Reversible CO<sub>2</sub> insertion into the silicon-nitrogen σ-bond of an N-heterocyclic iminosilane.
Wang, Jingyan; Hwang, Gi Byoung; Knapp, Caroline E.; Wilson, Daniel W. N.; Chemical communications (Cambridge, England) 60 (2024) 13051–13054; doi:10.1039/d4cc04798b

data_7133877
_publ_section_title
;
 Reversible CO<sub>2</sub> insertion into the silicon-nitrogen
 &#x3c3;-bond of an N-heterocyclic iminosilane.
;
_journal_issue                   89
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              13051
_journal_page_last               13054
_journal_paper_doi               10.1039/d4cc04798b
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C31 H45 N3 O2 Si'
_chemical_formula_sum            'C31 H45 N3 O2 Si'
_chemical_formula_weight         519.79
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-09-16
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-09-16 deposited with the CCDC.	2024-10-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   27.23555(7)
_cell_length_b                   27.23555(7)
_cell_length_c                   17.39351(8)
_cell_measurement_reflns_used    93152
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      77.2740
_cell_measurement_theta_min      4.4160
_cell_volume                     12902.07(8)
_computing_cell_refinement       'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.95a 64-bit (release 03-11-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip  (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_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     -9.00  17.00   0.50    1.00    --   49.61 -97.00 -87.00   52
  2  \w     46.00 102.00   0.50    1.00    --  102.44 -97.00 -87.00  112
  3  \w    125.00 153.00   0.50    1.00    --  102.44  97.00  19.00   56
  4  \w    -42.00 -15.00   0.50    1.00    --    6.00 124.00  -9.10   54
  5  \w    -38.00 -13.00   0.50    1.00    --   10.00 122.00 -79.90   50
  6  \w    -28.00  -2.00   0.50    1.00    --   14.00 114.00-134.55   52
  7  \w    -23.00   3.00   0.50    1.00    --   14.00 107.00  55.36   52
  8  \w     -8.00  22.00   0.50    1.00    --   22.00  99.00-170.45   60
  9  \w      6.00  31.00   0.50    1.00    --   38.00  95.00 122.49   50
 10  \w     11.00  38.00   0.50    1.00    --   42.00  92.00 -94.24   54
 11  \w     17.00  45.00   0.50    1.00    --   46.00  89.00  30.75   56
 12  \w     20.00  46.00   0.50    1.00    --   46.00  88.00  82.73   52
 13  \w     29.00  80.00   0.50    1.00    --   49.61 -99.00 -60.00  102
 14  \w    -20.00  58.00   0.50    1.00    --   49.61 -38.00-150.00  156
 15  \w     39.00  80.00   0.50    1.00    --   49.61 -97.00 -87.00   82
 16  \w     29.00  62.00   0.50    1.00    --   54.00  83.00 -81.01   66
 17  \w     77.00 103.00   0.50    1.00    --   54.00  83.00 -81.01   52
 18  \w     31.00  60.00   0.50    1.00    --   54.00  82.00 165.89   58
 19  \w     70.00  98.00   0.50    1.00    --   54.00  25.00-135.42   56
 20  \w     29.00  57.00   0.50    1.00    --   54.00  83.00-143.43   56
 21  \w     33.00  60.00   0.50    1.00    --   54.00  25.00-135.42   54
 22  \w     69.00 109.00   0.50    1.00    --   54.00  83.00-143.43   80
 23  \w     33.00  63.00   0.50    1.00    --   58.00  82.00 -33.46   60
 24  \w     34.00  61.00   0.50    1.00    --   58.00  81.00 104.02   54
 25  \w     75.00 110.00   0.50    1.00    --   58.00  82.00 -33.46   70
 26  \w     37.00  80.00   0.50    1.00    --   62.00  82.00 138.81   86
 27  \w     38.00  66.00   0.50    1.00    --   62.00  81.00  58.27   56
 28  \w     42.00  85.00   0.50    1.00    --   66.00  82.00-147.26   86
 29  \w     43.00  68.00   0.50    1.00    --   66.00  79.00 172.68   50
 30  \w     41.00  67.00   0.50    1.00    --   66.00  83.00 -74.40   52
 31  \w     91.00 124.00   0.50    1.00    --   66.00  83.00   6.00   66
 32  \w     41.00  66.00   0.50    1.00    --   66.00  83.00   6.00   50
 33  \w     48.00  74.00   0.50    1.00    --   70.00  82.00 101.33   52
 34  \w     85.00 128.00   0.50    1.00    --   70.00  83.00-116.11   86
 35  \w     45.00  80.00   0.50    1.00    --   70.00  83.00-116.11   70
 36  \w     77.00 130.00   0.50    1.00    --   70.00  83.00  78.60  106
 37  \w     47.00  73.00   0.50    1.00    --   70.00  80.00 176.81   52
 38  \w     45.00  70.00   0.50    1.00    --   70.00  83.00  18.30   50
 39  \w     45.00  71.00   0.50    1.00    --   70.00  83.00  78.60   52
 40  \w    106.00 131.00   0.50    1.00    --   70.00  83.00 -26.68   50
 41  \w     45.00  74.00   0.50    1.00    --   70.00  83.00 -26.68   58
 42  \w    108.00 138.00   0.50    1.00    --   74.00  77.00 123.15   60
 43  \w     52.00  84.00   0.50    1.00    --   74.00  77.00 123.15   64
 44  \w    112.00 137.00   0.50    1.00    --   74.00  75.00 -37.24   50
 45  \w     53.00  78.00   0.50    1.00    --   74.00  75.00 -37.24   50
 46  \w    103.00 137.00   0.50    1.00    --   74.00  76.00 -79.84   68
 47  \w     99.00 132.00   0.50    1.00    --   74.00  83.00  25.22   66
 48  \w    104.00 134.00   0.50    1.00    --   74.00  76.00 177.05   60
 49  \w     51.00  82.00   0.50    1.00    --   74.00  83.00  25.22   62
 50  \w     55.00  95.00   0.50    1.00    --   74.00  76.00 -79.84   80
 51  \w     53.00  97.00   0.50    1.00    --   74.00  76.00 177.05   88
 52  \w     32.00 117.00   0.50    1.00    --   90.00 -85.00  10.03  170
 53  \w     81.00 111.00   0.50    1.00    --  102.44  77.00 150.00   60
 54  \w     90.00 117.00   0.50    1.00    --  102.44-125.00-150.00   54
 55  \w     41.00  67.00   0.50    1.00    --  102.44-125.00-150.00   52
 56  \w     81.00 145.00   0.50    1.00    --  102.44  77.00 -90.00  128
 57  \w     46.00 100.00   0.50    1.00    --  102.44 -77.00  60.00  108
 58  \w     81.00 136.00   0.50    1.00    --  102.44  77.00  30.00  110
 59  \w     82.00 162.00   0.50    1.00    --  102.44  77.00  60.00  160
 60  \w     50.00 101.00   0.50    1.00    --  102.44-125.00 -90.00  102
 61  \w     81.00 159.00   0.50    1.00    --  102.44  77.00 120.00  156
 62  \w     81.00 160.00   0.50    1.00    --  102.44  77.00 -60.00  158
 63  \w     81.00 163.00   0.50    1.00    --  102.44  77.00-180.00  164
 64  \w     81.00 163.00   0.50    1.00    --  102.44  77.00 -30.00  164
 65  \w     81.00 166.00   0.50    1.00    --  102.44  77.00  90.00  170
 66  \w     81.00 148.00   0.50    1.00    --  102.44  77.00-120.00  134
 67  \w     81.00 159.00   0.50    1.00    --  102.44  77.00   0.00  156
 68  \w     81.00 166.00   0.50    1.00    --  102.44  77.00-150.00  170
 69  \w     59.00 106.00   0.50    1.00    --  102.44 -99.00 120.00   94
 70  \w    115.00 163.00   0.50    1.00    --  102.44  77.00 150.00   96
 71  \w     44.00  88.00   0.50    1.00    --  107.58-120.00-155.85   88
 72  \w     48.00 108.00   0.50    1.00    --  107.58 -96.00 -27.59  120
 73  \w     72.00 113.00   0.50    1.00    --  107.58 -40.00 -52.81   82
 74  \w     34.00  59.00   0.50    1.00    --  107.58 -40.00 -52.81   50
 75  \w     34.00 116.00   0.50    1.00    --  107.58 -36.00  56.16  164
 76  \w     49.00 110.00   0.50    1.00    --  107.58-106.00-144.12  122
 77  \w     55.00 113.00   0.50    1.00    --  107.58 -41.00-139.76  116
 78  \w     35.00 106.00   0.50    1.00    --  107.58 -47.00 160.89  142
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, HyPix-Arc 100'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0438893000
_diffrn_orient_matrix_UB_12      -0.0288492000
_diffrn_orient_matrix_UB_13      0.0329289000
_diffrn_orient_matrix_UB_21      0.0297786000
_diffrn_orient_matrix_UB_22      -0.0479431000
_diffrn_orient_matrix_UB_23      -0.0056417000
_diffrn_orient_matrix_UB_31      0.0196671000
_diffrn_orient_matrix_UB_32      0.0082712000
_diffrn_orient_matrix_UB_33      0.0820288000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0110
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            151242
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.164
_diffrn_reflns_theta_min         4.432
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.857
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.95a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.070
_exptl_crystal_description       block
_exptl_crystal_F_000             4512
_exptl_crystal_size_max          0.319
_exptl_crystal_size_mid          0.204
_exptl_crystal_size_min          0.169
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         6825
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0566P)^2^+8.0527P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1150
_refine_ls_wR_factor_ref         0.1176
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6168
_reflns_number_total             6825
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc04798b2.cif
_cod_data_source_block           xstr1658_autored
_cod_depositor_comments          'Adding full bibliography for 7133877.cif.'
_cod_original_cell_volume        12902.07(9)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7133877
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H20 N2 O2 Si1 '
_shelx_estimated_absorpt_t_max   0.869
_shelx_estimated_absorpt_t_min   0.772
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C19(H19), C21(H21), C30(H30), C14(H14)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C10(H10), C26(H26), C12(H12), C11(H11), C28(H28), C27(H27)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C6(H6A,H6B,H6C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C),
 C5(H5A,H5B,H5C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C32(H32A,H32B,H32C),
  C17(H17A,H17B,H17C), C159(H15A,H15B,H15C), C31(H31A,H31B,H31C)
;
_shelx_res_checksum              4022
_shelx_hkl_checksum              37297
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.257
_oxdiff_exptl_absorpt_empirical_full_min 0.801