Chlorine/Methyl Exchange Reactions in Silylated Aminostibanes: A New Route To Stibinostibonium Cations
Christian Hering; Mathias Lehmann; Axel Schulz; Alexander Villinger; Inorganic Chemistry 51 (2012) 8212–8224; doi:10.1021/ic300770b

data_4329836
_publ_contact_author_address
;
Universit\"at Rostock
Institut f\"ur Chemie
Abteilung f\"ur Anorganische Chemie
Albert-Einstein-Strasse 3a 
18059 Rostock
Bundesrepublik Deutschland
;
_publ_contact_author_email
;
axel.schulz@uni-rostock.de, alexander.villinger@uni-rostock.de'
;
_publ_contact_author_fax         '+49 (0)381/498-6382'
_publ_contact_author_name        'Axel Schulz'
_publ_contact_author_phone       '+49 (0)381/498-6400 or 6403'
_publ_section_title
;
 Chlorine/Methyl Exchange Reactions in Silylated Aminostibanes: A New
 Route To Stibinostibonium Cations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8212
_journal_page_last               8224
_journal_paper_doi               10.1021/ic300770b
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C28 H34 Cl F3 N O3 S Sb Si'
_chemical_formula_sum            'C28 H34 Cl F3 N O3 S Sb Si'
_chemical_formula_weight         706.91
_chemical_name_systematic
;
N-(trifluoromethylsulfonyl)dimethylsilyl-N-[2,6-bis(2,4,6-trimethylphenyl)
phenyl]amino-chloro-methylstibane 
;
_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_author_name               'Villinger, A.'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.841(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.987(9)
_cell_length_b                   9.225(4)
_cell_length_c                   16.128(8)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      64.877
_cell_measurement_theta_min      4.837
_cell_volume                     3077(2)
_computing_cell_refinement       'Bruker Apex v2.0-2'
_computing_data_collection       'Bruker Apex v2.0-2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Apex Kappa II-CCD-diffractometer'
_diffrn_measurement_method       'phi and psi 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  0.0436
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            56598
_diffrn_reflns_theta_full        32.50
_diffrn_reflns_theta_max         32.50
_diffrn_reflns_theta_min         2.42
_exptl_absorpt_coefficient_mu    1.138
_exptl_absorpt_correction_T_max  0.8478
_exptl_absorpt_correction_T_min  0.6782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_description       block
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.820
_refine_diff_density_min         -0.834
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         11079
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0565P)^2^+0.9043P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1039
_reflns_number_gt                8735
_reflns_number_total             11079
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic300770b_si_001_08.cif
_cod_data_source_block           av_ml87_ternsime2otf_sbmecl
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4329836