Synthesis of Silylium and Germylium Ions by a Substituent Exchange Reaction
Schäfer, André; Reißmann, Matti; Jung, Sebastian; Schäfer, Annemarie; Saak, Wolfgang; Brendler, Erica; Müller, Thomas; Organometallics 32 (2013) 4713–; doi:10.1021/om400366z

data_4081242
_publ_section_title
;
 Synthesis of Silylium and Germylium Ions by a Substituent Exchange
 Reaction
;
_journal_name_full               Organometallics
_journal_page_first              4713
_journal_paper_doi               10.1021/om400366z
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C51 H57 B6 Cl12 Si'
_chemical_formula_weight         1188.32
_chemical_name_systematic
;
 ?
;
_space_group_IT_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                 108.364(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.6834(11)
_cell_length_b                   13.0394(8)
_cell_length_c                   25.5056(16)
_cell_measurement_temperature    153(2)
_cell_volume                     5581.6(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_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  0.1290
_diffrn_reflns_av_sigmaI/netI    0.0736
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            94354
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.83
_exptl_absorpt_coefficient_mu    0.653
_exptl_absorpt_correction_T_max  0.9769
_exptl_absorpt_correction_T_min  0.6908
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2444
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.450
_refine_diff_density_min         -1.155
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         10576
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.1141
_refine_ls_R_factor_gt           0.0852
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0543P)^2^+19.8298P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1667
_refine_ls_wR_factor_ref         0.1789
_reflns_number_gt                7959
_reflns_number_total             10576
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400366z_si_002.cif
_cod_data_source_block           ju1
_cod_database_code               4081242