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_4128206
_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 H120 Ge2 Si8, 1.5(C6H14)'
_chemical_formula_sum            'C69 H141 Ge2 Si8'
_chemical_formula_weight         1340.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 106.345(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.2543(12)
_cell_length_b                   24.2181(10)
_cell_length_c                   20.2933(11)
_cell_measurement_reflns_used    144503
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      1.327
_cell_volume                     8608.8(8)
_computing_cell_refinement       CrysAlicePro
_computing_data_collection       CrystalClear
_computing_data_reduction        CrysAlicePro
_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    'SHELXT-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku VariMax Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1678
_diffrn_reflns_av_unetI/netI     0.0793
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            144503
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.327
_diffrn_source                   'rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    0.842
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_correction_T_min  0.906
_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            colorless
_exptl_crystal_density_diffrn    1.034
_exptl_crystal_description       block
_exptl_crystal_F_000             2924
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.070
_refine_diff_density_max         1.781
_refine_diff_density_min         -1.863
_refine_diff_density_rms         0.236
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     875
_refine_ls_number_reflns         16738
_refine_ls_number_restraints     741
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1653
_refine_ls_R_factor_gt           0.0953
_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^)+(0.1516P)^2^+60.5593P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2856
_refine_ls_wR_factor_ref         0.3436
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10202
_reflns_number_total             16738
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b00129_si_003.cif
_cod_data_source_block           compound17
_cod_database_code               4128206
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.906
_shelx_estimated_absorpt_t_max   0.943
_shelx_res_checksum              29149
_shelx_hkl_checksum              33241