1,4,5-Trigermabicyclo[2.1.0]pent-2-en-5-ylium: The Isolable Bishomocyclopropenylium Ion Containing a Heavier Group 14 Element
Yutaka Ishida; Akira Sekiguchi; Yoshio Kabe; Journal of the American Chemical Society 125 (2003) 11468–11469; doi:10.1021/ja030327a

data_4114174
_publ_section_title
;
 1,4,5-Trigermabicyclo[2.1.0]pent-2-en-5-ylium: The Isolable
 Bishomocyclopropenylium Ion Containing a Heavier Group 14 Element
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11468
_journal_page_last               11469
_journal_paper_doi               10.1021/ja030327a
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C68 H87 B F20 Ge3 Si3'
_chemical_formula_weight         1597.23
_chemical_name_systematic
; 
 2-Phenyl-1,4,5-tris(tri-tert-butylsilyl)-1,4,5-trigermabicyclo
[2.1.0]pent-2-en-5-ylium
 tetrakis(pentafluorophenyl)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                88.679(4)
_cell_angle_beta                 83.103(4)
_cell_angle_gamma                90.055(4)
_cell_formula_units_Z            4
_cell_length_a                   14.2100(9)
_cell_length_b                   14.4170(11)
_cell_length_c                   36.219(2)
_cell_measurement_reflns_used    77957
_cell_measurement_temperature    120
_cell_measurement_theta_max      28.07
_cell_measurement_theta_min      2.13
_cell_volume                     7364.3(8)
_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  'SHELXH-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.877
_diffrn_measured_fraction_theta_max 0.877
_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  0.0800
_diffrn_reflns_av_sigmaI/netI    0.1265
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            77957
_diffrn_reflns_theta_full        28.07
_diffrn_reflns_theta_max         28.07
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    1.355
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       rod
_exptl_crystal_F_000             3272
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.296
_refine_diff_density_min         -1.540
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1765
_refine_ls_number_reflns         31382
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1465
_refine_ls_R_factor_gt           0.0802
_refine_ls_shift/su_max          0.620
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0983P)^2^+8.6008P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1901
_refine_ls_wR_factor_ref         0.2235
_reflns_number_gt                17402
_reflns_number_total             31382
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja030327a_si2.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4114174