Synthesis and Characterization of Two Isomers of 14π-Electron Germaaromatics: Kinetically Stabilized 9-Germaanthracene and 9-Germaphenanthrene
Sasamori, Takahiro; Inamura, Koji; Hoshino, Wataru; Nakata, Norio; Mizuhata, Yoshiyuki; Watanabe, Yasuaki; Furukawa, Yukio; Tokitoh, Norihiro; Organometallics 25 (2006) 3533–; doi:10.1021/om060371+

data_4083797
_publ_section_title
;
 Synthesis and Characterization of Two Isomers of 14\p-Electron
 Germaaromatics:&#x00A0; Kinetically Stabilized 9-Germaanthracene and
 9-Germaphenanthrene
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3533
_journal_paper_doi               10.1021/om060371+
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C86 H152 Ge2 Si14, 2(C7 H8) '
_chemical_formula_sum            'C100 H168 Ge2 Si14'
_chemical_formula_weight         1908.82
_chemical_name_common            9-germaanthracene_dimer
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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                 112.585(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.9585(11)
_cell_length_b                   16.6614(10)
_cell_length_c                   20.4281(15)
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      2.60
_cell_volume                     5329.4(6)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalClear
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_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  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            45034
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.60
_exptl_absorpt_coefficient_mu    0.764
_exptl_absorpt_correction_T_max  0.8622
_exptl_absorpt_correction_T_min  0.7498
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.578
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         9912
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+4.6162P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.0891
_reflns_number_gt                9191
_reflns_number_total             9912
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060371%2Bsi20060501_014748.cif
_cod_data_source_block           gedimer
_cod_original_sg_symbol_Hall     '    -P 2yab'
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               4083797