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_4127746
_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            'C65 H77 B N4 O Si3'
_chemical_formula_weight         1025.38
_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   geom
_audit_creation_method           'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_cell_angle_alpha                87.583(3)
_cell_angle_beta                 83.914(3)
_cell_angle_gamma                71.068(4)
_cell_formula_units_Z            2
_cell_length_a                   12.7519(5)
_cell_length_b                   13.0890(5)
_cell_length_c                   18.6644(7)
_cell_measurement_reflns_used    8211
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.4700
_cell_measurement_theta_min      3.5390
_cell_volume                     2930.0(2)
_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-2016/6 (Sheldrick, 2016)'
_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  0.0661
_diffrn_reflns_av_unetI/netI     0.0677
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20114
_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         3.570
_exptl_absorpt_coefficient_mu    1.081
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31706
_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            orange
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_description       rhomb
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.170
_refine_diff_density_max         0.874
_refine_diff_density_min         -0.774
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     681
_refine_ls_number_reflns         10541
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0786
_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^)+(0.1406P)^2^+1.0993P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2082
_refine_ls_wR_factor_ref         0.2330
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8009
_reflns_number_total             10541
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b06603_si_002.cif
_cod_data_source_block           Compound-9
_cod_database_code               4127746
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.678
_shelx_estimated_absorpt_t_max   0.838
_shelx_res_checksum              52145
_shelx_hkl_checksum              67284