Base-stabilized acyclic amino(ylidyl)silylenes: electron-rich donors for the stabilization of silicon-element multiple bonds
Krischer, Felix; Mayer, Stephan; Hensle, Lennart; Knyszek, Daniel; Darmandeh, Heidar; Gessner, Viktoria H.; Chemical Science 16 (2025) 8346–8356; doi:10.1039/D5SC01812A

data_1574300
_publ_section_title
;
 Base-stabilized acyclic amino(ylidyl)silylenes: electron-rich donors for
 the stabilization of silicon-element multiple bonds
;
_journal_issue                   19
_journal_name_full               'Chemical Science'
_journal_page_first              8346
_journal_page_last               8356
_journal_paper_doi               10.1039/D5SC01812A
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C42 H63 N2 O2 P S3 Si'
_chemical_formula_sum            'C42 H63 N2 O2 P S3 Si'
_chemical_formula_weight         783.18
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-27
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-06-28 deposited with the CCDC.	2025-03-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.6410(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.63720(10)
_cell_length_b                   14.83500(10)
_cell_length_c                   20.8762(2)
_cell_measurement_reflns_used    28789
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.0010
_cell_measurement_theta_min      3.2890
_cell_volume                     4150.79(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -119.00 -55.00   0.50    4.00    --  -47.28 -58.00  22.00  128
  2  \w    -19.00  61.00   0.50    4.00    --   47.28 -58.00  22.00  160
  3  \w     39.00  87.00   0.50    4.00    --   47.28  58.00 163.00   96
  4  \w    -56.00 -19.00   0.50   16.00    --  -91.75  58.00 163.00   74
  5  \w   -122.00 -94.00   0.50   16.00    --  -91.75 -58.00  22.00   56
  6  \w   -161.00-126.00   0.50   16.00    --  -91.75 -58.00  22.00   70
  7  \w     99.00 161.00   0.50   16.00    --  105.91  58.00 163.00  124
  8  \w     34.00  70.00   0.50   16.00    --  105.91 -58.00  22.00   72
  9  \w    -22.00  28.00   0.50    4.00    --  -47.28  19.00-180.00  100
 10  \w     -5.00  28.00   0.50    4.00    --  -47.28  19.00 -90.00   66
 11  \w    -20.00  28.00   0.50    4.00    --  -47.28  19.00  60.00   96
 12  \w    -14.00  24.00   0.50    4.00    --  -47.28  58.00 163.00   76
 13  \w   -119.00 -86.00   0.50    4.00    --  -47.28-125.00 -60.00   66
 14  \w    -62.00 -21.00   0.50    4.00    --  -47.28  58.00 163.00   82
 15  \w     36.00  94.00   0.50    4.00    --   47.28-125.00  30.00  116
 16  \w    -65.00 -21.00   0.50   16.00    --  -91.75  61.00   0.00   88
 17  \w    -65.00 -39.00   0.50   16.00    --  -91.75  61.00 -30.00   52
 18  \w    -72.00 -21.00   0.50   16.00    --  -91.75 125.00-180.00  102
 19  \w    -48.00 -23.00   0.50   16.00    --  -91.75  45.00 -60.00   50
 20  \w    -62.00 -25.00   0.50   16.00    --  -91.75  61.00-150.00   74
 21  \w    -47.00 -22.00   0.50   16.00    --  -91.75  45.00-120.00   50
 22  \w    -47.00 -21.00   0.50   16.00    --  -91.75  45.00   0.00   52
 23  \w   -116.00 -77.00   0.50   16.00    --  -91.75 -61.00 -90.00   78
 24  \w   -156.00-120.00   0.50   16.00    --  -91.75 -61.00 -90.00   72
 25  \w   -163.00 -83.00   0.50   16.00    --  -91.75 -94.00 120.00  160
 26  \w    -62.00 -36.00   0.50   16.00    --  -91.75 125.00  90.00   52
 27  \w    -60.00 -22.00   0.50   16.00    --  -91.75  61.00-120.00   76
 28  \w     80.00 112.00   0.50   16.00    --  105.91-125.00  30.00   64
 29  \w     38.00  65.00   0.50   16.00    --  105.91-125.00  30.00   54
 30  \w     39.00  85.00   0.50   16.00    --  105.91 -96.00 132.73   92
 31  \w    140.00 177.00   0.50   16.00    --  105.91  30.00 120.00   74
 32  \w    103.00 135.00   0.50   16.00    --  105.91  30.00 120.00   64
 33  \w     61.00 106.00   0.50   16.00    --  105.91-102.00-160.76   90
 34  \w     68.00  94.00   0.50   16.00    --  105.91 -94.00  90.00   52
 35  \w     34.00  67.00   0.50   16.00    --  105.91-125.00   0.00   66
 36  \w     74.00 112.00   0.50   16.00    --  105.91-125.00   0.00   76
 37  \w     68.00  94.00   0.50   16.00    --  105.91 -94.00-120.00   52
 38  \w     69.00 106.00   0.50   16.00    --  105.91 -94.00  60.00   74
 39  \w     45.00  73.00   0.50   16.00    --  105.91 -61.00  60.00   56
 40  \w     36.00  62.00   0.50   16.00    --  105.91 -94.00  30.00   52
 41  \w     54.00 105.00   0.50   16.00    --  105.91 -97.00-125.83  102
 42  \w     36.00  89.00   0.50   16.00    --  105.91-125.00  90.00  106
 43  \w     98.00 174.00   0.50   16.00    --  105.91  45.00  90.00  152
 44  \w     52.00 106.00   0.50   16.00    --  105.91-100.00 164.47  108
 45  \w     96.00 147.00   0.50   16.00    --  105.91 125.00 150.00  102
 46  \w     72.00 105.00   0.50   16.00    --  105.91 -97.00 -12.40   66
 47  \w     36.00  92.00   0.50   16.00    --  105.91-125.00 -30.00  112
 48  \w     33.00  59.00   0.50   16.00    --  105.91 -61.00-180.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0927941000
_diffrn_orient_matrix_UB_12      -0.0578697000
_diffrn_orient_matrix_UB_13      0.0030605000
_diffrn_orient_matrix_UB_21      0.0284147000
_diffrn_orient_matrix_UB_22      -0.0642531000
_diffrn_orient_matrix_UB_23      -0.0516446000
_diffrn_orient_matrix_UB_31      0.0615492000
_diffrn_orient_matrix_UB_32      -0.0575234000
_diffrn_orient_matrix_UB_33      0.0544438000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_sigmaI/netI    0.0682
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            54915
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.073
_diffrn_reflns_theta_max         67.073
_diffrn_reflns_theta_min         3.297
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.557
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.692
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_description       plate
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.149
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.052
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         7406
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0387
_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^)+(0.0631P)^2^+2.2226P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1085
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6705
_reflns_number_total             7406
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc01812a2.cif
_cod_data_source_block           FK-1009_a
_cod_depositor_comments
'Adding full bibliography for 1574297--1574307.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1574300
_shelx_shelxl_version_number     2019/3
_cell_oxdiff_length_a            13.64191(19)
_cell_oxdiff_length_b            14.83348(17)
_cell_oxdiff_length_c            20.8739(2)
_cell_oxdiff_angle_alpha         90.0671(9)
_cell_oxdiff_angle_beta          100.6800(10)
_cell_oxdiff_angle_gamma         90.0051(10)
_cell_oxdiff_volume              4150.81(9)
_cell_oxdiff_measurement_reflns_used 28789
_oxdiff_exptl_absorpt_empirical_full_min 0.458
_oxdiff_exptl_absorpt_empirical_full_max 2.305
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1
_chemical_oxdiff_formula         'C42 H63 N2 O2 Si1 P1 S3 '
_shelx_res_checksum              909