Tin-Centered Radical and Cation: Stable and Free
Akira Sekiguchi; Tomohide Fukawa; Vladimir Ya. Lee; Masaaki Nakamoto; Journal of the American Chemical Society 125 (2003) 9250–9251; doi:10.1021/ja030156+

data_4114003
_publ_section_title
;
 Tin-Centered Radical and Cation: Stable and Free
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9250
_journal_page_last               9251
_journal_paper_doi               10.1021/ja030156+
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C51 H63 B F20 Si3 Sn'
_chemical_formula_weight         1269.78
_chemical_name_systematic
;
  Tris[di-tert-butyl(methyl)silyl]stannanylium
  tetrakis(pentafluorophenyl)borate
;
_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                 101.9660(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.0930(3)
_cell_length_b                   21.0470(2)
_cell_length_c                   18.1240(4)
_cell_measurement_reflns_used    58792
_cell_measurement_temperature    120
_cell_measurement_theta_max      27.95
_cell_measurement_theta_min      2.19
_cell_volume                     5632.21(18)
_computing_cell_refinement       'HKL scalepack'
_computing_data_collection       'MacScience Xpress'
_computing_data_reduction        Denzo
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device       'MacScience DIP2030 Image plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_sigmaI/netI    0.0238
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            58792
_diffrn_reflns_theta_full        27.95
_diffrn_reflns_theta_max         27.95
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    0.618
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'Dark brown'
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_description       Cube
_exptl_crystal_F_000             2584
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.387
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       0.0066(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         13122
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0795P)^2^+5.3108P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1200
_refine_ls_wR_factor_ref         0.1238
_reflns_number_gt                11763
_reflns_number_total             13122
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0301562B_2.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               4114003