Reversible Isomerizations between 1,4-Digermabenzenes and 1,4-Digerma-Dewar-benzenes: Air-Stable Activators for Small Molecules.
Sugahara, Tomohiro; Guo, Jing-Dong; Hashizume, Daisuke; Sasamori, Takahiro; Tokitoh, Norihiro; Journal of the American Chemical Society 141 (2019) 2263–2267; doi:10.1021/jacs.9b00129

data_4128197
_publ_section_title
;
 Reversible Isomerizations between 1,4-Digermabenzenes and
 1,4-Digerma-Dewar-benzenes: Air-Stable Activators for Small Molecules.
;
_journal_issue                   6
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2263
_journal_page_last               2267
_journal_paper_doi               10.1021/jacs.9b00129
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         C76H118Ge2Si8
_chemical_formula_sum            'C76 H118 Ge2 Si8'
_chemical_formula_weight         1401.72
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                95.899(4)
_cell_angle_beta                 105.824(4)
_cell_angle_gamma                106.200(3)
_cell_formula_units_Z            1
_cell_length_a                   11.4109(9)
_cell_length_b                   11.6276(10)
_cell_length_c                   16.4067(13)
_cell_measurement_reflns_used    34015
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      26.499
_cell_measurement_theta_min      1.315
_cell_volume                     1973.2(3)
_computing_cell_refinement       HKL2000
_computing_data_collection       CrystalClear
_computing_data_reduction        HKL2000
_computing_molecular_graphics
'-Yadokari-XG 2011 (Wakita Nemoto et al., 2011)'
_computing_publication_material
' Yadokari-XG 2011 (Wakita Nemoto et al., 2011)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0642
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            34015
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_min         1.315
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.922
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 MULABS - Empirical Correction for Absorption Anisotropy
 Blessing, R. H., Acta Cryst., A51, 33-38 (1995).
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_description       plate
_exptl_crystal_F_000             750
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         7914
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[?^2^(Fo^2^)+(0.0188P)^2^+3.0131P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0935
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6328
_reflns_number_total             7914
_reflns_threshold_expression     'I > 2?(I)'
_cod_data_source_file            ja9b00129_si_003.cif
_cod_data_source_block           compound07
_cod_database_code               4128197
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.947
_shelx_estimated_absorpt_t_max   0.973
_shelx_res_checksum              2190
_shelx_hkl_checksum              91974