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_1574305
_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         'C70 H76 N6 O2 P2 Si2, 4(C6 H6)'
_chemical_formula_sum            'C94 H100 N6 O2 P2 Si2'
_chemical_formula_weight         1463.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-17
_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                 96.7770(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.82520(10)
_cell_length_b                   16.08220(10)
_cell_length_c                   26.2606(2)
_cell_measurement_reflns_used    30352
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.3740
_cell_measurement_theta_min      2.6720
_cell_volume                     8314.24(9)
_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 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     58.00  84.00   0.50    0.50    --  105.91 -77.00  60.00   52
  2  \w     33.00  62.00   0.50    0.50    --  105.91 -77.00 -30.00   58
  3  \w     33.00  73.00   0.50    0.50    --  105.91 -61.00 -30.00   80
  4  \w     93.00 177.00   0.50    0.50    --  105.91  45.00 -60.00  168
  5  \w    102.00 155.00   0.50    0.50    --  105.91 113.00-159.00  106
  6  \w     46.00  80.00   0.50    0.50    --  105.91 -77.00-180.00   68
  7  \w    -22.00  16.00   0.50    0.12    --   47.28 -19.00-150.00   76
  8  \w    -60.00  21.00   0.50    0.12    --  -47.28  57.00   0.00  162
  9  \w    -39.00  25.00   0.50    0.12    --  -47.28  38.00-120.00  128
 10  \w    -39.00  11.00   0.50    0.12    --  -47.28  38.00 -60.00  100
 11  \w     -7.00  19.00   0.50    0.12    --  -47.28  57.00 120.00   52
 12  \w    -61.00 -35.00   0.50    0.12    --  -47.28  57.00 120.00   52
 13  \w    -48.00 -21.00   0.50    0.50    --  -91.75  45.00 120.00   54
 14  \w    -48.00 -22.00   0.50    0.50    --  -91.75  45.00  60.00   52
 15  \w    -67.00 -28.00   0.50    0.50    --  -91.75 125.00   0.00   78
 16  \w    -49.00 -19.00   0.50    0.50    --  -91.75 125.00 -30.00   60
 17  \w    -83.00 -19.00   0.50    0.50    --  -91.75 125.00-150.00  128
 18  \w    -80.00 -41.00   0.50    0.50    --  -91.75 113.00-159.00   78
 19  \w    -75.00  -4.00   0.50    0.12    --  -47.28 113.00-159.00  142
 20  \w    -48.00 -23.00   0.50    0.50    --  -91.75  45.00-120.00   50
 21  \w   -143.00-116.00   0.50    0.50    --  -91.75 -61.00-180.00   54
 22  \w   -143.00 -84.00   0.50    0.50    --  -91.75 -45.00-150.00  118
 23  \w   -107.00 -81.00   0.50    0.50    --  -91.75 -61.00-180.00   52
 24  \w   -166.00 -88.00   0.50    0.50    --  -91.75 -30.00-120.00  156
 25  \w   -161.00 -87.00   0.50    0.50    --  -91.75 -45.00 120.00  148
 26  \w   -143.00 -86.00   0.50    0.50    --  -91.75 -15.00 150.00  114
 27  \w   -122.00 -83.00   0.50    0.50    --  -91.75-113.00 108.00   78
 28  \w   -115.00 -90.00   0.50    0.12    --  -47.28-125.00 -60.00   50
 29  \w   -119.00 -94.00   0.50    0.12    --  -47.28-125.00-150.00   50
 30  \w     80.00 112.00   0.50    0.50    --  105.91-125.00   0.00   64
 31  \w     68.00 112.00   0.50    0.50    --  105.91-125.00 -30.00   88
 32  \w     37.00  63.00   0.50    0.50    --  105.91-125.00   0.00   52
 33  \w     34.00  88.00   0.50    0.50    --  105.91-125.00  60.00  108
 34  \w     74.00 108.00   0.50    0.50    --  105.91-113.00 108.00   68
 35  \w     27.00  81.00   0.50    0.12    --   47.28-113.00 108.00  108
 36  \w     45.00 105.00   0.50    0.50    --  105.91 -94.00  30.00  120
 37  \w     53.00  93.00   0.50    0.50    --  105.91 -94.00  60.00   80
 38  \w     33.00 100.00   0.50    0.50    --  105.91 -94.00 120.00  134
 39  \w     48.00  96.00   0.50    0.50    --  105.91 -94.00 150.00   96
 40  \w     34.00 104.00   0.50    0.50    --  105.91 -94.00 -60.00  140
 41  \w     81.00 106.00   0.50    0.50    --  105.91-101.00-165.47   50
 42  \w     37.00 100.00   0.50    0.50    --  105.91 -94.00-180.00  126
;
_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      -0.0063692000
_diffrn_orient_matrix_UB_12      0.0408643000
_diffrn_orient_matrix_UB_13      0.0522958000
_diffrn_orient_matrix_UB_21      -0.0573254000
_diffrn_orient_matrix_UB_22      0.0561974000
_diffrn_orient_matrix_UB_23      -0.0252977000
_diffrn_orient_matrix_UB_31      -0.0528758000
_diffrn_orient_matrix_UB_32      -0.0658812000
_diffrn_orient_matrix_UB_33      0.0108735000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0608
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            53814
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.068
_diffrn_reflns_theta_max         67.068
_diffrn_reflns_theta_min         3.229
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.148
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.202
_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    1.170
_exptl_crystal_description       block
_exptl_crystal_F_000             3120
_exptl_crystal_size_max          0.446
_exptl_crystal_size_mid          0.326
_exptl_crystal_size_min          0.313
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         7425
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0620P)^2^+8.5108P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1114
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6997
_reflns_number_total             7425
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc01812a2.cif
_cod_data_source_block           MAS-019_a
_cod_depositor_comments
'Adding full bibliography for 1574297--1574307.cif.'
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               1574305
_shelx_shelxl_version_number     2019/3
_cell_oxdiff_length_a            19.8251(3)
_cell_oxdiff_length_b            16.0892(2)
_cell_oxdiff_length_c            26.2471(4)
_cell_oxdiff_angle_alpha         89.9884(12)
_cell_oxdiff_angle_beta          96.7328(12)
_cell_oxdiff_angle_gamma         90.0143(11)
_cell_oxdiff_volume              8314.3(2)
_cell_oxdiff_measurement_reflns_used 30352
_oxdiff_exptl_absorpt_empirical_full_min 0.794
_oxdiff_exptl_absorpt_empirical_full_max 1.333
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1
_chemical_oxdiff_formula         'C70 H72 N6 O2 Si2 P2 '
_shelx_res_checksum              9996