Persistent Dialkyl(silyl)stannylium Ions
Annemarie Schäfer; Wolfgang Saak; Detlev Haase; Thomas Müller; Journal of the American Chemical Society 133 (2011) 14562–14565; doi:10.1021/ja206338u

data_4106782
_publ_section_title
;
 Persistent Dialkyl(silyl)stannylium Ions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14562
_journal_page_last               14565
_journal_paper_doi               10.1021/ja206338u
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C46 H55 B F20 Si5 Sn'
_chemical_formula_weight         1257.85
_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           SHELXL-97
_cell_angle_alpha                83.9300(10)
_cell_angle_beta                 74.3710(10)
_cell_angle_gamma                83.4880(10)
_cell_formula_units_Z            2
_cell_length_a                   12.1975(4)
_cell_length_b                   12.7938(4)
_cell_length_c                   18.1555(5)
_cell_measurement_reflns_used    9885
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      37.32
_cell_measurement_theta_min      2.34
_cell_volume                     2702.47(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Diamond (Crystal Impact, 2010)'
_computing_publication_material  'SHELX-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_av_sigmaI/netI    0.0183
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            124256
_diffrn_reflns_theta_full        37.77
_diffrn_reflns_theta_max         37.77
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    0.685
_exptl_absorpt_correction_T_max  0.7788
_exptl_absorpt_correction_T_min  0.6321
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SAINT'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_description       plate
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.74
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.38
_refine_diff_density_max         1.317
_refine_diff_density_min         -1.390
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     692
_refine_ls_number_reflns         28585
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+1.1668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0833
_reflns_number_gt                24027
_reflns_number_total             28585
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja206338u_si_001.cif
_cod_data_source_block           AS1281W
_cod_database_code               4106782