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_1574302
_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         'C36 H38 N3 O3 P Si'
_chemical_formula_sum            'C36 H38 N3 O3 P Si'
_chemical_formula_weight         619.75
_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             2024-12-12
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2025-03-06 deposited with the CCDC.	2025-03-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.0340(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.78680(10)
_cell_length_b                   18.12460(10)
_cell_length_c                   14.91140(10)
_cell_measurement_reflns_used    14480
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.2880
_cell_measurement_theta_min      3.8290
_cell_volume                     3154.27(4)
_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_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 0.999
_diffrn_measured_fraction_theta_max 0.953
_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    -70.00   5.00   0.50    0.40    --  -47.28  79.00 161.00  150
  2  \w     34.00  94.00   0.50    0.40    --   47.28-125.00 -60.00  120
  3  \w     95.00 177.00   0.50    1.60    --  105.91  30.00  90.00  164
  4  \w     96.00 175.00   0.50    1.60    --  105.91  45.00 120.00  158
  5  \w    115.00 140.00   0.50    1.60    --  105.91  79.00 161.00   50
  6  \w    -21.00  28.00   0.50    0.40    --  -47.28  19.00 -90.00   98
  7  \w      2.00  37.00   0.50    0.40    --   47.28 -79.00  38.00   70
  8  \w     38.00  71.00   0.50    1.60    --  105.91 -61.00 120.00   66
  9  \w     34.00  60.00   0.50    1.60    --  105.91 -61.00  60.00   52
 10  \w     35.00 125.00   0.50    1.60    --  105.91 -79.00  38.00  180
 11  \w     41.00  71.00   0.50    1.60    --  105.91 -61.00-180.00   60
 12  \w     39.00  70.00   0.50    1.60    --  105.91 -61.00 -60.00   62
 13  \w     34.00  74.00   0.50    1.60    --  105.91 -61.00 -30.00   80
 14  \w    -78.00 -52.00   0.50    1.60    --  -91.75  79.00 161.00   52
 15  \w    -46.00 -21.00   0.50    1.60    --  -91.75  45.00  90.00   50
 16  \w    -46.00 -21.00   0.50    1.60    --  -91.75  45.00 -30.00   50
 17  \w    -48.00 -23.00   0.50    1.60    --  -91.75  45.00 -60.00   50
 18  \w    -56.00 -20.00   0.50    1.60    --  -91.75  61.00-150.00   72
 19  \w    -81.00 -34.00   0.50    1.60    --  -91.75 125.00-150.00   94
 20  \w    -99.00 -69.00   0.50    1.60    --  -91.75 -77.00 120.00   60
 21  \w   -137.00-112.00   0.50    1.60    --  -91.75 -77.00 120.00   50
 22  \w   -115.00 -88.00   0.50    0.40    --  -47.28-125.00 120.00   54
 23  \w   -161.00 -80.00   0.50    1.60    --  -91.75 -79.00  38.00  162
 24  \w   -100.00 -74.00   0.50    0.40    --  -47.28-125.00-180.00   52
;
_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      0.1119683000
_diffrn_orient_matrix_UB_12      0.0127086000
_diffrn_orient_matrix_UB_13      0.0648236000
_diffrn_orient_matrix_UB_21      0.0499187000
_diffrn_orient_matrix_UB_22      -0.0715346000
_diffrn_orient_matrix_UB_23      -0.0341725000
_diffrn_orient_matrix_UB_31      0.0488760000
_diffrn_orient_matrix_UB_32      0.0441211000
_diffrn_orient_matrix_UB_33      -0.0742877000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0482
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23088
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.622
_diffrn_reflns_theta_min         3.861
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.464
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62375
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_description       block
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.265
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.086
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         6321
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0341
_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^)+(0.0447P)^2^+1.1031P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0921
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5671
_reflns_number_total             6321
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc01812a2.cif
_cod_data_source_block           LH-821_a
_cod_depositor_comments
'Adding full bibliography for 1574297--1574307.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1574302
_shelx_shelxl_version_number     2019/3
_cell_oxdiff_length_a            11.7884(2)
_cell_oxdiff_length_b            18.1238(3)
_cell_oxdiff_length_c            14.9095(2)
_cell_oxdiff_angle_alpha         89.9330(14)
_cell_oxdiff_angle_beta          98.0204(14)
_cell_oxdiff_angle_gamma         90.0524(14)
_cell_oxdiff_volume              3154.26(9)
_cell_oxdiff_measurement_reflns_used 14480
_oxdiff_exptl_absorpt_empirical_full_min 0.658
_oxdiff_exptl_absorpt_empirical_full_max 1.344
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1
_chemical_oxdiff_formula         'C36 H56 N3 O3 P Si'
_shelx_res_checksum              19165