Synthesis of the First Persilylated Ammonium Ion, [(Me3Si)3NSi(H)Me2]+, by Silylium-Catalyzed Methyl/Hydrogen Exchange Reactions
Labbow, René; Reiß, Fabian; Schulz, Axel; Villinger, Alexander; Organometallics  (2014) 140605100750002–; doi:10.1021/om500519j

data_4083528
_publ_section_title
;
 Synthesis of the First Persilylated Ammonium Ion,
 [(Me3Si)3NSi(H)Me2]+, by Silylium-Catalyzed Methyl/Hydrogen Exchange
 Reactions
;
_journal_name_full               Organometallics
_journal_page_first              140605100750002
_journal_paper_doi               10.1021/om500519j
_journal_year                    2014
_chemical_formula_moiety         'C11 H34 N Si4 +, C24 B F20 -'
_chemical_formula_sum            'C35 H34 B F20 N Si4'
_chemical_formula_weight         971.80
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 90.121(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0593(3)
_cell_length_b                   19.9706(5)
_cell_length_c                   16.6264(4)
_cell_measurement_reflns_used    9033
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      2.92
_cell_volume                     4004.15(17)
_computing_cell_refinement       'Bruker Apex V7.51A'
_computing_data_collection       'Bruker Apex V7.51A'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-Nonius Apex X8-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_sigmaI/netI    0.0610
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            53749
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.02
_exptl_absorpt_coefficient_mu    0.272
_exptl_absorpt_correction_T_max  0.9892
_exptl_absorpt_correction_T_min  0.8829
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.756
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         11637
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0959
_refine_ls_R_factor_gt           0.0536
_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^)+(0.0733P)^2^+1.3581P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1431
_reflns_number_gt                7951
_reflns_number_total             11637
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om500519j_si_002.cif
_cod_data_source_block           av_rl22
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4083528