Synthesis of an Isolable Bis(silylene)-Stabilized Silylone and Its Reactivity Toward Small Gaseous Molecules.
Wang, Yuwen; Karni, Miriam; Yao, Shenglai; Kaushansky, Alexander; Apeloig, Yitzhak; Driess, Matthias; Journal of the American Chemical Society 141 (2019) 12916–12927; doi:10.1021/jacs.9b06603

data_4127744
_publ_section_title
;
 Synthesis of an Isolable Bis(silylene)-Stabilized Silylone and Its
 Reactivity Toward Small Gaseous Molecules.
;
_journal_issue                   32
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12916
_journal_page_last               12927
_journal_paper_doi               10.1021/jacs.9b06603
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C45 H64 N6 O Si3'
_chemical_formula_weight         789.29
_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   mixed
_audit_creation_method           'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_cell_angle_alpha                70.283(4)
_cell_angle_beta                 88.832(4)
_cell_angle_gamma                80.984(4)
_cell_formula_units_Z            2
_cell_length_a                   9.6926(4)
_cell_length_b                   13.9099(6)
_cell_length_c                   17.6215(8)
_cell_measurement_reflns_used    5378
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.1250
_cell_measurement_theta_min      2.5910
_cell_volume                     2207.51(18)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0397
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14939
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.496
_diffrn_reflns_theta_max         67.496
_diffrn_reflns_theta_min         2.665
_exptl_absorpt_coefficient_mu    1.299
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38799
_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            colourless
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_description       plate
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.114
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         7933
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0549
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0958P)^2^+0.0973P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1438
_refine_ls_wR_factor_ref         0.1588
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6317
_reflns_number_total             7933
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b06603_si_002.cif
_cod_data_source_block           Compound-7
_cod_database_code               4127744
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.772
_shelx_estimated_absorpt_t_max   0.943
_shelx_res_checksum              10696
_shelx_hkl_checksum              20416