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_1574306
_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         'C54 H73 N4 O2 P S Si, C7 H8'
_chemical_formula_sum            'C61 H81 N4 O2 P S Si'
_chemical_formula_weight         993.41
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-06-07
_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                76.2790(10)
_cell_angle_beta                 89.3570(10)
_cell_angle_gamma                87.9160(10)
_cell_formula_units_Z            2
_cell_length_a                   9.95910(10)
_cell_length_b                   12.80600(10)
_cell_length_c                   22.0685(3)
_cell_measurement_reflns_used    16257
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      76.6460
_cell_measurement_theta_min      3.6390
_cell_volume                     2732.39(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      105(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_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    -78.00  20.00   0.50    3.50    --  -47.03  99.00  -2.00  196
  2  \w     27.00  54.00   0.50    3.50    --   47.03 -99.00-108.00   54
  3  \w   -128.00-102.00   0.50   14.00    --  -91.75 -99.00-108.00   52
  4  \w    -59.00 -31.00   0.50   14.00    --  -91.75  99.00  -2.00   56
  5  \w     66.00  92.00   0.50   14.00    --  105.91 -99.00-108.00   52
  6  \w    110.00 166.00   0.50   14.00    --  105.91  99.00  -2.00  112
  7  \w   -119.00 -77.00   0.50    3.50    --  -47.03-125.00  60.00   84
  8  \w    -60.00  25.00   0.50    3.50    --  -47.03  57.00 -30.00  170
  9  \w    -35.00  25.00   0.50    3.50    --  -47.03  38.00 -90.00  120
 10  \w   -108.00 -81.00   0.50    3.50    --  -47.03-125.00-120.00   54
 11  \w   -118.00 -84.00   0.50    3.50    --  -47.03-125.00   0.00   68
 12  \w    -15.00  27.00   0.50    3.50    --  -47.03  19.00-120.00   84
 13  \w   -159.00-108.00   0.50   14.00    --  -91.75 -30.00  90.00  102
 14  \w   -117.00 -91.00   0.50   14.00    --  -91.75 -77.00 120.00   52
 15  \w    -48.00 -22.00   0.50   14.00    --  -91.75  45.00   0.00   52
 16  \w    -48.00 -21.00   0.50   14.00    --  -91.75  45.00-150.00   54
 17  \w    -51.00 -19.00   0.50   14.00    --  -91.75  61.00-150.00   64
 18  \w   -101.00 -76.00   0.50   14.00    --  -91.75 -61.00 -30.00   50
 19  \w    -48.00 -20.00   0.50   14.00    --  -91.75  45.00  90.00   56
 20  \w    -47.00 -21.00   0.50   14.00    --  -91.75  45.00 -90.00   52
 21  \w   -162.00 -69.00   0.50   14.00    --  -91.75 -77.00-150.00  186
 22  \w    -46.00 -20.00   0.50   14.00    --  -91.75  45.00-180.00   52
 23  \w    -46.00 -21.00   0.50   14.00    --  -91.75  45.00  30.00   50
 24  \w     33.00  95.50   0.50   14.00    --  105.91 -94.00-180.00  125
 25  \w     61.00  97.00   0.50   14.00    --  105.91 -94.00-150.00   72
 26  \w     78.00 104.00   0.50   14.00    --  105.91 -94.00 -30.00   52
 27  \w     33.00  59.00   0.50   14.00    --  105.91 -94.00 -30.00   52
 28  \w     77.00  99.00   0.50   14.00    --  105.91 -94.00  30.00   44
 29  \w     81.00 100.50   0.50   14.00    --  105.91-125.00-180.00   39
 30  \w     41.00  72.00   0.50   14.00    --  105.91 -94.00  30.00   62
 31  \w     38.00  69.00   0.50   14.00    --  105.91-125.00-180.00   62
 32  \w     96.00 178.00   0.50   14.00    --  105.91  30.00  30.00  164
 33  \w     95.00 178.00   0.50   14.00    --  105.91  30.00 -60.00  166
 34  \w     33.00  58.00   0.50   14.00    --  105.91 -61.00 150.00   50
 35  \w     33.00 106.00   0.50   14.00    --  105.91-107.00 -66.67  146
 36  \w     99.00 177.00   0.50   14.00    --  105.91  45.00 -90.00  156
 37  \w     34.00  97.00   0.50   14.00    --  105.91 -94.00  60.00  126
 38  \w     66.00  93.50   0.50   14.00    --  105.91 -94.00 120.00   55
 39  \w     47.00 105.00   0.50   14.00    --  105.91 -94.00 -60.00  116
 40  \w     37.00 101.50   0.50   14.00    --  105.91 -77.00  60.00  129
;
_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      0.1036677000
_diffrn_orient_matrix_UB_12      0.0432387000
_diffrn_orient_matrix_UB_13      0.0383744000
_diffrn_orient_matrix_UB_21      0.0971951000
_diffrn_orient_matrix_UB_22      0.0193363000
_diffrn_orient_matrix_UB_23      -0.0560452000
_diffrn_orient_matrix_UB_31      -0.0613747000
_diffrn_orient_matrix_UB_32      0.1144980000
_diffrn_orient_matrix_UB_33      -0.0234537000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            32168
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.999
_diffrn_reflns_theta_min         3.555
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.366
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.915
_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    1.207
_exptl_crystal_description       block
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         9892
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0345
_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^)+(0.0434P)^2^+1.1491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0913
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8612
_reflns_number_total             9892
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc01812a2.cif
_cod_data_source_block           LH-478_a
_cod_depositor_comments
'Adding full bibliography for 1574297--1574307.cif.'
_cod_database_code               1574306
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.923
_shelx_estimated_absorpt_t_max   0.947
_cell_oxdiff_length_a            9.95905(12)
_cell_oxdiff_length_b            12.80602(13)
_cell_oxdiff_length_c            22.0685(2)
_cell_oxdiff_angle_alpha         76.2791(9)
_cell_oxdiff_angle_beta          89.3575(9)
_cell_oxdiff_angle_gamma         87.9162(9)
_cell_oxdiff_volume              2732.39(5)
_cell_oxdiff_measurement_reflns_used 16257
_oxdiff_exptl_absorpt_empirical_full_min 0.761
_oxdiff_exptl_absorpt_empirical_full_max 1.674
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_oxdiff_digest_frames
;
01903019875edf7a84ac1050f3413e0daf0356635fe
;
_diffrn_oxdiff_digest_hkl
;
01fff5690cb2a1dfc6fbde38a7a51f276870ea
;
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1
_chemical_oxdiff_formula         'C54 H55 N4 P S O2 Si'
_shelx_res_checksum              83461