Synthesis and Properties of Benzofuran-Fused Silole and Germole Derivatives: Reversible Dimerization and Crystal Structures of Monomers and Dimers
Zhang, Fei-Bao; Adachi, Yohei; Ooyama, Yousuke; Ohshita, Joji; Organometallics 35 (2016) 2327–; doi:10.1021/acs.organomet.6b00222

data_4086588
_publ_section_title
;
 Synthesis and Properties of Benzofuran-Fused Silole and Germole
 Derivatives: Reversible Dimerization and Crystal Structures of Monomers
 and Dimers
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              2327
_journal_paper_doi               10.1021/acs.organomet.6b00222
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C56 H36 Ge2 O4'
_chemical_formula_weight         918.03
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                98.300(2)
_cell_angle_beta                 106.103(2)
_cell_angle_gamma                99.866(2)
_cell_formula_units_Z            1
_cell_length_a                   9.7837(15)
_cell_length_b                   10.8094(16)
_cell_length_c                   10.8576(16)
_cell_measurement_reflns_used    8772
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      27.9591
_cell_measurement_theta_min      2.4836
_cell_volume                     1064.3(3)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX2(Bruker AXS)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'XSHELL V6.3.1(Bruker AXS)'
_computing_publication_material  'Generate Report (Bruker AXS)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'multilayered conforcal mirror'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0197
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10542
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.95
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'Bruker Turbo X-ray Source'
_exptl_absorpt_coefficient_mu    1.462
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker AXS Inc.)'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             468
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.208
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3753
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0221
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+0.9785P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0560
_refine_ls_wR_factor_ref         0.0568
_reflns_number_gt                3607
_reflns_number_total             3753
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00222_si_003.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 4086587--4086590.cif.'
_cod_database_code               4086588
_shelx_res_checksum              97915
_shelx_hkl_checksum              85280