An Isolable Bis(silylene)-Stabilized Germylone and Its Reactivity.
Wang, Yuwen; Karni, Miriam; Yao, Shenglai; Apeloig, Yitzhak; Driess, Matthias; Journal of the American Chemical Society 141 (2019) 1655–1664; doi:10.1021/jacs.8b11605

data_4133603
_publ_section_title
;
 An Isolable Bis(silylene)-Stabilized Germylone and Its Reactivity.
;
_journal_issue                   4
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1655
_journal_page_last               1664
_journal_paper_doi               10.1021/jacs.8b11605
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C90 H116 Ge2 N8 O2 Si4'
_chemical_formula_weight         1599.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_cell_angle_alpha                90
_cell_angle_beta                 110.913(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1807(3)
_cell_length_b                   27.2268(4)
_cell_length_c                   18.0640(3)
_cell_measurement_reflns_used    8676
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.3080
_cell_measurement_theta_min      2.8660
_cell_volume                     8812.1(3)
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_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0599
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            35455
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.499
_diffrn_reflns_theta_max         67.499
_diffrn_reflns_theta_min         2.952
_exptl_absorpt_coefficient_mu    1.744
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43360
_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            'dark blue'
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_description       rhomb
_exptl_crystal_F_000             3392
_exptl_crystal_size_max          0.138
_exptl_crystal_size_mid          0.114
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1076
_refine_ls_number_reflns         15864
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0617P)^2^+2.4593P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1324
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11526
_reflns_number_total             15864
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b11605_si_002.cif
_cod_data_source_block           Compound-3
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4133603
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.795
_shelx_estimated_absorpt_t_max   0.918
_shelx_res_checksum              44809
_shelx_hkl_checksum              7302