The Cation Cluster of Heavier Group 14 Elements: A Free Germyl Cation with Trishomoaromaticity
Akira Sekiguchi; Yutaka Ishida; Yoshio Kabe; Masaaki Ichinohe; Journal of the American Chemical Society 124 (2002) 8776–8777; doi:10.1021/ja020395h

data_4114972
_publ_section_title
;
 The Cation Cluster of Heavier Group 14 Elements: A Free Germyl Cation
 with Trishomoaromaticity
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8776
_journal_page_last               8777
_journal_paper_doi               10.1021/ja020395h
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C103 H174 B F16 Ge10 I Si6'
_chemical_formula_weight         2748.57
_chemical_name_systematic
;\
5-Iodo-2,4,6,8,9,10-hexakis(tri-tert-butylsilyl)heptacyclo-\
[4.4.0.0^1,3^.0^2,5^.0^3,9^.0^4,7^.0^8,10^]decagerman-7-ylium\
tetrakis(2,3,5,6-tetrafluorophenyl)borate
;
_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                87.001(5)
_cell_angle_beta                 87.703(4)
_cell_angle_gamma                83.786(4)
_cell_formula_units_Z            2
_cell_length_a                   15.6610(12)
_cell_length_b                   17.3370(12)
_cell_length_c                   23.302(2)
_cell_measurement_reflns_used    58240
_cell_measurement_temperature    120
_cell_measurement_theta_max      27.94
_cell_measurement_theta_min      2.15
_cell_volume                     6277.3(8)
_computing_cell_refinement       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 0.863
_diffrn_measured_fraction_theta_max 0.863
_diffrn_measurement_device_type  '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  0.1140
_diffrn_reflns_av_sigmaI/netI    0.1560
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            58240
_diffrn_reflns_theta_full        27.94
_diffrn_reflns_theta_max         27.94
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    2.725
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2796
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.939
_refine_diff_density_min         -1.866
_refine_diff_density_rms         0.193
_refine_ls_extinction_coef       0.00240(19)
_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   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1235
_refine_ls_number_reflns         25998
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1721
_refine_ls_R_factor_gt           0.0839
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1072P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1898
_refine_ls_wR_factor_ref         0.2377
_reflns_number_gt                13675
_reflns_number_total             25998
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja020395h.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
 Correcting the _chemical_name_systematic data item value by replacing
 the '<', '>' symbols with the '^' symbol. This is the preferred way of
 denoting superscript symbols in CIF files.

 Antanas Vaitkus,
 2018-10-12
;
_cod_original_cell_volume        6277.3(9)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4114972