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_4060112
_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 S Si6'
_chemical_formula_sum            'C45 H80 Ge S Si6'
_chemical_formula_weight         894.28
_chemical_name_common            benzothiagermete
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                76.768(11)
_cell_angle_beta                 83.650(12)
_cell_angle_gamma                72.101(9)
_cell_formula_units_Z            2
_cell_length_a                   10.125(3)
_cell_length_b                   11.941(3)
_cell_length_c                   22.971(7)
_cell_measurement_reflns_used    7207
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      3.2
_cell_volume                     2570.3(13)
_diffrn_ambient_temperature      93(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  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            16974
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.18
_exptl_absorpt_coefficient_mu    0.805
_exptl_absorpt_correction_T_max  0.9841
_exptl_absorpt_correction_T_min  0.7943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.02
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         8857
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+3.5828P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.1004
_reflns_number_gt                7760
_reflns_number_total             8857
_reflns_threshold_expression     >2sigma(I)
_cod_database_code               4060112