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_4127745
_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            'C63 H75 B N4 O Si3'
_chemical_formula_weight         999.35
_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                112.095(7)
_cell_angle_beta                 91.889(6)
_cell_angle_gamma                94.254(6)
_cell_formula_units_Z            2
_cell_length_a                   9.0272(7)
_cell_length_b                   18.6044(14)
_cell_length_c                   18.9208(12)
_cell_measurement_reflns_used    2596
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      70.5210
_cell_measurement_theta_min      4.1940
_cell_volume                     2929.8(4)
_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 0.998
_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  0.0971
_diffrn_reflns_av_unetI/netI     0.1256
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19676
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.499
_diffrn_reflns_theta_max         67.499
_diffrn_reflns_theta_min         2.575
_exptl_absorpt_coefficient_mu    1.069
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.00626
_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            'light yellow'
_exptl_crystal_density_diffrn    1.133
_exptl_crystal_description       plate
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.248
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.016
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     671
_refine_ls_number_reflns         10523
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1267
_refine_ls_R_factor_gt           0.0693
_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^)+(0.0504P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1450
_refine_ls_wR_factor_ref         0.1867
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5926
_reflns_number_total             10523
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b06603_si_002.cif
_cod_data_source_block           Compound-8
_cod_database_code               4127745
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.777
_shelx_estimated_absorpt_t_max   0.983
_shelx_res_checksum              62024
_shelx_hkl_checksum              86831