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_1574307
_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         'C46 H72 N3 O2 P S Si'
_chemical_formula_sum            'C46 H72 N3 O2 P S Si'
_chemical_formula_weight         790.18
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-14
_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                 100.7750(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.42850(10)
_cell_length_b                   27.55120(10)
_cell_length_c                   14.39760(10)
_cell_measurement_reflns_used    66367
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.5010
_cell_measurement_theta_min      3.2080
_cell_volume                     4453.43(5)
_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   -122.00 -34.00   0.50    0.90    --  -47.28 -18.00  37.00  176
  2  \w    -23.00  28.00   0.50    0.90    --  -47.28  18.00-153.00  102
  3  \w    -27.00  29.00   0.50    0.90    --   47.28 -18.00  37.00  112
  4  \w     34.00 122.00   0.50    0.90    --   47.28  18.00-153.00  176
  5  \w   -166.00 -79.00   0.50    3.60    --  -91.75 -18.00  37.00  174
  6  \w     93.00 178.00   0.50    3.60    --  105.91  18.00-153.00  170
  7  \w    -23.00  28.00   0.50    0.90    --  -47.28  19.00-120.00  102
  8  \w    -23.00  28.00   0.50    0.90    --  -47.28  19.00   0.00  102
  9  \w    -70.00  25.00   0.50    0.90    --  -47.28  77.00 150.00  190
 10  \w    -86.00 -13.00   0.50    0.90    --  -47.28 125.00-180.00  146
 11  \w    -40.00  26.00   0.50    0.90    --  -47.28  38.00 -90.00  132
 12  \w    -24.00  62.00   0.50    0.90    --   47.28 -57.00-180.00  172
 13  \w   -166.00 -78.00   0.50    3.60    --  -91.75 -15.00 120.00  176
 14  \w    -48.00 -20.00   0.50    3.60    --  -91.75  45.00 -90.00   56
 15  \w    -85.00 -19.00   0.50    3.60    --  -91.75 125.00 -60.00  132
 16  \w    -48.00 -20.00   0.50    3.60    --  -91.75  45.00 150.00   56
 17  \w    -48.00 -20.00   0.50    3.60    --  -91.75  45.00 120.00   56
 18  \w   -102.00 -19.00   0.50    3.60    --  -91.75  77.00 -30.00  166
 19  \w    -85.00 -19.00   0.50    3.60    --  -91.75 125.00  30.00  132
 20  \w    -68.00 -19.00   0.50    3.60    --  -91.75  61.00  60.00   98
 21  \w     93.00 178.00   0.50    3.60    --  105.91  45.00 -60.00  170
 22  \w     33.00 106.00   0.50    3.60    --  105.91 -94.00-150.00  146
 23  \w     34.00 112.00   0.50    3.60    --  105.91-125.00  60.00  156
 24  \w     33.00 106.00   0.50    3.60    --  105.91 -94.00  30.00  146
 25  \w     33.00 106.00   0.50    3.60    --  105.91 -94.00-120.00  146
 26  \w     34.00 112.00   0.50    3.60    --  105.91-125.00 120.00  156
 27  \w     92.00 178.00   0.50    3.60    --  105.91  15.00 -60.00  172
 28  \w     33.00 106.00   0.50    3.60    --  105.91 -94.00 120.00  146
 29  \w     33.00 106.00   0.50    3.60    --  105.91 -94.00   0.00  146
 30  \w     33.00 108.00   0.50    3.60    --  105.91 -77.00 120.00  150
 31  \w     33.00 106.00   0.50    3.60    --  105.91 -94.00 -30.00  146
 32  \w     33.00 106.00   0.50    3.60    --  105.91 -94.00 -60.00  146
 33  \w     33.00  74.00   0.50    3.60    --  105.91 -61.00-150.00   82
 34  \w     33.00 108.00   0.50    3.60    --  105.91-110.00 142.35  150
 35  \w     93.00 178.00   0.50    3.60    --  105.91  30.00-150.00  170
 36  \w     33.00 106.00   0.50    3.60    --  105.91 -94.00-180.00  146
 37  \w     33.00  74.00   0.50    3.60    --  105.91 -61.00-120.00   82
 38  \w     93.00 178.00   0.50    3.60    --  105.91  45.00  60.00  170
 39  \w     35.00 122.00   0.50    0.90    --   47.28  19.00 -90.00  174
 40  \w     25.00 119.00   0.50    0.90    --   47.28  77.00 -60.00  188
 41  \w     25.00 119.00   0.50    0.90    --   47.28  77.00 120.00  188
 42  \w     25.00 119.00   0.50    0.90    --   47.28  77.00  90.00  188
 43  \w     25.00 119.00   0.50    0.90    --   47.28  77.00  30.00  188
 44  \w     25.00 119.00   0.50    0.90    --   47.28  77.00-180.00  188
 45  \w     25.00 119.00   0.50    0.90    --   47.28  77.00   0.00  188
 46  \w     25.00 119.00   0.50    0.90    --   47.28  77.00 -90.00  188
 47  \w     25.00 119.00   0.50    0.90    --   47.28  77.00-150.00  188
 48  \w   -163.00-102.00   0.50    3.60    --  -91.75 -75.00-141.94  122
 49  \w   -163.00 -73.00   0.50    3.60    --  -91.75 -66.00 -30.55  180
 50  \w   -163.00 -69.00   0.50    3.60    --  -91.75 -76.00  49.21  188
 51  \w   -163.00 -70.00   0.50    3.60    --  -91.75 -74.00-106.87  186
 52  \w   -163.00 -69.00   0.50    3.60    --  -91.75 -77.00-180.00  188
 53  \w   -163.00 -69.00   0.50    3.60    --  -91.75 -77.00 130.81  188
 54  \w   -163.00 -71.00   0.50    3.60    --  -91.75 -71.00  11.90  184
 55  \w   -163.00 -71.00   0.50    3.60    --  -91.75 -72.00 -82.59  184
 56  \w   -163.00 -69.00   0.50    3.60    --  -91.75 -77.00  83.00  188
;
_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      0.1298649000
_diffrn_orient_matrix_UB_12      0.0069699000
_diffrn_orient_matrix_UB_13      -0.0126636000
_diffrn_orient_matrix_UB_21      -0.0371287000
_diffrn_orient_matrix_UB_22      -0.0111901000
_diffrn_orient_matrix_UB_23      -0.1062453000
_diffrn_orient_matrix_UB_31      -0.0242911000
_diffrn_orient_matrix_UB_32      0.0543489000
_diffrn_orient_matrix_UB_33      -0.0202069000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_av_sigmaI/netI    0.0785
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            129827
_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         67.998
_diffrn_reflns_theta_min         3.208
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.539
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.658
_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    1.179
_exptl_crystal_description       needle
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.040
_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     497
_refine_ls_number_reflns         8107
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0330
_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^)+(0.0441P)^2^+2.0830P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0866
_refine_ls_wR_factor_ref         0.0881
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7604
_reflns_number_total             8107
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc01812a2.cif
_cod_data_source_block           FK-494_auto_a
_cod_depositor_comments
'Adding full bibliography for 1574297--1574307.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1574307
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.780
_shelx_estimated_absorpt_t_max   0.941
_cell_oxdiff_length_a            11.42679(10)
_cell_oxdiff_length_b            27.5469(2)
_cell_oxdiff_length_c            14.40147(10)
_cell_oxdiff_angle_alpha         90.0224(6)
_cell_oxdiff_angle_beta          100.7647(7)
_cell_oxdiff_angle_gamma         89.9990(7)
_cell_oxdiff_volume              4453.42(6)
_cell_oxdiff_measurement_reflns_used 66367
_oxdiff_exptl_absorpt_empirical_full_min 0.670
_oxdiff_exptl_absorpt_empirical_full_max 1.859
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_oxdiff_digest_frames
;
01cbb36508aa2f6ac2f37aeac8e77cfe4308538e22d
;
_diffrn_oxdiff_digest_hkl
;
01498c9b30c299acc679647718a92c253f3024
;
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1
_chemical_oxdiff_formula         'C50 H50 N3 O2 Si1 P1 S1 '
_shelx_res_checksum              77364