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_1574299
_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         'C36 H38 N3 P S2 Si'
_chemical_formula_sum            'C36 H38 N3 P S2 Si'
_chemical_formula_weight         635.87
_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             2022-05-04
_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                 114.3500(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.81430(10)
_cell_length_b                   14.40780(10)
_cell_length_c                   17.4032(2)
_cell_measurement_reflns_used    29052
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.3530
_cell_measurement_theta_min      3.2620
_cell_volume                     3384.13(6)
_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 0.981
_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    -72.00  -2.00   0.50    0.35    --  -47.28 106.00 -51.00  140
  2  \w     24.00  73.00   0.50    0.35    --   47.28-106.00-150.00   98
  3  \w   -141.00 -87.00   0.50    1.40    --  -91.75-106.00-150.00  108
  4  \w    117.00 142.00   0.50    1.40    --  105.91 106.00 -51.00   50
  5  \w     68.00 107.00   0.50    1.40    --  105.91-106.00-150.00   78
  6  \w     35.00  62.00   0.50    1.40    --  105.91-106.00-150.00   54
  7  \w   -119.00 -92.00   0.50    0.35    --  -47.28-125.00 -60.00   54
  8  \w   -105.00 -78.00   0.50    0.35    --  -47.28-125.00  60.00   54
  9  \w   -119.00 -92.00   0.50    0.35    --  -47.28-125.00  30.00   54
 10  \w   -116.00 -89.00   0.50    0.35    --  -47.28-125.00   0.00   54
 11  \w   -115.00 -73.00   0.50    0.35    --  -47.28-125.00 -90.00   84
 12  \w    -35.00  26.00   0.50    0.35    --  -47.28  38.00 -30.00  122
 13  \w    -40.00  26.00   0.50    0.35    --  -47.28  38.00-150.00  132
 14  \w    -61.00  25.00   0.50    0.35    --  -47.28  57.00 -90.00  172
 15  \w    -68.00 -21.00   0.50    1.40    --  -91.75  61.00  60.00   94
 16  \w    -68.00 -19.00   0.50    1.40    --  -91.75  61.00 -30.00   98
 17  \w   -166.00 -78.00   0.50    1.40    --  -91.75 -15.00  90.00  176
 18  \w    -48.00 -23.00   0.50    1.40    --  -91.75  45.00 150.00   50
 19  \w    -47.00 -21.00   0.50    1.40    --  -91.75  45.00  30.00   52
 20  \w   -126.00 -88.00   0.50    1.40    --  -91.75 -94.00  30.00   76
 21  \w    -75.00 -49.00   0.50    1.40    --  -91.75 106.00 -51.00   52
 22  \w    -48.00 -20.00   0.50    1.40    --  -91.75  45.00-120.00   56
 23  \w   -163.00 -80.00   0.50    1.40    --  -91.75 -45.00 -90.00  166
 24  \w     40.00  65.00   0.50    1.40    --  105.91 -94.00   0.00   50
 25  \w     36.00  61.00   0.50    1.40    --  105.91 -61.00 -30.00   50
 26  \w     69.00 106.00   0.50    1.40    --  105.91 -94.00-150.00   74
 27  \w     34.00  63.00   0.50    1.40    --  105.91 -94.00-150.00   58
 28  \w     44.00 103.00   0.50    1.40    --  105.91 -94.00 -90.00  118
 29  \w     34.00  80.00   0.50    1.40    --  105.91 -94.00-120.00   92
 30  \w     42.00  74.00   0.50    1.40    --  105.91 -61.00  60.00   64
 31  \w     48.00 172.00   0.50    1.40    --  105.91   0.00-150.00  248
 32  \w     33.00 105.00   0.50    1.40    --  105.91 -95.00  42.99  144
 33  \w     33.00  98.00   0.50    1.40    --  105.91 -94.00 150.00  130
 34  \w     68.00 106.00   0.50    1.40    --  105.91 -94.00  90.00   76
 35  \w     45.00  71.00   0.50    1.40    --  105.91 -61.00 120.00   52
 36  \w     42.00  68.00   0.50    1.40    --  105.91 -94.00  60.00   52
 37  \w    100.00 172.00   0.50    1.40    --  105.91  15.00-120.00  144
 38  \w     35.00  63.00   0.50    1.40    --  105.91 -94.00  90.00   56
 39  \w     44.00  70.00   0.50    1.40    --  105.91 -61.00-150.00   52
 40  \w     58.00  89.00   0.50    1.40    --  105.91 -94.00 -60.00   62
 41  \w     76.00 101.00   0.50    1.40    --  105.91 -94.00  60.00   50
 42  \w     33.00 105.00   0.50    1.40    --  105.91 -94.00 -30.00  144
 43  \w     68.00  95.00   0.50    1.40    --  105.91 -94.00   0.00   54
;
_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      0.1076964000
_diffrn_orient_matrix_UB_12      -0.0263681000
_diffrn_orient_matrix_UB_13      0.0183598000
_diffrn_orient_matrix_UB_21      0.0329265000
_diffrn_orient_matrix_UB_22      0.0313187000
_diffrn_orient_matrix_UB_23      0.0922510000
_diffrn_orient_matrix_UB_31      -0.0182850000
_diffrn_orient_matrix_UB_32      -0.0988456000
_diffrn_orient_matrix_UB_33      0.0243173000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_sigmaI/netI    0.0534
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            45900
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.881
_diffrn_reflns_theta_min         3.275
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.431
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64035
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       block
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.207
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.078
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.049
_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     394
_refine_ls_number_reflns         7005
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0491P)^2^+1.5226P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.0913
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6443
_reflns_number_total             7005
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc01812a2.cif
_cod_data_source_block           MAS-014_auto_a
_cod_depositor_comments
'Adding full bibliography for 1574297--1574307.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1574299
_shelx_shelxl_version_number     2019/3
_cell_oxdiff_length_a            14.8212(3)
_cell_oxdiff_length_b            14.3993(2)
_cell_oxdiff_length_c            17.4054(3)
_cell_oxdiff_angle_alpha         90.0111(13)
_cell_oxdiff_angle_beta          114.3497(17)
_cell_oxdiff_angle_gamma         89.9906(14)
_cell_oxdiff_volume              3384.14(10)
_cell_oxdiff_measurement_reflns_used 29052
_oxdiff_exptl_absorpt_empirical_full_min 0.692
_oxdiff_exptl_absorpt_empirical_full_max 1.565
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_oxdiff_digest_frames
;
01fb120b75d931ad51bdc70a57907bef31005834803
;
_diffrn_oxdiff_digest_hkl
;
0140effcf0389a0a2033369eedbe90d9b61e6e
;
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1
_chemical_oxdiff_formula         'C20 H20 N3 Si1 P1 S2'
_shelx_res_checksum              28588