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_1574301
_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         '2(C35 H38 N3 P Si), 0.5(C6 H6)'
_chemical_formula_sum            'C73 H79 N6 P2 Si2'
_chemical_formula_weight         1158.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-26
_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                 94.6640(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   64.6062(4)
_cell_length_b                   10.33540(10)
_cell_length_c                   19.79680(10)
_cell_measurement_reflns_used    45969
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.7120
_cell_measurement_theta_min      2.7260
_cell_volume                     13175.16(17)
_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 (G.M. Sheldrick, 2015)'
_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    -73.00  23.00   0.50    0.35    --  -47.28  84.00  39.00  192
  2  \w     -6.00  20.00   0.50    0.35    --   47.28 -84.00 -81.00   52
  3  \w    -85.00 -49.00   0.50    1.40    --  -91.75  84.00  39.00   72
  4  \w   -155.00-102.00   0.50    1.40    --  -91.75 -84.00 -81.00  106
  5  \w    143.00 178.00   0.50    1.40    --  105.91  84.00  39.00   70
  6  \w    101.00 136.00   0.50    1.40    --  105.91  84.00  39.00   70
  7  \w   -110.00 -73.00   0.50    0.35    --  -47.28-125.00  30.00   74
  8  \w   -117.00 -87.00   0.50    0.35    --  -47.28-125.00   0.00   60
  9  \w    -23.00  27.00   0.50    0.35    --  -47.28  19.00 -30.00  100
 10  \w    -50.00  25.00   0.50    0.35    --  -47.28  57.00-180.00  150
 11  \w    -62.00  24.00   0.50    0.35    --  -47.28  57.00 -60.00  172
 12  \w     -6.00  19.00   0.50    0.35    --  -47.28  19.00-150.00   50
 13  \w    -16.00  18.00   0.50    0.35    --   47.28 -19.00   0.00   68
 14  \w    -48.00 -22.00   0.50    1.40    --  -91.75  45.00 150.00   52
 15  \w    -48.00 -23.00   0.50    1.40    --  -91.75  45.00-120.00   50
 16  \w    -46.00 -20.00   0.50    1.40    --  -91.75  45.00 120.00   52
 17  \w   -124.00 -83.00   0.50    1.40    --  -91.75 -30.00 120.00   82
 18  \w    -48.00 -20.00   0.50    1.40    --  -91.75  45.00  60.00   56
 19  \w   -165.00-131.00   0.50    1.40    --  -91.75 -30.00 120.00   68
 20  \w    -68.00 -38.00   0.50    1.40    --  -91.75  61.00  30.00   60
 21  \w    -48.00 -22.00   0.50    1.40    --  -91.75  45.00-150.00   52
 22  \w     39.00  67.00   0.50    1.40    --  105.91 -77.00  90.00   56
 23  \w     35.00 101.00   0.50    1.40    --  105.91 -94.00  60.00  132
 24  \w     37.00  63.00   0.50    1.40    --  105.91 -61.00-180.00   52
 25  \w     44.00 112.00   0.50    1.40    --  105.91-125.00   0.00  136
 26  \w     73.00 105.00   0.50    1.40    --  105.91 -94.00 150.00   64
 27  \w     38.00 106.00   0.50    1.40    --  105.91 -94.00  90.00  136
 28  \w    124.00 178.00   0.50    1.40    --  105.91  45.00   0.00  108
 29  \w     93.00 119.00   0.50    1.40    --  105.91  45.00   0.00   52
 30  \w     33.00  98.00   0.50    1.40    --  105.91 -94.00-150.00  130
 31  \w     34.00  59.00   0.50    1.40    --  105.91 -61.00 -90.00   50
 32  \w     93.00 178.00   0.50    1.40    --  105.91  30.00 -30.00  170
 33  \w     38.00 106.00   0.50    1.40    --  105.91 -94.00-120.00  136
 34  \w     36.00  61.00   0.50    1.40    --  105.91 -77.00 120.00   50
 35  \w    105.00 130.00   0.50    1.40    --  105.91  15.00-180.00   50
 36  \w    153.00 178.00   0.50    1.40    --  105.91  15.00-180.00   50
 37  \w     81.00 106.00   0.50    1.40    --  105.91 -94.00 -90.00   50
 38  \w     42.00  67.00   0.50    1.40    --  105.91 -94.00 -90.00   50
 39  \w     36.00  68.00   0.50    1.40    --  105.91 -95.00  10.06   64
 40  \w     42.00  74.00   0.50    1.40    --  105.91 -61.00 120.00   64
 41  \w     94.00 178.00   0.50    1.40    --  105.91  30.00 -90.00  168
 42  \w     83.00 108.00   0.50    1.40    --  105.91 -77.00  90.00   50
 43  \w     75.00 100.00   0.50    1.40    --  105.91 -77.00 120.00   50
 44  \w     36.00 108.00   0.50    1.40    --  105.91-112.00  66.38  144
 45  \w     60.00  85.00   0.50    1.40    --  105.91 -84.00 -81.00   50
;
_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      0.0195794000
_diffrn_orient_matrix_UB_12      -0.0139766000
_diffrn_orient_matrix_UB_13      -0.0389565000
_diffrn_orient_matrix_UB_21      -0.0076137500
_diffrn_orient_matrix_UB_22      -0.1334177500
_diffrn_orient_matrix_UB_23      -0.0263052000
_diffrn_orient_matrix_UB_31      -0.0114501500
_diffrn_orient_matrix_UB_32      0.0650313500
_diffrn_orient_matrix_UB_33      -0.0623516000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0592
_diffrn_reflns_av_unetI/netI     0.0140
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       77
_diffrn_reflns_limit_h_min       -77
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12149
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.000
_diffrn_reflns_theta_min         2.745
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.297
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.571
_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    1.168
_exptl_crystal_description       block
_exptl_crystal_F_000             4936
_exptl_crystal_size_max          0.404
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.882
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.184
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     755
_refine_ls_number_reflns         12149
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.184
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0618
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0831P)^2^+36.8808P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1830
_refine_ls_wR_factor_ref         0.1845
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11551
_reflns_number_total             12149
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc01812a2.cif
_cod_data_source_block           MAS-003_twin1_hklf5
_cod_depositor_comments
'Adding full bibliography for 1574297--1574307.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1574301
_shelx_shelxl_version_number     2019/3
_cell_oxdiff_length_a            64.6027(4)
_cell_oxdiff_length_b            10.33380(7)
_cell_oxdiff_length_c            19.79452(11)
_cell_oxdiff_angle_alpha         89.9998(5)
_cell_oxdiff_angle_beta          94.6507(4)
_cell_oxdiff_angle_gamma         89.9605(5)
_cell_oxdiff_volume              13171.14(14)
_cell_oxdiff_measurement_reflns_used 47386
_oxdiff_exptl_absorpt_empirical_full_min 0.711
_oxdiff_exptl_absorpt_empirical_full_max 2.256
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_oxdiff_digest_frames
;
01cb4fa651b7cacb0c491abe1963356718037709614
;
_diffrn_oxdiff_digest_hkl
;
015e8076625673d76a6c98c9002a20bf38e10f
;
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1
_chemical_oxdiff_formula         'C35 H38 N3 Si1 P1'
_shelx_res_checksum              25509