Synthesis and Properties of the First Stable Germabenzene
Norio Nakata; Nobuhiro Takeda; Norihiro Tokitoh; Journal of the American Chemical Society 124 (2002) 6914–6920; doi:10.1021/ja0262941

data_4114892
_publ_contact_author_address
;
    Institute for Chemical Research, Kyoto University, Gokasho, Uji, 
    Kyoto 611-0011, Japan. 
;
_publ_contact_author_email       ' tokitoh@boc.kuicr.kyoto-u.ac.jp'
_publ_contact_author_fax         ' +81-774-38-3209 '
_publ_contact_author_name        'Norihiro Tokitoh'
_publ_contact_author_phone       ' +81-774-38-3200 '
_publ_section_title
;
 Synthesis and Properties of the First Stable Germabenzene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6914
_journal_page_last               6920
_journal_paper_doi               10.1021/ja0262941
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C32 H64 Ge Si6'
_chemical_formula_weight         689.96
_chemical_name_common            germabenzene
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             'Jul 6 2000'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.4873(10)
_cell_length_b                   10.9402(7)
_cell_length_c                   20.2958(10)
_cell_measurement_temperature    103(2)
_cell_volume                     4104.9(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_sigmaI/netI    0.0501
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30718
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    0.940
_exptl_absorpt_correction_T_max  0.7657
_exptl_absorpt_correction_T_min  0.7049
_exptl_absorpt_correction_type   empilical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.116
_exptl_crystal_description       prism
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.158
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.003(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         7962
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0224
_refine_ls_shift/su_max          0.103
_refine_ls_shift/su_mean         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.1367P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0556
_refine_ls_wR_factor_ref         0.0561
_reflns_number_gt                7807
_reflns_number_total             7962
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0262941_s2.cif
_cod_data_source_block           gebz
_cod_database_code               4114892