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_1574298
_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_absolute_configuration unk
_chemical_formula_moiety         'C41 H45 N2 O2 P S Si'
_chemical_formula_sum            'C41 H45 N2 O2 P S Si'
_chemical_formula_weight         688.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-25
_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                90
_cell_angle_beta                 94.8050(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.86550(10)
_cell_length_b                   10.66970(10)
_cell_length_c                   17.54370(10)
_cell_measurement_reflns_used    43659
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.2920
_cell_measurement_theta_min      4.4720
_cell_volume                     1840.19(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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   -120.00 -34.00   0.50    0.20    --  -47.28 -38.00 -40.00  172
  2  \w    -40.00  26.00   0.50    0.20    --  -47.28  38.00 114.00  132
  3  \w     35.00 120.00   0.50    0.20    --   47.28  38.00 114.00  170
  4  \w    -26.00  46.00   0.50    0.20    --   47.28 -38.00 -40.00  144
  5  \w   -165.00 -78.00   0.50    0.80    --  -91.75 -38.00 -40.00  174
  6  \w     93.00 178.00   0.50    0.80    --  105.91  38.00 114.00  170
  7  \w   -119.00 -73.00   0.50    0.20    --  -47.28-125.00 -60.00   92
  8  \w   -119.00 -73.00   0.50    0.20    --  -47.28-125.00 120.00   92
  9  \w    -40.00  26.00   0.50    0.20    --  -47.28  38.00-120.00  132
 10  \w    -40.00  26.00   0.50    0.20    --  -47.28  38.00-180.00  132
 11  \w   -119.00 -73.00   0.50    0.20    --  -47.28-125.00 -90.00   92
 12  \w     34.00  95.00   0.50    0.20    --   47.28-125.00   0.00  122
 13  \w    -48.00 -20.00   0.50    0.80    --  -91.75  45.00-150.00   56
 14  \w    -48.00 -20.00   0.50    0.80    --  -91.75  45.00 -90.00   56
 15  \w   -166.00 -78.00   0.50    0.80    --  -91.75 -15.00  30.00  176
 16  \w    -68.00 -19.00   0.50    0.80    --  -91.75  61.00 -60.00   98
 17  \w    -85.00 -19.00   0.50    0.80    --  -91.75 125.00  30.00  132
 18  \w    -48.00 -20.00   0.50    0.80    --  -91.75  45.00 -60.00   56
 19  \w   -163.00 -77.00   0.50    0.80    --  -91.75 -56.00-165.16  172
 20  \w    -85.00 -19.00   0.50    0.80    --  -91.75 125.00-180.00  132
 21  \w    -48.00 -20.00   0.50    0.80    --  -91.75  45.00 120.00   56
 22  \w     93.00 178.00   0.50    0.80    --  105.91  45.00  30.00  170
 23  \w     33.00 108.00   0.50    0.80    --  105.91 -77.00 -30.00  150
 24  \w     33.00 106.00   0.50    0.80    --  105.91 -94.00 120.00  146
 25  \w     34.00 112.00   0.50    0.80    --  105.91-125.00  30.00  156
 26  \w     33.00  74.00   0.50    0.80    --  105.91 -61.00 120.00   82
 27  \w     34.00 112.00   0.50    0.80    --  105.91-125.00-150.00  156
 28  \w     34.00 112.00   0.50    0.80    --  105.91-125.00 -90.00  156
 29  \w     33.00  74.00   0.50    0.80    --  105.91 -61.00 -30.00   82
 30  \w     33.00  74.00   0.50    0.80    --  105.91 -61.00-180.00   82
 31  \w     34.00 112.00   0.50    0.80    --  105.91-125.00 -30.00  156
 32  \w     33.00 106.00   0.50    0.80    --  105.91 -96.00  46.18  146
 33  \w     33.00  74.00   0.50    0.80    --  105.91 -61.00 -60.00   82
 34  \w     33.00  74.00   0.50    0.80    --  105.91 -61.00  90.00   82
 35  \w     93.00 178.00   0.50    0.80    --  105.91  45.00-180.00  170
 36  \w     33.00  74.00   0.50    0.80    --  105.91 -61.00-120.00   82
 37  \w     33.00 106.00   0.50    0.80    --  105.91 -94.00  90.00  146
 38  \w     33.00 106.00   0.50    0.80    --  105.91 -94.00  60.00  146
 39  \w   -119.00 -25.00   0.50    0.20    --  -47.28 -77.00  60.00  188
 40  \w   -119.00 -32.00   0.50    0.20    --  -47.28 -57.00 150.00  174
 41  \w   -119.00 -25.00   0.50    0.20    --  -47.28 -77.00 120.00  188
 42  \w   -119.00 -25.00   0.50    0.20    --  -47.28 -77.00-120.00  188
 43  \w   -119.00 -32.00   0.50    0.20    --  -47.28 -57.00 -90.00  174
 44  \w     25.00 119.00   0.50    0.20    --   47.28  77.00-180.00  188
 45  \w     25.00 119.00   0.50    0.20    --   47.28  77.00   0.00  188
 46  \w     25.00 119.00   0.50    0.20    --   47.28  77.00-120.00  188
 47  \w     25.00 119.00   0.50    0.20    --   47.28  77.00 -60.00  188
 48  \w   -163.00 -74.00   0.50    0.80    --  -91.75 -64.00-126.42  178
 49  \w   -163.00 -70.00   0.50    0.80    --  -91.75 -74.00  19.63  186
 50  \w   -163.00 -69.00   0.50    0.80    --  -91.75 -77.00 150.00  188
 51  \w   -163.00 -70.00   0.50    0.80    --  -91.75 -74.00 -49.87  186
 52  \w   -163.00 -69.00   0.50    0.80    --  -91.75 -76.00  70.69  188
 53  \w   -163.00 -69.00   0.50    0.80    --  -91.75 -76.00 -70.88  188
 54  \w   -163.00 -74.00   0.50    0.80    --  -91.75 -64.00 -98.79  178
 55  \w   -163.00 -69.00   0.50    0.80    --  -91.75 -77.00  43.18  188
 56  \w   -163.00 -69.00   0.50    0.80    --  -91.75 -77.00-180.00  188
 57  \w   -163.00 -71.00   0.50    0.80    --  -91.75 -72.00 -27.68  184
 58  \w   -163.00 -71.00   0.50    0.80    --  -91.75 -71.00 100.89  184
;
_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      0.0461259000
_diffrn_orient_matrix_UB_12      0.1279441000
_diffrn_orient_matrix_UB_13      0.0336111000
_diffrn_orient_matrix_UB_21      0.1404443000
_diffrn_orient_matrix_UB_22      -0.0557358000
_diffrn_orient_matrix_UB_23      0.0257765000
_diffrn_orient_matrix_UB_31      0.0520051000
_diffrn_orient_matrix_UB_32      0.0370705000
_diffrn_orient_matrix_UB_33      -0.0772664000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_av_sigmaI/netI    0.0605
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            53970
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.984
_diffrn_reflns_theta_min         2.527
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.792
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.562
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
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    1.243
_exptl_crystal_description       block
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details
;
 Flack x determined using 3048 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         6680
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0276
_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^)+(0.0492P)^2^+0.4073P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0734
_reflns_Friedel_coverage         0.887
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                6585
_reflns_number_total             6680
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc01812a2.cif
_cod_data_source_block           MAS-002_auto_a
_cod_depositor_comments
'Adding full bibliography for 1574297--1574307.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1574298
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.705
_shelx_estimated_absorpt_t_max   0.885
_cell_oxdiff_length_a            9.86533(8)
_cell_oxdiff_length_b            10.66896(8)
_cell_oxdiff_length_c            17.54476(14)
_cell_oxdiff_angle_alpha         89.9968(6)
_cell_oxdiff_angle_beta          94.7868(7)
_cell_oxdiff_angle_gamma         90.0044(6)
_cell_oxdiff_volume              1840.19(2)
_cell_oxdiff_measurement_reflns_used 43659
_oxdiff_exptl_absorpt_empirical_full_min 0.748
_oxdiff_exptl_absorpt_empirical_full_max 1.698
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_oxdiff_digest_frames
;
01bea40c6f59478fabc58de725c1a6b01f08448c247
;
_diffrn_oxdiff_digest_hkl
;
01e26f5776cfa529c6884a56d09d417a853467
;
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1
_chemical_oxdiff_formula         'C30 H40 N2 O2 Si1 P1 S1'
_shelx_res_checksum              50732