Synthesis and reactivity of a parent phosphathioethynolato-borane and a boraarsaketene
Jürgensen, Malte; Kunz, Tanja; Arrowsmith, Merle; Dietz, Maximilian; Hagspiel, Stephan; Braunschweig, Holger; Chemical Science 16 (2025) 8870–8877; doi:10.1039/D5SC01996F

data_1574409
_publ_section_title
;
 Synthesis and reactivity of a parent phosphathioethynolato-borane and a
 boraarsaketene
;
_journal_issue                   20
_journal_name_full               'Chemical Science'
_journal_page_first              8870
_journal_page_last               8877
_journal_paper_doi               10.1039/D5SC01996F
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C22 H28 B F3 N2 O3 S, 1.5(C6 H6)'
_chemical_formula_sum            'C31 H37 B F3 N2 O3 S'
_chemical_formula_weight         585.49
_chemical_name_common            (SIMes)BH2OTf
_chemical_name_systematic        1-SIMes
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_audit_creation_method           'CIF-fill 1.2x (K.Radacki, 2005-21)'
_audit_update_record
;
2025-03-03 deposited with the CCDC.	2025-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.5500(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5510(2)
_cell_length_b                   8.99420(10)
_cell_length_c                   20.2775(2)
_cell_measurement_reflns_used    23067
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.5470
_cell_measurement_theta_min      2.1780
_cell_volume                     3012.78(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'BIS 2011.8 / APEX2 ver. 2014.9 (Bruker AXS)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(12)
_diffrn_detector                 HPA
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HyPix Arc150'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -35.00  -9.00   0.50    0.50    --  -10.00 119.00 129.65   52
   2  \w     26.00  60.00   0.50    0.50    --   14.00  59.00 154.53   68
   3  \w     34.00  60.00   0.50    0.50    --   22.00  58.00 168.36   52
   4  \w     34.00  60.00   0.50    0.50    --   22.00  57.00 121.77   52
   5  \w     43.00  78.00   0.50    0.50    --   30.00  52.00 177.47   70
   6  \w     44.00  79.00   0.50    0.50    --   30.00  51.00-150.95   70
   7  \w     48.00  83.00   0.50    0.50    --   34.00  51.00 160.50   70
   8  \w    -90.00 -55.00   0.50    0.50    --  -42.00 -51.00 154.26   70
   9  \w    -90.00 -55.00   0.50    0.50    --  -42.00 -52.00-169.27   70
  10  \w     55.00  90.00   0.50    0.50    --   42.00  52.00 138.41   70
  11  \w     56.00  91.00   0.50    0.50    --   42.00  51.00 144.14   70
  12  \w    -98.00 -63.00   0.50    0.50    --  -50.00 -52.00 121.51   70
  13  \w   -102.00 -67.00   0.50    0.50    --  -54.00 -51.00 173.28   70
  14  \w   -102.00 -67.00   0.50    0.50    --  -54.00 -52.00 108.45   70
  15  \w   -103.00 -68.00   0.50    0.50    --  -54.00 -47.00  84.82   70
  16  \w   -106.00 -71.00   0.50    0.50    --  -58.00 -51.00  69.20   70
  17  \w   -107.00 -72.00   0.50    0.50    --  -58.00 -48.00  76.55   70
  18  \w   -110.00 -75.00   0.50    0.50    --  -62.00 -51.00 137.55   70
  19  \w   -110.00 -75.00   0.50    0.50    --  -62.00 -52.00 149.24   70
  20  \w   -110.00 -75.00   0.50    0.50    --  -62.00 -52.00  97.54   70
  21  \w   -114.00 -79.00   0.50    0.50    --  -66.00 -52.00 -28.56   70
  22  \w   -118.00 -83.00   0.50    0.50    --  -70.00 -54.00-161.70   70
  23  \w   -121.00 -86.00   0.50    1.00    --  -74.00 -58.00-177.17   70
  24  \w    -96.00 -28.00   0.50    1.00    --  -76.33 112.00-150.00  136
  25  \w   -124.00 -89.00   0.50    1.00    --  -78.00 -61.00 137.22   70
  26  \w   -128.00 -95.00   0.50    1.00    --  -79.50-117.00 164.55   66
  27  \w   -128.00 -93.00   0.50    1.00    --  -79.50 -50.00  53.10   70
  28  \w   -126.00 -91.00   0.50    1.00    --  -79.50 -59.00  15.10   70
  29  \w   -124.00 -95.00   0.50    1.00    --  -79.50 -65.00 179.53   58
  30  \w   -125.00 -91.00   0.50    1.00    --  -79.50 -60.00  91.29   68
  31  \w   -125.00 -90.00   0.50    1.00    --  -79.50 -62.00 112.48   70
  32  \w   -125.00 -91.00   0.50    1.00    --  -79.50 -61.00 125.52   68
  33  \w   -125.00 -90.00   0.50    1.00    --  -79.50 -62.00 162.59   70
  34  \w   -128.00 -93.00   0.50    1.00    --  -79.50 -52.00 142.97   70
  35  \w   -125.00 -91.00   0.50    1.00    --  -79.50 -60.00 -31.41   68
  36  \w   -126.00 -91.00   0.50    1.00    --  -79.50 -59.00 100.52   70
  37  \w   -125.00 -90.00   0.50    1.00    --  -79.50 -62.00 179.50   70
  38  \w   -128.00 -97.00   0.50    1.00    --  -79.50-114.00 176.29   62
  39  \w   -125.00 -91.00   0.50    1.00    --  -79.50 -60.00 -22.16   68
  40  \w   -125.00 -91.00   0.50    1.00    --  -79.50 -60.00  96.85   68
  41  \w   -128.00 -97.00   0.50    1.00    --  -79.50-113.00  92.75   62
  42  \w   -128.00 -97.00   0.50    1.00    --  -79.50-113.00  45.96   62
  43  \w   -102.00 -31.00   0.50    1.00    --  -79.50 126.00 117.57  142
  44  \w   -124.00 -91.00   0.50    1.00    --  -79.50 -61.00-154.28   66
  45  \w   -117.00 -91.00   0.50    1.00    --  -79.50 -58.00-178.73   52
  46  \w    -89.00 -35.00   0.50    1.00    --  -79.50 130.00  17.25  108
  47  \w   -124.00 -99.00   0.50    1.00    --  -79.50 -64.00 -84.08   50
  48  \w   -117.00 -91.00   0.50    1.00    --  -79.50 -60.00 117.09   52
  49  \w   -118.00 -91.00   0.50    1.00    --  -79.50 -61.00 140.95   54
  50  \w   -128.00-103.00   0.50    1.00    --  -79.50-119.00  13.31   50
  51  \w    -89.00 -42.00   0.50    1.00    --  -79.50 135.00  80.92   94
  52  \w   -127.00-102.00   0.50    1.00    --  -79.50 -55.00-141.06   50
  53  \w   -120.00 -93.00   0.50    1.00    --  -79.50 -63.00-160.91   54
  54  \w   -118.00 -92.00   0.50    1.00    --  -79.50 -57.00  77.78   52
  55  \w   -120.00 -93.00   0.50    1.00    --  -79.50 -50.00 -50.71   54
  56  \w     56.00  82.00   0.50    1.00    --   82.37 -95.00   0.00   52
  57  \w     53.00  89.00   0.50    1.00    --   82.37 -95.00 -90.00   72
  58  \w     48.00  74.00   0.50    1.00    --   82.37 -95.00-120.00   52
  59  \w     56.00  99.00   0.50    1.00    --   82.37-112.00-120.00   86
  60  \w     71.00 122.00   0.50    1.00    --   82.37  15.00 -90.00  102
  61  \w     64.00 125.00   0.50    1.00    --   82.37  15.00   0.00  122
  62  \w    102.00 127.00   0.50    1.00    --   82.37  15.00-150.00   50
  63  \w     43.00  71.00   0.50    1.00    --   82.37-112.00  90.00   56
  64  \w     54.00  98.00   0.50    1.00    --   82.37-112.00  60.00   88
  65  \w    104.00 130.00   0.50    1.00    --   82.37  15.00-180.00   52
  66  \w     34.00  60.00   0.50    1.00    --   82.37-112.00 -60.00   52
  67  \w    104.00 130.00   0.50    1.00    --   85.25  64.00-121.92   52
  68  \w     99.00 126.00   0.50    1.00    --   85.25  54.00  -2.22   54
  69  \w    104.00 129.00   0.50    1.00    --   85.25 112.00  47.86   50
  70  \w     97.00 122.00   0.50    1.00    --   85.25  58.00 -37.87   50
  71  \w     39.00  98.00   0.50    1.00    --   85.25-109.00-176.83  118
  72  \w    104.00 129.00   0.50    1.00    --   85.25 113.00 -16.55   50
  73  \w    100.00 134.00   0.50    1.00    --   85.25  52.00  19.15   68

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-R'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_av_unetI/netI     0.0124
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            27730
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.060
_diffrn_reflns_theta_min         2.183
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R X-ray Source'
_exptl_absorpt_coefficient_mu    1.404
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.383
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021) 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            'clear pale colourless'
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_description       plate
_exptl_crystal_F_000             1236
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene'
_exptl_crystal_size_max          0.434
_exptl_crystal_size_mid          0.149
_exptl_crystal_size_min          0.028
_refine_diff_density_max         0.285
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details 'H. D. Flack (1983)'
_refine_ls_abs_structure_Flack   0.487(17)
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_number_parameters     383
_refine_ls_number_reflns         5588
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.0881
_reflns_Friedel_coverage         0.872
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                5522
_reflns_number_total             5588
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc01996f2.cif
_cod_data_source_block           MaDi133_MaJu_a
_cod_depositor_comments
'Adding full bibliography for 1574408--1574414.cif.'
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               1574409
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.584
_shelx_estimated_absorpt_t_max   0.959
_shelx_res_checksum              51125