021/acs.organomet.5b00556

data_4087737
_publ_section_title
;
 Quantitative Assessment of the Lewis Acidity of Silylium Ions
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              4952
_journal_paper_doi               10.1021/acs.organomet.5b00556
_journal_volume                  34
_journal_year                    2015
_chemical_formula_structural     '[(C11H15)3SiOP(C6H5)3] [Al(OC(CF3)3)4]'
_chemical_formula_sum            'C67 H60 Al F36 O5 P Si'
_chemical_formula_weight         1715.19
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   15.7478(12)
_cell_length_b                   15.7478(12)
_cell_length_c                   51.824(5)
_cell_measurement_reflns_used    9793
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.23
_cell_measurement_theta_min      2.17
_cell_volume                     11130.2(16)
_computing_cell_refinement       'Bruker SAINT V8.34A'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT V8.34A'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0156
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       72
_diffrn_reflns_limit_l_min       -72
_diffrn_reflns_number            127366
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.024
_diffrn_reflns_theta_min         1.544
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.203
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9567
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/3 (Sheldrick)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_description       block
_exptl_crystal_F_000             5208
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_refine_diff_density_max         2.859
_refine_diff_density_min         -0.963
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.228
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         7253
_refine_ls_number_restraints     432
_refine_ls_restrained_S_all      1.312
_refine_ls_R_factor_all          0.1255
_refine_ls_R_factor_gt           0.1013
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+60.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2573
_refine_ls_wR_factor_ref         0.2797
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5585
_reflns_number_total             7253
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00556_si_002.cif
_cod_data_source_block           hg62
_cod_original_cell_volume        11130(2)
_cod_database_code               4087737
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.905
_shelx_estimated_absorpt_t_max   0.941
_shelx_res_checksum              94567
_shelx_hkl_checksum              67436