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_4106783
_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            'C52.5 H65 B F20 Si5 Sn'
_chemical_formula_weight         1345.99
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 108.4890(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.8702(4)
_cell_length_b                   21.1514(5)
_cell_length_c                   18.8102(5)
_cell_measurement_reflns_used    9691
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      35.05
_cell_measurement_theta_min      2.76
_cell_volume                     5988.2(3)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0130
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            253257
_diffrn_reflns_theta_full        35.08
_diffrn_reflns_theta_max         35.08
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.624
_exptl_absorpt_correction_T_max  0.7214
_exptl_absorpt_correction_T_min  0.6942
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SAINT'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_description       block
_exptl_crystal_F_000             2740
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.61
_exptl_crystal_size_min          0.56
_refine_diff_density_max         1.179
_refine_diff_density_min         -0.836
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     714
_refine_ls_number_reflns         26437
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0275
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+3.1012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0790
_reflns_number_gt                22319
_reflns_number_total             26437
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja206338u_si_002.cif
_cod_data_source_block           AS1280
_cod_original_formula_sum        'C52.50 H65 B F20 Si5 Sn'
_cod_database_code               4106783