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_1574304
_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         'C48 H48 N5 P Si'
_chemical_formula_sum            'C48 H48 N5 P Si'
_chemical_formula_weight         753.97
_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             2023-06-06
_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                 105.3050(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.4704(2)
_cell_length_b                   8.81830(10)
_cell_length_c                   23.8065(2)
_cell_measurement_reflns_used    21214
_cell_measurement_temperature    109(2)
_cell_measurement_theta_max      76.5600
_cell_measurement_theta_min      2.6030
_cell_volume                     4145.00(7)
_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      109(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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     48.00  73.00   0.50    0.22    --   47.28  73.00 -62.00   50
  2  \w    138.00 164.00   0.50    0.88    --  105.91  73.00 -62.00   52
  3  \w     85.00 110.00   0.50    0.88    --  105.91  73.00 -62.00   50
  4  \w     96.00 176.00   0.50    0.88    --  105.91  30.00 -90.00  160
  5  \w     97.00 176.00   0.50    0.88    --  105.91  15.00-120.00  158
  6  \w     35.00 108.00   0.50    0.88    --  105.91-125.00-180.00  146
  7  \w     39.00  64.00   0.50    0.88    --  105.91-125.00  90.00   50
  8  \w     82.00 108.00   0.50    0.88    --  105.91-125.00  90.00   52
  9  \w     33.00  95.00   0.50    0.88    --  105.91 -73.00 168.00  124
 10  \w     -7.00  26.00   0.50    0.22    --   47.28 -73.00 168.00   66
 11  \w     29.00  56.00   0.50    0.22    --   47.28 -73.00 168.00   54
 12  \w     33.00  71.00   0.50    0.88    --  105.91 -61.00  90.00   76
 13  \w     45.00  70.00   0.50    0.88    --  105.91 -61.00 -60.00   50
 14  \w     33.00  73.00   0.50    0.88    --  105.91 -61.00-150.00   80
 15  \w    -68.00  22.00   0.50    0.22    --  -47.28  73.00 -62.00  180
 16  \w    -79.00 -19.00   0.50    0.88    --  -91.75  73.00 -62.00  120
 17  \w    -48.00 -23.00   0.50    0.88    --  -91.75  45.00  60.00   50
 18  \w    -54.00 -20.00   0.50    0.88    --  -91.75  61.00  90.00   68
 19  \w    -45.00 -20.00   0.50    0.88    --  -91.75  45.00 150.00   50
 20  \w    -47.00 -21.00   0.50    0.88    --  -91.75  45.00 120.00   52
 21  \w    -48.00 -22.00   0.50    0.88    --  -91.75  45.00  90.00   52
 22  \w    -48.00 -21.00   0.50    0.88    --  -91.75  45.00 -90.00   54
 23  \w    -78.00 -53.00   0.50    0.88    --  -91.75 125.00-180.00   50
 24  \w   -117.00 -74.00   0.50    0.22    --  -47.28-125.00 -60.00   86
 25  \w   -103.00 -76.00   0.50    0.22    --  -47.28-125.00  60.00   54
 26  \w   -149.00 -93.00   0.50    0.88    --  -91.75 -73.00 168.00  112
 27  \w   -106.00 -26.00   0.50    0.22    --  -47.28 -73.00 168.00  160
;
_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      -0.0365238000
_diffrn_orient_matrix_UB_12      -0.0848738000
_diffrn_orient_matrix_UB_13      0.0394449000
_diffrn_orient_matrix_UB_21      -0.0289933000
_diffrn_orient_matrix_UB_22      -0.1135681000
_diffrn_orient_matrix_UB_23      -0.0495042000
_diffrn_orient_matrix_UB_31      0.0625227000
_diffrn_orient_matrix_UB_32      -0.1022696000
_diffrn_orient_matrix_UB_33      0.0221878000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0591
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            31602
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.994
_diffrn_reflns_theta_min         3.315
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.164
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.467
_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    1.208
_exptl_crystal_description       block
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         7555
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0402P)^2^+1.7931P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0904
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6812
_reflns_number_total             7555
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc01812a2.cif
_cod_data_source_block           LH-477_a
_cod_depositor_comments
'Adding full bibliography for 1574297--1574307.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1574304
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.714
_shelx_estimated_absorpt_t_max   0.913
_cell_oxdiff_length_a            20.4786(4)
_cell_oxdiff_length_b            8.81252(17)
_cell_oxdiff_length_c            23.8139(5)
_cell_oxdiff_angle_alpha         90.0266(16)
_cell_oxdiff_angle_beta          105.3157(17)
_cell_oxdiff_angle_gamma         89.9866(16)
_cell_oxdiff_volume              4145.02(14)
_cell_oxdiff_measurement_reflns_used 21216
_oxdiff_exptl_absorpt_empirical_full_min 0.533
_oxdiff_exptl_absorpt_empirical_full_max 1.528
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_oxdiff_digest_frames
;
01f3d3498ade47fff4e79fe96b025ac35c022566050
;
_diffrn_oxdiff_digest_hkl
;
01a94a2977d6cb598f931777d1e32b749da0fc
;
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1
_chemical_oxdiff_formula         'C48 H50 N5 P Si'
_shelx_res_checksum              39804