Reactions of a Germacyclopropabenzene with Elemental Chalcogens: Syntheses and Structures of a Series of Stable 2H-Benzo[c][1,2]chalcogenagermetes
Sasamori, Takahiro; Sasaki, Takayo; Takeda, Nobuhiro; Tokitoh, Norihiro; Organometallics 24 (2005) 612–618; doi:10.1021/om049216q

data_4060114
_publ_section_title
;
 Reactions of a Germacyclopropabenzene with Elemental Chalcogens:
 Syntheses and Structures of a Series of Stable
 2H-Benzo[c][1,2]chalcogenagermetes
;
_journal_coden_ASTM              ORGND7
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              612
_journal_page_last               618
_journal_paper_doi               10.1021/om049216q
_journal_volume                  24
_journal_year                    2005
_chemical_formula_moiety         'C45 H80 Ge Si6 Te'
_chemical_formula_sum            'C45 H80 Ge Si6 Te'
_chemical_formula_weight         989.82
_chemical_name_common            compound5
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 93.7513(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8849(14)
_cell_length_b                   18.3366(13)
_cell_length_c                   20.7964(15)
_cell_measurement_reflns_used    14544
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.26
_cell_volume                     5283.5(8)
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 7.31
_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  0.0935
_diffrn_reflns_av_sigmaI/netI    0.0706
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            49865
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    1.285
_exptl_absorpt_correction_T_max  0.9386
_exptl_absorpt_correction_T_min  0.7395
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         9304
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0596P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1095
_reflns_number_gt                6392
_reflns_number_total             9304
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4060114