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_4128201
_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         'C60 H118 Ge2 Si8 0.25(C6H14)'
_chemical_formula_sum            'C61.5 H121.5 Ge2 Si8'
_chemical_formula_weight         1230.98
_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
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                86.122(3)
_cell_angle_beta                 82.522(3)
_cell_angle_gamma                89.579(3)
_cell_formula_units_Z            4
_cell_length_a                   15.6836(6)
_cell_length_b                   21.5547(8)
_cell_length_c                   22.0320(8)
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_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      25.50
_cell_measurement_theta_min      1.043
_cell_volume                     7367.8(5)
_computing_cell_refinement       CrysAlisPro
_computing_data_collection       CrystalClear
_computing_data_reduction        CrysAlisPro
_computing_molecular_graphics    'Yadokari-XG 2011 (Wakita Nemoto et al., 2011)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT-2016/4 (Sheldrick, 2016)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'EIGER X 1M'
_diffrn_measurement_method       'Oscillation Photograph'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.78254
_diffrn_reflns_av_R_equivalents  0.1802
_diffrn_reflns_av_unetI/netI     0.2393
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            49659
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         1.043
_diffrn_source                   'synchrotron radiation SPring-8 BL40XU'
_exptl_absorpt_coefficient_mu    1.261
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.975
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.110
_exptl_crystal_description       prism
_exptl_crystal_F_000             2666
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.967
_refine_diff_density_min         -0.862
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1335
_refine_ls_number_reflns         20269
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1448
_refine_ls_R_factor_gt           0.0924
_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/[\s^2^(Fo^2^)+(0.0292P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2097
_refine_ls_wR_factor_ref         0.2503
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10851
_reflns_number_total             20269
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b00129_si_003.cif
_cod_data_source_block           compound12
_cod_original_formula_sum        'C61.50 H121.50 Ge2 Si8'
_cod_database_code               4128201
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.975
_shelx_estimated_absorpt_t_max   0.987
_shelx_res_checksum              87835
_shelx_hkl_checksum              68273