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_4133602
_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            'C45 H58 Cl2 Ge N4 O Si2'
_chemical_formula_weight         870.62
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.8289(2)
_cell_length_b                   15.5259(2)
_cell_length_c                   17.5625(2)
_cell_measurement_reflns_used    13324
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.5250
_cell_measurement_theta_min      2.4810
_cell_volume                     5134.14(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0250
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20299
_diffrn_reflns_point_group_measured_fraction_full 0.859
_diffrn_reflns_point_group_measured_fraction_max 0.859
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         67.500
_diffrn_reflns_theta_min         3.690
_exptl_absorpt_coefficient_mu    2.469
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31994
_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            yellow
_exptl_crystal_density_diffrn    1.126
_exptl_crystal_description       rod
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.650
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.636
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details
;
 Flack x determined using 2930 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   1.020(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         7944
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0677P)^2^+4.8519P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1119
_reflns_Friedel_coverage         0.663
_reflns_Friedel_fraction_full    0.711
_reflns_Friedel_fraction_max     0.711
_reflns_number_gt                7625
_reflns_number_total             7944
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b11605_si_002.cif
_cod_data_source_block           Compound-2
_cod_database_code               4133602
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.297
_shelx_estimated_absorpt_t_max   0.827
_shelx_res_checksum              96792
_shelx_hkl_checksum              13489
_shelx_fab_checksum              11168
_platon_squeeze_void_probe_radius 1.20