Structure and reactivity of a triflimide-bridged bis(trimethylsilyl) cation.
Daum, Joshua H.; Bhuvanesh, Nattamai; Ozerov, Oleg V.; Chemical communications (Cambridge, England) 61 (2025) 10816–10818; doi:10.1039/d5cc01223f

data_7134647
_publ_section_title
;
 Structure and reactivity of a triflimide-bridged bis(trimethylsilyl)
 cation.
;
_journal_issue                   58
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10816
_journal_page_last               10818
_journal_paper_doi               10.1039/d5cc01223f
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C H B11 Cl11, C8 H18 F6 N O4 S2 Si2'
_chemical_formula_sum            'C9 H19 B11 Cl11 F6 N O4 S2 Si2'
_chemical_formula_weight         948.41
_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             2024-07-30
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-03-03 deposited with the CCDC.	2025-06-02 downloaded from the CCDC.
;
_cell_angle_alpha                71.799(2)
_cell_angle_beta                 72.239(2)
_cell_angle_gamma                62.887(2)
_cell_formula_units_Z            4
_cell_length_a                   15.9754(3)
_cell_length_b                   16.3642(3)
_cell_length_c                   17.2574(4)
_cell_measurement_reflns_used    39593
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      77.1450
_cell_measurement_theta_min      2.7040
_cell_volume                     3743.54(15)
_computing_cell_refinement       'CrysAlisPro 1.171.43.98a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.128a 64-bit (release 20-06-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.98a (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 2019/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_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  38.00   0.50    0.50    --    0.00 -76.00  77.00  232
  2  \w    -38.00  79.00   0.50    0.50    --    0.00  76.00-155.00  234
  3  \w    -38.00  79.00   0.50    0.50    --    0.00  76.00-155.00  234
  4  \w   -138.00 -22.00   0.50    3.00    --  -59.97 -76.00  77.00  232
  5  \w    -98.00  19.00   0.50    3.00    --  -59.97  76.00-155.00  234
  6  \w     22.00 138.00   0.50    3.00    --   59.97  76.00-155.00  232
  7  \w   -141.00 -25.00   0.50    6.00    -- -103.75  76.00-155.00  232
  8  \w   -177.00 -66.00   0.50    6.00    -- -103.75 -76.00  77.00  222
  9  \w     42.00 158.00   0.50    6.00    --  119.93 -76.00  77.00  232
 10  \w     82.00 178.00   0.50    6.00    --  119.93  76.00-155.00  192
 11  \w    -89.00 -56.00   0.50    0.50    --    0.00-178.00 -60.00   66
 12  \w    -89.00 -56.00   0.50    0.50    --    0.00-178.00  60.00   66
 13  \w    -38.00  16.00   0.50    0.50    --    0.00  77.00 120.00  108
 14  \w    -86.00 -16.00   0.50    3.00    --  -59.97 125.00 -60.00  140
 15  \w   -143.00-106.00   0.50    3.00    --  -59.97 -99.00-180.00   74
 16  \w   -137.00-103.00   0.50    3.00    --  -59.97 -57.00   0.00   68
 17  \w   -139.00-110.00   0.50    3.00    --  -59.97 -77.00-150.00   58
 18  \w   -138.00 -94.00   0.50    3.00    --  -59.97-125.00-120.00   88
 19  \w   -139.00-110.00   0.50    3.00    --  -59.97 -77.00-120.00   58
 20  \w   -137.00-103.00   0.50    3.00    --  -59.97 -57.00-150.00   68
 21  \w    103.00 137.00   0.50    3.00    --   59.97  57.00-120.00   68
 22  \w     34.00 112.00   0.50    3.00    --   59.97-125.00-150.00  156
 23  \w    110.00 139.00   0.50    3.00    --   59.97  77.00  60.00   58
 24  \w    -18.00  98.00   0.50    3.00    --   59.97 -76.00  77.00  232
 25  \w     34.00 112.00   0.50    3.00    --   59.97-125.00 -60.00  156
 26  \w    -28.00  12.00   0.50    3.00    --   59.97 -19.00 -90.00   80
 27  \w    110.00 139.00   0.50    3.00    --   59.97  77.00 -90.00   58
 28  \w   -177.00-106.00   0.50    6.00    -- -103.75 -61.00-150.00  142
 29  \w   -125.00 -53.00   0.50    6.00    -- -103.75 178.00   0.00  144
 30  \w    -49.00 -22.00   0.50    6.00    -- -103.75  45.00-150.00   54
 31  \w    -49.00 -22.00   0.50    6.00    -- -103.75  45.00 -30.00   54
 32  \w    -49.00 -22.00   0.50    6.00    -- -103.75  45.00  60.00   54
 33  \w   -177.00 -69.00   0.50    6.00    -- -103.75 -46.00 132.59  216
 34  \w   -177.00-110.00   0.50    6.00    -- -103.75 -77.00  60.00  134
 35  \w   -125.00 -53.00   0.50    6.00    -- -103.75 178.00-120.00  144
 36  \w    -83.00 -25.00   0.50    6.00    -- -103.75 112.00-150.00  116
 37  \w   -177.00 -69.00   0.50    6.00    -- -103.75 -46.00 132.59  216
 38  \w    -49.00 -22.00   0.50    6.00    -- -103.75  45.00  30.00   54
 39  \w    106.00 178.00   0.50    6.00    --  119.93  61.00 -90.00  144
 40  \w     36.00 105.00   0.50    6.00    --  119.93 -95.00-180.00  138
 41  \w     40.00 108.00   0.50    6.00    --  119.93-112.00  30.00  136
 42  \w     40.00 108.00   0.50    6.00    --  119.93-112.00 -60.00  136
 43  \w     44.00  75.00   0.50    6.00    --  119.93 -61.00  90.00   62
 44  \w    103.00 178.00   0.50    6.00    --  119.93 112.00  90.00  150
 45  \w     63.00 146.00   0.50    6.00    --  119.93 178.00   0.00  166
 46  \w     40.00 108.00   0.50    6.00    --  119.93-112.00   0.00  136
 47  \w     63.00 146.00   0.50    6.00    --  119.93 178.00   0.00  166
 48  \w     36.00 105.00   0.50    6.00    --  119.93 -95.00  30.00  138
 49  \w     35.00 176.00   0.50    6.00    --  119.93  15.00 150.00  282
 50  \w     36.00 105.00   0.50    6.00    --  119.93 -95.00  30.00  138
 51  \w     35.00 176.00   0.50    6.00    --  119.93  15.00 150.00  282
 52  \w     40.00 108.00   0.50    6.00    --  119.93-112.00 120.00  136
 53  \w     40.00 108.00   0.50    6.00    --  119.93-112.00 -90.00  136
 54  \w     40.00 108.00   0.50    6.00    --  119.93-112.00-180.00  136
 55  \w     36.00 105.00   0.50    6.00    --  119.93 -95.00  60.00  138
 56  \w     36.00 105.00   0.50    6.00    --  119.93 -95.00 -60.00  138
 57  \w    110.00 178.00   0.50    6.00    --  119.93  77.00 -30.00  136
 58  \w    103.00 178.00   0.50    6.00    --  119.93 112.00 150.00  150
 59  \w     36.00 105.00   0.50    6.00    --  119.93 -95.00 -60.00  138
 60  \w    -35.00 -10.00   0.50    0.50    --    0.00  77.00-180.00   50
 61  \w    -19.00  16.00   0.50    0.50    --    0.00  77.00  60.00   70
 62  \w    -49.00 -24.00   0.50    0.50    --   10.00 122.00-162.30   50
 63  \w    -23.00   2.00   0.50    0.50    --   22.00  93.00-102.66   50
 64  \w    -16.00  10.00   0.50    0.50    --   26.00  85.00-131.43   52
 65  \w    -20.00   5.00   0.50    3.00    --  -30.00 -72.00-156.18   50
 66  \w    -19.00   6.00   0.50    3.00    --  -30.00 -74.00 -95.88   50
 67  \w     -7.00  18.00   0.50    3.00    --   30.00  74.00 134.45   50
 68  \w     -6.00  19.00   0.50    3.00    --   30.00  71.00 -42.46   50
 69  \w     -6.00  20.00   0.50    3.00    --   30.00  72.00-155.90   52
 70  \w     -1.00  25.00   0.50    3.00    --   34.00  67.00 -59.69   52
 71  \w      0.00  26.00   0.50    3.00    --   34.00  66.00-176.61   52
 72  \w    -33.00  -8.00   0.50    3.00    --  -38.00 -61.00 111.18   50
 73  \w    -31.00  -6.00   0.50    3.00    --  -38.00 -62.00 -44.50   50
 74  \w    -37.00 -12.00   0.50    3.00    --  -42.00 -58.00-120.85   50
 75  \w    -37.00 -12.00   0.50    3.00    --  -42.00 -58.00 -72.17   50
 76  \w    -42.00 -17.00   0.50    3.00    --  -46.00 -55.00  80.24   50
 77  \w    -44.00 -18.00   0.50    3.00    --  -46.00 -54.00 -94.56   52
 78  \w    -48.00 -22.00   0.50    3.00    --  -46.00 -51.00 -56.97   52
 79  \w    -43.00 -17.00   0.50    3.00    --  -46.00 -54.00 -25.18   52
 80  \w    -42.00 -17.00   0.50    3.00    --  -46.00 -55.00-126.11   50
 81  \w    -42.00 -16.00   0.50    3.00    --  -46.00 -55.00-175.63   52
 82  \w    -80.00 -33.00   0.50    3.00    --  -66.00 -46.00-144.42   94
 83  \w   -149.00-103.00   0.50    3.00    --  -70.00 -46.00  94.46   92
 84  \w    -86.00 -36.00   0.50    3.00    --  -70.00 -46.00  94.46  100
 85  \w    -68.00 -43.00   0.50    3.00    --  -78.00 -47.00-118.90   50
 86  \w   -118.00 -93.00   0.50    3.00    --  -78.00 -47.00-118.90   50
 87  \w   -147.00-121.00   0.50    3.00    --  -78.00 -47.00   0.19   52
 88  \w    -78.00 -43.00   0.50    3.00    --  -78.00 -47.00   0.19   70
 89  \w   -153.00-127.00   0.50    3.00    --  -78.00 -47.00 -58.86   52
 90  \w    -70.00 -44.00   0.50    3.00    --  -78.00 -47.00 161.71   52
 91  \w    -68.00 -43.00   0.50    3.00    --  -78.00 -47.00 -58.86   50
 92  \w    -75.00 -49.00   0.50    3.00    --  -82.00 -47.00 133.92   52
 93  \w   -128.00-101.00   0.50    3.00    --  -82.00 -47.00 133.92   54
 94  \w    -74.00 -47.00   0.50    3.00    --  -82.00 -47.00 -66.92   54
 95  \w    -74.00 -48.00   0.50    3.00    --  -82.00 -47.00  55.68   52
 96  \w    -77.00 -51.00   0.50    3.00    --  -86.00 -47.00 -94.83   52
 97  \w    -88.00 -51.00   0.50    3.00    --  -86.00 -47.00-144.59   74
 98  \w    -93.00 -51.00   0.50    3.00    --  -86.00 -47.00 -82.40   84
 99  \w    -88.00 -51.00   0.50    3.00    --  -86.00 -47.00 155.16   74
100  \w   -160.00-134.00   0.50    3.00    --  -86.00 -47.00 -82.40   52
101  \w    -77.00 -51.00   0.50    3.00    --  -86.00 -47.00 -10.14   52
102  \w    -91.00 -52.00   0.50    3.00    --  -86.00 -47.00 -21.57   78
103  \w    -78.00 -52.00   0.50    3.00    --  -86.00 -47.00 -39.77   52
104  \w    -76.00 -51.00   0.50    3.00    --  -86.00 -47.00  28.36   50
105  \w    -77.00 -51.00   0.50    3.00    --  -86.00 -47.00-165.09   52
106  \w    -86.00 -51.00   0.50    3.00    --  -86.00 -47.00  79.30   70
107  \w   -165.00-139.00   0.50    3.00    --  -86.00 -47.00  79.30   52
108  \w    -84.00 -59.00   0.50    6.00    --  -94.00 -46.00 107.15   50
109  \w    -92.00 -67.00   0.50    6.00    -- -102.00 -46.00-101.82   50
110  \w   -139.00-104.00   0.50    6.00    -- -103.75 -45.00-120.00   70
111  \w    -94.00 -69.00   0.50    6.00    -- -103.75 -45.00 -91.43   50
112  \w   -108.00 -72.00   0.50    6.00    -- -103.75 -45.00   0.00   72
113  \w    -95.00 -69.00   0.50    6.00    -- -103.75 -45.00  90.00   52
114  \w    -96.00 -70.00   0.50    6.00    -- -103.75 -46.00 -68.04   52
115  \w   -175.00-146.00   0.50    6.00    -- -103.75 -45.00   0.00   58
116  \w    -95.00 -69.00   0.50    6.00    -- -103.75 -45.00 161.47   52
117  \w   -172.00-135.00   0.50    6.00    -- -103.75 -46.00 -21.14   74
118  \w    -98.00 -69.00   0.50    6.00    -- -103.75 -46.00 -21.14   58
119  \w   -101.00 -69.00   0.50    6.00    -- -103.75 -45.00  60.00   64
120  \w   -177.00-151.00   0.50    6.00    -- -103.75 -45.00  90.00   52
121  \w   -175.00-150.00   0.50    6.00    -- -103.75 -46.00 -68.04   50
122  \w    -95.00 -69.00   0.50    6.00    -- -103.75 -46.00 143.82   52
123  \w   -111.00 -69.00   0.50    6.00    -- -103.75 -46.00 -61.00   84
124  \w    -99.00 -70.00   0.50    6.00    -- -103.75 -45.00  14.09   58
125  \w    -95.00 -69.00   0.50    6.00    -- -103.75 -46.00  76.51   52
126  \w   -113.00 -69.00   0.50    6.00    -- -103.75 -45.00-170.31   88
127  \w   -154.00-122.00   0.50    6.00    -- -103.75 -45.00-170.31   64
128  \w   -109.00 -69.00   0.50    6.00    -- -103.75 -46.00 113.42   80
129  \w   -129.00 -69.00   0.50    6.00    -- -103.75 -45.00-133.47  120
130  \w   -102.00 -69.00   0.50    6.00    -- -103.75 -46.00 -38.41   66
131  \w   -174.00-146.00   0.50    6.00    -- -103.75 -46.00 -38.41   56
132  \w    -94.00 -90.00   0.50    6.00    -- -103.75 -45.00-120.00    8
;
_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      -0.0707292000
_diffrn_orient_matrix_UB_12      -0.0409059000
_diffrn_orient_matrix_UB_13      0.0619620000
_diffrn_orient_matrix_UB_21      0.0345247000
_diffrn_orient_matrix_UB_22      -0.0761810000
_diffrn_orient_matrix_UB_23      -0.0504144000
_diffrn_orient_matrix_UB_31      0.0774210000
_diffrn_orient_matrix_UB_32      -0.0647881000
_diffrn_orient_matrix_UB_33      0.0528133000
_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  0.0840
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            69970
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.070
_diffrn_reflns_theta_min         2.747
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           '1 mA'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_source_voltage           '50 kV'
_exptl_absorpt_coefficient_mu    9.635
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.387
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.98a (Rigaku Oxford Diffraction, 2023) 
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_colour_primary    colourless
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.328
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.082
_refine_diff_density_max         0.934
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     887
_refine_ls_number_reflns         14161
_refine_ls_number_restraints     197
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0669
_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^)+(0.1001P)^2^+11.9708P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1810
_refine_ls_wR_factor_ref         0.1866
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12263
_reflns_number_total             14161
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc01223f2.cif
_cod_data_source_block           oo_oz680
_cod_depositor_comments          'Adding full bibliography for 7134647.cif.'
_cod_database_code               7134647
_shelx_shelxl_version_number     2019/1
_chemical_oxdiff_formula         C12H20F6O4Si2Cl11B11S
_shelx_estimated_absorpt_t_max   0.505
_shelx_estimated_absorpt_t_min   0.144
_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. Restrained distances
 S2Q-C5P \\sim S2P-C5P
 with sigma of 0.02
 S2P-O4P \\sim S2Q-O4P
 with sigma of 0.02
 S2A-O4A \\sim S2-O4
 with sigma of 0.01
 Si2-O4A \\sim Si2-O4
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O3 \\sim S2 \\sim O4 \\sim C5 \\sim S2A \\sim O3A \\sim O4A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
S2Q \\sim O4P \\sim S2P \\sim O3P \\sim C5P \\sim O3Q \\sim N1P: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 O3, S2, O4, C5, S2A, O3A, O4A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 S2Q, O4P, S2P, O3P, C5P, O3Q, N1P
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Sof(S2A)=Sof(O3A)=Sof(S2Q)=Sof(O3Q)=Sof(O4A)=1-FVAR(1)
 Sof(S2)=Sof(O3)=Sof(O4)=Sof(S2P)=Sof(O3P)=FVAR(1)
6.a Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C1P(H1PA,H1PB,H1PC), C2P(H2PA,H2PB,H2PC), C3P(H3PA,
 H3PB,H3PC), C6P(H6PA,H6PB,H6PC), C7P(H7PA,H7PB,H7PC), C8P(H8PA,H8PB,H8PC)
6.b Boron cage BH refined with riding coordinates:
 C1C(H1CA), C1D(H1D)
;
_shelx_res_checksum              57564
_shelx_hkl_checksum              32977
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder'
_olex2_submission_original_sample_id OOB_JD_240729_SDc_OZ680_fluo2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   33205
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.397
_oxdiff_exptl_absorpt_empirical_full_min 0.365