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_1574410
_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 N2 P S, 0.5(C6 H6)'
_chemical_formula_sum            'C25 H31 B N2 P S'
_chemical_formula_weight         433.36
_chemical_name_common            (SIMes)BH2(SCP)
_chemical_name_systematic        2-SIMes
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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   mixed
_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                 90.5620(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.51490(10)
_cell_length_b                   19.1431(2)
_cell_length_c                   17.13230(10)
_cell_measurement_reflns_used    27873
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.3240
_cell_measurement_theta_min      3.4490
_cell_volume                     2464.51(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.96a (Rigaku OD, 2021)'
_computing_data_collection       'BIS 2011.8 / APEX2 ver. 2014.9 (Bruker AXS)'
_computing_data_reduction        'CrysAlisPro 1.171.41.96a (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      99.99(10)
_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     62.00  93.00   0.50    0.50    --   46.00  51.00  -3.02   62
   2  \w     75.00 130.00   0.50    0.50    --   83.50  20.00 150.95  110
   3  \w     54.00 129.00   0.50    0.50    --   80.41  15.00  30.00  150
   4  \w     54.00 129.00   0.50    0.50    --   80.41  15.00 -30.00  150
   5  \w     70.00 130.00   0.50    0.50    --   83.50  18.00-111.11  120
   6  \w     20.00  87.00   0.50    0.50    --   60.91-126.00-120.00  134
   7  \w     35.00  97.00   0.50    0.50    --   80.41-112.00-180.00  124
   8  \w     35.00  97.00   0.50    0.50    --   80.41-112.00 -30.00  124
   9  \w     35.00  97.00   0.50    0.50    --   80.41-112.00   0.00  124
  10  \w     35.00  97.00   0.50    0.50    --   80.41-112.00  30.00  124
  11  \w     35.00  97.00   0.50    0.50    --   80.41-112.00  60.00  124
  12  \w     35.00  97.00   0.50    0.50    --   80.41-112.00 120.00  124
  13  \w     35.00  97.00   0.50    0.50    --   80.41-112.00 150.00  124
  14  \w     35.00  97.00   0.50    0.50    --   80.41-112.00  90.00  124
  15  \w     35.00  97.00   0.50    0.50    --   80.41-112.00 -60.00  124
  16  \w     35.00  97.00   0.50    0.50    --   80.41-112.00 -90.00  124
  17  \w     40.00  86.00   0.50    0.50    --   80.41 -95.00 -60.00   92
  18  \w     35.00  97.00   0.50    0.50    --   80.41-112.00-120.00  124
  19  \w     35.00  97.00   0.50    0.50    --   80.41-112.00-150.00  124
  20  \w     51.00  93.00   0.50    0.50    --   83.50-101.00-179.19   84
  21  \w     40.00  86.00   0.50    0.50    --   80.41 -95.00-150.00   92
  22  \w     40.00  86.00   0.50    0.50    --   80.41 -95.00-120.00   92
  23  \w     40.00  86.00   0.50    0.50    --   80.41 -95.00 -90.00   92
  24  \w     20.00  66.00   0.50    0.50    --   60.91 -95.00   0.00   92
  25  \w    -99.00 -33.00   0.50    0.50    --  -79.50 121.00 105.41  132
  26  \w    -94.00 -30.00   0.50    0.50    --  -76.35 112.00  30.00  128
  27  \w    -94.00 -30.00   0.50    0.50    --  -76.35 112.00-180.00  128
  28  \w    -94.00 -30.00   0.50    0.50    --  -76.35 112.00 -90.00  128
  29  \w    -94.00 -30.00   0.50    0.50    --  -76.35 112.00  90.00  128
  30  \w    -94.00 -35.00   0.50    0.50    --  -79.50 108.00 111.18  118
  31  \w   -122.00 -94.00   0.50    0.50    --  -79.50 -64.00  93.62   56
  32  \w   -123.00 -93.00   0.50    0.50    --  -79.50 -60.00 151.51   60
  33  \w   -125.00 -94.00   0.50    0.50    --  -79.50 -55.00 130.13   62
  34  \w   -109.00 -78.00   0.50    0.50    --  -62.00 -48.00 157.74   62
  35  \w   -119.00 -89.00   0.50    0.50    --  -74.00 -55.00  99.89   60
  36  \w   -123.00 -92.00   0.50    0.50    --  -78.00 -58.00  45.81   62
  37  \w   -122.00 -92.00   0.50    0.50    --  -78.00 -59.00   1.92   60
  38  \w   -122.00 -89.00   0.50    0.50    --  -74.00 -42.00  59.55   66
  39  \w   -109.00 -78.00   0.50    0.50    --  -62.00 -48.00  11.38   62
  40  \w   -104.00 -74.00   0.50    0.50    --  -58.00 -51.00 -73.05   60
  41  \w   -109.00 -78.00   0.50    0.50    --  -62.00 -48.00-105.17   62
  42  \w   -128.00 -94.00   0.50    0.50    --  -79.50 -43.00 -42.87   68
  43  \w   -125.00 -87.00   0.50    0.50    --  -79.50-133.00  38.77   76
  44  \w   -125.00 -88.00   0.50    0.50    --  -79.50-130.00 -44.85   74
  45  \w   -126.00 -94.00   0.50    0.50    --  -79.50-118.00  62.62   64
  46  \w   -125.00 -90.00   0.50    0.50    --  -79.50-127.00 107.43   70

;
_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  0.0252
_diffrn_reflns_av_unetI/netI     0.0109
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            47497
_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         70.052
_diffrn_reflns_theta_min         3.462
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R X-ray Source'
_exptl_absorpt_coefficient_mu    1.867
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.645
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.96a (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 colourless'
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_description       block
_exptl_crystal_F_000             924
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene'
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.031
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         4681
_refine_ls_number_restraints     474
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0418
_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^)+(0.0616P)^2^+1.4453P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1144
_refine_ls_wR_factor_ref         0.1159
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4328
_reflns_number_total             4681
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc01996f2.cif
_cod_data_source_block           MaDi171_MaJu_a
_cod_depositor_comments
'Adding full bibliography for 1574408--1574414.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1574410
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.684
_shelx_estimated_absorpt_t_max   0.946
_shelx_res_checksum              52640