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_1574303
_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         'C41 H63 N2 O3 P S Si, C6 H6'
_chemical_formula_sum            'C47 H69 N2 O3 P S Si'
_chemical_formula_weight         801.16
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-10
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-04-23 deposited with the CCDC.	2025-03-27 downloaded from the CCDC.
;
_cell_angle_alpha                74.2670(10)
_cell_angle_beta                 77.1070(10)
_cell_angle_gamma                69.783(2)
_cell_formula_units_Z            2
_cell_length_a                   10.2796(2)
_cell_length_b                   12.9114(2)
_cell_length_c                   18.3044(2)
_cell_measurement_reflns_used    52754
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.6090
_cell_measurement_theta_min      2.5660
_cell_volume                     2171.70(7)
_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_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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     34.00  61.00   0.50    0.05    --   47.28  18.00  66.00   54
  2  \w     62.00  88.00   0.50    0.05    --   47.28  77.00  60.00   52
  3  \w     26.00  52.00   0.50    0.05    --   47.28  77.00  60.00   52
  4  \w     90.00 116.00   0.50    0.05    --   47.28  18.00  66.00   52
  5  \w     25.00  51.00   0.50    0.05    --   47.28  77.00 -30.00   52
  6  \w     36.00  63.00   0.50    0.05    --   47.28  19.00-180.00   54
  7  \w     14.00  39.00   0.50    0.05    --   42.00  89.00 104.25   50
  8  \w    -10.00  22.00   0.50    0.05    --   22.00  97.00 133.87   64
  9  \w      9.00  40.00   0.50    0.05    --   38.00  91.00  28.81   62
 10  \w    -28.00  -3.00   0.50    0.05    --   10.00 107.00 -18.52   50
 11  \w     -4.00  21.00   0.50    0.05    --   26.00  98.00-105.65   50
 12  \w    -15.00  24.00   0.50    0.05    --   18.00  98.00 -85.27   78
 13  \w     17.00  42.00   0.50    0.05    --   46.00  90.00-146.90   50
 14  \w     17.00  42.00   0.50    0.05    --   46.00  90.00 -11.99   50
 15  \w     13.00  38.00   0.50    0.05    --   42.00  90.00 151.81   50
 16  \w     62.00  88.00   0.50    0.05    --   54.00  77.00  93.06   52
 17  \w     35.00  71.00   0.50    0.05    --   58.00  77.00 162.04   72
 18  \w     32.00  58.00   0.50    0.05    --   54.00  77.00  93.06   52
 19  \w     43.00  68.00   0.50    0.05    --   66.00  77.00  47.35   50
 20  \w     35.00  60.00   0.50    0.05    --   58.00  77.00  -3.43   50
 21  \w     83.00 109.00   0.50    0.05    --   58.00  77.00  -3.43   52
 22  \w     99.00 135.00   0.50    0.05    --   62.00  76.00-104.37   72
 23  \w     35.00  61.00   0.50    0.05    --   58.00  77.00-117.88   52
 24  \w     40.00  66.00   0.50    0.05    --   62.00  76.00-104.37   52
 25  \w     43.00  69.00   0.50    0.05    --   66.00  77.00 -66.84   52
 26  \w     36.00  62.00   0.50    0.05    --   58.00  76.00 -23.42   52
 27  \w     48.00  73.00   0.50    0.05    --   70.00  76.00 -25.00   50
 28  \w    101.00 126.00   0.50    0.05    --   58.00  75.00 -75.17   50
 29  \w     36.00  74.00   0.50    0.05    --   58.00  75.00 -75.17   76
 30  \w     32.00  57.00   0.50    0.05    --   54.00  75.00-132.79   50
 31  \w     43.00  75.00   0.50    0.05    --   62.00  72.00  19.79   64
 32  \w     40.00  66.00   0.50    0.05    --   62.00  75.00  41.87   52
 33  \w     48.00  74.00   0.50    0.05    --   70.00  76.00  58.39   52
 34  \w     36.00  62.00   0.50    0.05    --   58.00  76.00 127.22   52
 35  \w     41.00  66.00   0.50    0.05    --   62.00  73.00  98.60   50
 36  \w    130.00 171.00   0.50    0.20    --  105.91  18.00  66.00   82
 37  \w     76.00 107.00   0.50    0.20    --  105.91 -77.00 -90.00   62
 38  \w     42.00  73.00   0.50    0.20    --  105.91 -61.00-180.00   62
 39  \w    -19.00   6.00   0.50    0.05    --   47.28 -18.00-102.00   50
 40  \w     40.00  65.00   0.50    0.20    --  105.91 -61.00  60.00   50
 41  \w     33.00  62.00   0.50    0.20    --  105.91 -77.00 -90.00   58
 42  \w     77.00 104.00   0.50    0.20    --  105.91 -94.00 -90.00   54
 43  \w     82.00 111.00   0.50    0.20    --  105.91-125.00-120.00   58
 44  \w     39.00 112.00   0.50    0.20    --  105.91-125.00-150.00  146
 45  \w     49.00  75.00   0.50    0.20    --  105.91-125.00-120.00   52
 46  \w     49.00 105.00   0.50    0.20    --  105.91-125.00-180.00  112
 47  \w     33.00  66.00   0.50    0.20    --  105.91 -94.00 -90.00   66
 48  \w     34.00  80.00   0.50    0.05    --   47.28-125.00 -90.00   92
 49  \w     45.00 104.00   0.50    0.20    --  105.91 -94.00-120.00  118
 50  \w     33.00 105.00   0.50    0.20    --  105.91 -94.00 -30.00  144
 51  \w     33.00 104.00   0.50    0.20    --  105.91 -94.00  30.00  142
 52  \w     73.00 106.00   0.50    0.20    --  105.91 -94.00  60.00   66
 53  \w     36.00  70.00   0.50    0.20    --  105.91 -94.00  60.00   68
 54  \w     33.00  79.00   0.50    0.20    --  105.91 -94.00 120.00   92
 55  \w    -23.00  21.00   0.50    0.05    --  -47.28  18.00  66.00   88
 56  \w    -62.00 -11.00   0.50    0.05    --  -47.28  57.00 120.00  102
 57  \w     -7.00  18.00   0.50    0.05    --  -47.28  57.00 120.00   50
 58  \w    -68.00 -31.00   0.50    0.20    --  -91.75  61.00  30.00   74
 59  \w    -48.00 -23.00   0.50    0.20    --  -91.75  45.00 -30.00   50
 60  \w    -92.00 -35.00   0.50    0.05    --  -47.28 -18.00-102.00  114
 61  \w    -86.00 -17.00   0.50    0.05    --  -47.28 125.00-150.00  138
 62  \w    -58.00 -32.00   0.50    0.05    --  -54.00 -77.00  85.47   52
 63  \w   -161.00 -71.00   0.50    0.20    --  -91.75 -77.00   0.00  180
 64  \w   -146.00 -69.00   0.50    0.20    --  -91.75 -77.00  60.00  154
 65  \w   -106.00 -80.00   0.50    0.05    --  -54.00 -77.00  85.47   52
 66  \w   -104.00 -69.00   0.50    0.20    --  -91.75 -77.00 170.37   70
 67  \w   -157.00 -69.00   0.50    0.20    --  -91.75 -77.00 150.00  176
 68  \w   -115.00 -69.00   0.50    0.20    --  -91.75 -76.00 108.67   92
 69  \w    -94.00 -59.00   0.50    0.20    --  -82.00 -76.00 -13.78   70
 70  \w   -162.00 -69.00   0.50    0.20    --  -91.75 -76.00 -43.12  186
 71  \w   -140.00 -71.00   0.50    0.20    --  -91.75 -77.00-120.00  138
 72  \w   -103.00 -69.00   0.50    0.20    --  -91.75 -77.00 -90.00   68
 73  \w    -84.00 -59.00   0.50    0.20    --  -82.00 -76.00-172.58   50
 74  \w   -161.00 -71.00   0.50    0.20    --  -91.75 -75.00-135.03  180
 75  \w   -128.00 -70.00   0.50    0.20    --  -91.75 -75.00-149.24  116
 76  \w   -162.00-133.00   0.50    0.20    --  -90.00 -75.00 -14.97   58
 77  \w   -100.00 -68.00   0.50    0.20    --  -90.00 -75.00 -14.97   64
 78  \w   -105.00 -70.00   0.50    0.20    --  -91.75 -75.00  49.48   70
 79  \w    -79.00 -53.00   0.50    0.20    --  -74.00 -74.00 159.26   52
 80  \w    -86.00 -60.00   0.50    0.20    --  -82.00 -74.00 152.01   52
 81  \w   -158.00 -70.00   0.50    0.20    --  -91.75 -74.00 129.73  176
 82  \w   -163.00-112.00   0.50    0.20    --  -91.75 -75.00  49.48  102
 83  \w    -85.00 -60.00   0.50    0.20    --  -82.00 -74.00  14.38   50
 84  \w   -160.00-109.00   0.50    0.20    --  -91.75 -73.00 -62.44  102
 85  \w   -137.00-111.00   0.50    0.20    --  -74.00 -73.00-125.19   52
 86  \w    -82.00 -56.00   0.50    0.20    --  -78.00 -74.00-145.83   52
 87  \w    -78.00 -53.00   0.50    0.20    --  -74.00 -73.00-125.19   50
 88  \w    -79.00 -53.00   0.50    0.20    --  -74.00 -73.00 -67.92   52
 89  \w    -96.00 -71.00   0.50    0.20    --  -91.75 -73.00-175.88   50
 90  \w   -162.00-116.00   0.50    0.20    --  -91.75 -73.00-175.88   92
 91  \w   -103.00 -71.00   0.50    0.20    --  -91.75 -73.00 -62.44   64
 92  \w    -86.00 -61.00   0.50    0.20    --  -82.00 -72.00 -48.63   50
 93  \w    -96.00 -71.00   0.50    0.20    --  -91.75 -73.00   6.15   50
 94  \w   -153.00-110.00   0.50    0.20    --  -91.75 -73.00   6.15   86
 95  \w    -94.00 -62.00   0.50    0.20    --  -82.00 -72.00  67.92   64
 96  \w    -89.00 -61.00   0.50    0.20    --  -82.00 -72.00  76.71   56
 97  \w    -79.00 -45.00   0.50    0.05    --  -66.00 -72.00  79.85   68
 98  \w    -78.00 -51.00   0.50    0.20    --  -70.00 -73.00 167.90   54
 99  \w   -104.00 -62.00   0.50    0.20    --  -82.00 -72.00 105.62   84
100  \w   -119.00 -72.00   0.50    0.20    --  -91.75 -71.00  71.16   94
101  \w   -150.00 -73.00   0.50    0.20    --  -91.75 -71.00  35.21  154
102  \w   -140.00-113.00   0.50    0.20    --  -82.00 -71.00 -74.15   54
103  \w   -159.00 -74.00   0.50    0.20    --  -91.75 -72.00-163.06  170
104  \w   -161.00 -70.00   0.50    0.20    --  -90.00 -71.00-110.03  182
105  \w    -92.00 -62.00   0.50    0.20    --  -82.00 -71.00 -74.15   60
106  \w   -162.00 -71.00   0.50    0.20    --  -91.75 -71.00 -79.84  182
107  \w   -163.00 -72.00   0.50    0.20    --  -91.75 -70.00  92.22  182
108  \w   -141.00-115.00   0.50    0.20    --  -91.75 -71.00 152.37   52
109  \w   -101.00 -71.00   0.50    0.20    --  -91.75 -71.00 152.37   60
110  \w    -75.00 -46.00   0.50    0.05    --  -66.00 -70.00 172.79   58
111  \w    -74.00 -48.00   0.50    0.05    --  -66.00 -68.00 128.47   52
112  \w    -78.00 -52.00   0.50    0.20    --  -70.00 -67.00 115.79   52
113  \w    -82.00 -56.00   0.50    0.20    --  -74.00 -67.00 106.36   52
114  \w    -94.00 -64.00   0.50    0.20    --  -82.00 -65.00-110.39   60
115  \w   -123.00 -97.00   0.50    0.20    --  -91.75 -18.00-102.00   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      -0.0300754000
_diffrn_orient_matrix_UB_12      0.1291454000
_diffrn_orient_matrix_UB_13      -0.0197167000
_diffrn_orient_matrix_UB_21      -0.1574384000
_diffrn_orient_matrix_UB_22      0.0158444000
_diffrn_orient_matrix_UB_23      0.0065531000
_diffrn_orient_matrix_UB_31      -0.0186799000
_diffrn_orient_matrix_UB_32      0.0000448000
_diffrn_orient_matrix_UB_33      0.0858732000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0665
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            71149
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.080
_diffrn_reflns_theta_max         67.080
_diffrn_reflns_theta_min         2.534
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.598
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.245
_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            colourless
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_description       block
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.464
_exptl_crystal_size_mid          0.266
_exptl_crystal_size_min          0.182
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         7735
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0420P)^2^+0.9745P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0839
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7452
_reflns_number_total             7735
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc01812a2.cif
_cod_data_source_block           FK-629B_a
_cod_depositor_comments
'Adding full bibliography for 1574297--1574307.cif.'
_cod_database_code               1574303
_shelx_shelxl_version_number     2019/3
_cell_oxdiff_length_a            10.27963(16)
_cell_oxdiff_length_b            12.9114(2)
_cell_oxdiff_length_c            18.3044(2)
_cell_oxdiff_angle_alpha         74.2670(13)
_cell_oxdiff_angle_beta          77.1074(13)
_cell_oxdiff_angle_gamma         69.7828(15)
_cell_oxdiff_volume              2171.70(6)
_cell_oxdiff_measurement_reflns_used 52754
_oxdiff_exptl_absorpt_empirical_full_min 0.736
_oxdiff_exptl_absorpt_empirical_full_max 1.696
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1
_chemical_oxdiff_formula         'C41 H63 N2 O3 P S Si'
_shelx_res_checksum              9593