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_1574297
_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 O2 P S Si'
_chemical_formula_sum            'C41 H63 N2 O2 P S Si'
_chemical_formula_weight         707.05
_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             2021-11-19
_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                103.2980(10)
_cell_angle_beta                 98.3310(10)
_cell_angle_gamma                90.0900(10)
_cell_formula_units_Z            2
_cell_length_a                   9.87940(10)
_cell_length_b                   9.96850(10)
_cell_length_c                   21.1954(3)
_cell_measurement_reflns_used    17923
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.3040
_cell_measurement_theta_min      4.2680
_cell_volume                     2008.66(4)
_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 0.998
_diffrn_measured_fraction_theta_max 0.997
_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     94.00 178.00   0.50    0.60    --  105.91  45.00   0.00  168
  2  \w    103.00 142.00   0.50    0.60    --  105.91  91.00 -89.00   78
  3  \w    113.00 139.00   0.50    0.60    --  105.91  30.00-150.00   52
  4  \w    148.00 178.00   0.50    0.60    --  105.91  30.00-150.00   60
  5  \w     71.00 111.00   0.50    0.60    --  105.91-125.00   0.00   80
  6  \w     52.00 112.00   0.50    0.60    --  105.91-125.00  60.00  120
  7  \w     40.00  75.00   0.50    0.60    --  105.91 -98.00  79.69   70
  8  \w     79.00 106.00   0.50    0.60    --  105.91 -98.00  79.69   54
  9  \w     33.00  87.00   0.50    0.60    --  105.91 -94.00  90.00  108
 10  \w     51.00 105.00   0.50    0.60    --  105.91 -94.00 120.00  108
 11  \w     39.00 105.00   0.50    0.60    --  105.91 -94.00 -30.00  132
 12  \w     15.00  70.00   0.50    0.15    --   47.28 -91.00 156.00  110
 13  \w     45.00  70.00   0.50    0.60    --  105.91 -91.00 156.00   50
 14  \w     39.00 100.00   0.50    0.60    --  105.91 -94.00-120.00  122
 15  \w     51.00 106.00   0.50    0.60    --  105.91 -94.00-150.00  110
 16  \w     64.00 103.00   0.50    0.60    --  105.91 -94.00-180.00   78
 17  \w    -15.00  22.00   0.50    0.15    --   47.28 -19.00 -90.00   74
 18  \w     46.00  74.00   0.50    0.60    --  105.91 -61.00-120.00   56
 19  \w     37.00  81.00   0.50    0.60    --  105.91 -77.00 -30.00   88
 20  \w     33.00  59.00   0.50    0.60    --  105.91 -77.00 150.00   52
 21  \w    -38.00  26.00   0.50    0.15    --  -47.28  38.00-150.00  128
 22  \w    -21.00  21.00   0.50    0.15    --  -47.28  19.00-180.00   84
 23  \w    -16.00  13.00   0.50    0.15    --  -47.28  19.00 -30.00   58
 24  \w    -74.00  23.00   0.50    0.15    --  -47.28  91.00 -89.00  194
 25  \w    -82.00 -21.00   0.50    0.60    --  -91.75 125.00 -60.00  122
 26  \w    -77.00 -51.00   0.50    0.60    --  -91.75  91.00 -89.00   52
 27  \w    -63.00 -19.00   0.50    0.60    --  -91.75  61.00-180.00   88
 28  \w    -48.00 -23.00   0.50    0.60    --  -91.75  45.00-180.00   50
 29  \w    -48.00 -23.00   0.50    0.60    --  -91.75  45.00 -90.00   50
 30  \w    -48.00 -23.00   0.50    0.60    --  -91.75  45.00-150.00   50
 31  \w    -48.00 -20.00   0.50    0.60    --  -91.75  45.00  30.00   56
 32  \w    -47.00 -20.00   0.50    0.60    --  -91.75  45.00  90.00   54
 33  \w    -49.00 -21.00   0.50    0.60    --  -91.75  61.00 120.00   56
 34  \w    -48.00 -20.00   0.50    0.60    --  -91.75  45.00 120.00   56
 35  \w    -66.00 -33.00   0.50    0.60    --  -91.75  61.00  60.00   66
 36  \w   -162.00-130.00   0.50    0.60    --  -91.75 -15.00 -90.00   64
 37  \w   -162.00-125.00   0.50    0.60    --  -91.75 -15.00-150.00   74
 38  \w   -110.00 -84.00   0.50    0.60    --  -91.75 -15.00-150.00   52
 39  \w   -119.00 -79.00   0.50    0.60    --  -91.75 -15.00 -90.00   80
 40  \w   -120.00 -92.00   0.50    0.15    --  -47.28 -19.00-120.00   56
 41  \w   -119.00 -73.00   0.50    0.15    --  -47.28-125.00 -60.00   92
 42  \w   -162.00 -87.00   0.50    0.60    --  -91.75 -91.00 156.00  150
;
_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      -0.0463837000
_diffrn_orient_matrix_UB_12      -0.1236479000
_diffrn_orient_matrix_UB_13      -0.0578629000
_diffrn_orient_matrix_UB_21      -0.0781486000
_diffrn_orient_matrix_UB_22      0.0974388000
_diffrn_orient_matrix_UB_23      -0.0380784000
_diffrn_orient_matrix_UB_31      0.1288873000
_diffrn_orient_matrix_UB_32      0.0216288000
_diffrn_orient_matrix_UB_33      -0.0301175000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_sigmaI/netI    0.0497
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24161
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.996
_diffrn_reflns_theta_min         4.335
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.643
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.447
_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            yellow
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_description       block
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         7289
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0443P)^2^+0.9183P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0916
_refine_ls_wR_factor_ref         0.0938
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6657
_reflns_number_total             7289
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc01812a2.cif
_cod_data_source_block           FK-362_auto_a
_cod_depositor_comments
'Adding full bibliography for 1574297--1574307.cif.'
_cod_database_code               1574297
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.714
_shelx_estimated_absorpt_t_max   0.908
_cell_oxdiff_length_a            9.87936(12)
_cell_oxdiff_length_b            9.96848(14)
_cell_oxdiff_length_c            21.1954(3)
_cell_oxdiff_angle_alpha         103.2977(11)
_cell_oxdiff_angle_beta          98.3311(10)
_cell_oxdiff_angle_gamma         90.0900(10)
_cell_oxdiff_volume              2008.64(4)
_cell_oxdiff_measurement_reflns_used 17923
_oxdiff_exptl_absorpt_empirical_full_min 0.788
_oxdiff_exptl_absorpt_empirical_full_max 1.299
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_oxdiff_digest_frames
;
01b76e03839e56eb4c264cfa7e5c74c8c503502c981
;
_diffrn_oxdiff_digest_hkl
;
01d4c33f2cc89a305b3080e0149878933874ef
;
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1
_chemical_oxdiff_formula         'C41 H63 N2 O2 Si1 P1 S1'
_shelx_res_checksum              91810