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_1574413
_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_absolute_configuration unk
_chemical_formula_moiety         'C29 H32 B F3 N5 P S, 2 (C6 H6)'
_chemical_formula_sum            'C41 H44 B F3 N5 P S'
_chemical_formula_weight         737.65
_chemical_name_common            (SIMes)BH2S(CN3PPhCF3)
_chemical_name_systematic        3-PhCF3
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-01-02
_audit_creation_method           'CIF-fill 1.5o (K.Radacki, 2005-24)'
_audit_update_record
;
2025-03-03 deposited with the CCDC.	2025-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 121.3370(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.0260(2)
_cell_length_b                   24.25870(10)
_cell_length_c                   9.71050(10)
_cell_measurement_reflns_used    52353
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.7010
_cell_measurement_theta_min      3.2790
_cell_volume                     3828.05(7)
_computing_cell_refinement       'CrysAlisPro 1.171.43.142a (Rigaku OD, 2024)'
_computing_data_collection
;
 CrysAlisPro system (CCD 42.72a 64-bit (release 07-10-2022))
;
_computing_data_reduction        'CrysAlisPro 1.171.43.142a (Rigaku OD, 2024)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2019/2 (Sheldrick, 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                 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 0.995
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w    104.00 135.00   0.50    0.05    --   85.25  46.00-162.51   62
  2  \w     17.00  43.00   0.50    0.05    --    6.00  64.00 -24.17   52
  3  \w    100.00 135.00   0.50    0.05    --   85.25  46.00 138.96   70
  4  \w    100.00 131.00   0.50    0.05    --   85.25  58.00 145.20   62
  5  \w     98.00 127.00   0.50    0.05    --   85.25  57.00  94.33   58
  6  \w    104.00 130.00   0.50    0.05    --   85.25  43.00  34.61   52
  7  \w     87.00 136.00   0.50    0.05    --   85.25  24.00  95.45   98
  8  \w    106.00 131.00   0.50    0.05    --   85.25  42.00  12.32   50
  9  \w    103.00 128.00   0.50    0.05    --   85.25  45.00-127.11   50
 10  \w     98.00 130.00   0.50    0.05    --   85.25  37.00 -50.69   64
 11  \w     87.00 113.00   0.50    0.05    --   82.35  15.00-150.00   52
 12  \w     98.00 123.00   0.50    0.05    --   85.25  45.00  -4.31   50
 13  \w     73.00 122.00   0.50    0.05    --   85.25  21.00  18.83   98
 14  \w     59.00  89.00   0.50    0.05    --   85.25  12.00 -40.84   60
 15  \w    106.00 132.00   0.50    0.05    --   85.25  12.00 -40.84   52
 16  \w     88.00 114.00   0.50    0.05    --   82.35  15.00  60.00   52
 17  \w     87.00 113.00   0.50    0.05    --   85.25  20.00 150.39   52
 18  \w    106.00 131.00   0.50    0.05    --   85.25 110.00  78.72   50
 19  \w     96.00 125.00   0.50    0.05    --   85.25 126.00 158.86   58
 20  \w     92.00 118.00   0.50    0.05    --   85.25 138.00 -57.71   52
 21  \w     97.00 122.00   0.50    0.05    --   85.25 125.00 -83.56   50
 22  \w     92.00 118.00   0.50    0.05    --   85.25 134.00-103.99   52
 23  \w     44.00  69.00   0.50    0.05    --   85.25 -72.00  48.35   50
 24  \w     39.00  67.00   0.50    0.05    --   85.25-131.00 146.81   56
 25  \w     65.00  91.00   0.50    0.05    --   85.25-139.00   7.72   52
 26  \w     79.00 105.00   0.50    0.05    --   85.25-138.00 -41.76   52
 27  \w     44.00  70.00   0.50    0.05    --   85.25-130.00-117.53   52
 28  \w     39.00  65.00   0.50    0.05    --   85.25-138.00 -41.76   52
 29  \w     44.00 104.00   0.50    0.05    --   85.25-134.00  19.20  120
 30  \w     38.00  66.00   0.50    0.05    --   85.25-122.00  88.90   56
 31  \w     59.00  85.00   0.50    0.05    --   85.25-126.00  86.43   52
 32  \w     48.00  97.00   0.50    0.05    --   85.25-116.00  52.87   98
 33  \w     74.00  99.00   0.50    0.05    --   85.25-122.00  88.90   50
 34  \w     36.00  98.00   0.50    0.05    --   78.00-115.00 131.59  124
 35  \w     39.00  82.00   0.50    0.05    --   85.25-127.00 153.26   86
 36  \w     76.00 102.00   0.50    0.05    --   85.25-131.00 146.81   52
 37  \w     67.00  92.00   0.50    0.05    --   82.35-112.00  90.00   50
 38  \w     42.00  93.00   0.50    0.05    --   85.25-101.00 172.96  102
 39  \w     47.00  73.00   0.50    0.05    --   82.35-112.00  30.00   52
 40  \w     60.00  92.00   0.50    0.05    --   85.25-100.00 133.65   64
 41  \w     37.00  62.00   0.50    0.05    --   82.35-112.00 -90.00   50
 42  \w     37.00  62.00   0.50    0.05    --   82.35-112.00-150.00   50
 43  \w     46.00  72.00   0.50    0.05    --   85.25-101.00-137.79   52
 44  \w     43.00  93.00   0.50    0.05    --   85.25 -98.00-161.51  100
 45  \w     42.00  92.00   0.50    0.05    --   85.25 -99.00-127.59  100
 46  \w     42.00  89.00   0.50    0.05    --   82.35 -95.00-180.00   94
 47  \w     40.00  65.00   0.50    0.05    --   82.35 -95.00-120.00   50
 48  \w     16.00  66.00   0.50    0.05    --   58.30 -95.00-180.00  100
 49  \w     47.00  92.00   0.50    0.05    --   85.25 -97.00 -70.29   90
 50  \w     65.00  90.00   0.50    0.05    --   82.35 -95.00 -30.00   50
 51  \w     36.00  76.00   0.50    0.05    --   71.06 -95.00 -30.00   80
 52  \w     56.00  92.00   0.50    0.05    --   85.25 -95.00 -54.68   72
 53  \w     65.00  90.00   0.50    0.05    --   82.35 -95.00 -90.00   50
 54  \w     56.00  92.00   0.50    0.05    --   85.25 -94.00  -8.37   72
 55  \w     40.00  65.00   0.50    0.05    --   82.35 -95.00  90.00   50
 56  \w     45.00  70.00   0.50    0.05    --   85.25 -88.00 131.28   50
 57  \w     61.00  93.00   0.50    0.05    --   85.25 -98.00 158.18   64
 58  \w     55.00  91.00   0.50    0.05    --   85.25 -95.00 102.24   72
 59  \w     45.00  70.00   0.50    0.05    --   85.25 -76.00-114.86   50
 60  \w     46.00  83.00   0.50    0.05    --   85.25 -85.00 -95.51   74
 61  \w    -97.00 -62.00   0.50    0.05    --  -78.00 114.00 -98.74   70
 62  \w    -97.00 -42.00   0.50    0.05    --  -78.00 114.00  14.93  110
 63  \w    -91.00 -48.00   0.50    0.05    --  -79.50 108.00-155.88   86
 64  \w   -122.00 -87.00   0.50    0.05    --  -74.00 -54.00 -87.97   70
 65  \w   -125.00-100.00   0.50    0.05    --  -79.50 -51.00-162.46   50
 66  \w   -107.00 -72.00   0.50    0.05    --  -58.00 -49.00 -77.83   70
 67  \w   -120.00 -89.00   0.50    0.05    --  -74.00 -57.00 -15.65   62
 68  \w   -128.00 -97.00   0.50    0.05    --  -79.50 -50.00  50.71   62
 69  \w   -107.00 -72.00   0.50    0.05    --  -58.00 -49.00 129.20   70
 70  \w   -127.00 -91.00   0.50    0.05    --  -79.50 -56.00 119.60   72
 71  \w   -103.00 -68.00   0.50    0.05    --  -54.00 -47.00 -13.35   70
 72  \w   -103.00 -68.00   0.50    0.05    --  -54.00 -48.00-137.15   70
 73  \w   -115.00 -87.00   0.50    0.05    --  -66.00 -44.00-149.85   56
 74  \w   -127.00 -94.00   0.50    0.05    --  -79.50-126.00 -57.61   66
 75  \w   -122.00 -97.00   0.50    0.05    --  -79.50-122.00  30.31   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-R'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
;
 CrysAlisPro convention (1999,Acta A55,543-557)
;
_diffrn_orient_matrix_UB_11      -0.0902535000
_diffrn_orient_matrix_UB_12      -0.0147350000
_diffrn_orient_matrix_UB_13      -0.1234729000
_diffrn_orient_matrix_UB_21      0.0281466000
_diffrn_orient_matrix_UB_22      -0.0344542000
_diffrn_orient_matrix_UB_23      -0.0960623000
_diffrn_orient_matrix_UB_31      0.0071315000
_diffrn_orient_matrix_UB_32      -0.0512570000
_diffrn_orient_matrix_UB_33      0.1001146000
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            80146
_diffrn_reflns_point_group_measured_fraction_full 0.921
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.375
_diffrn_reflns_theta_min         2.719
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    1.564
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.557
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.43.142a (Rigaku Oxford Diffraction, 2024) 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            yellow
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       block
_exptl_crystal_F_000             1552
_exptl_crystal_preparation
;
 For data collection the crystal was immersed in a film of perfluoropolyether 
 oil, mounted on a polyimide loop and transferred to stream of cold nitrogen 
 (Oxford Cryostream 800).
;
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene'
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.245
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details 'Refined as an inversion twin.'
_refine_ls_abs_structure_Flack   0.226(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1014
_refine_ls_number_reflns         14270
_refine_ls_number_restraints     353
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0625P)^2^+0.7451P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1037
_reflns_Friedel_coverage         0.765
_reflns_Friedel_fraction_full    0.837
_reflns_Friedel_fraction_max     0.800
_reflns_number_gt                13415
_reflns_number_total             14270
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc01996f2.cif
_cod_data_source_block           MaJu043_MaJu_a
_cod_depositor_comments
'Adding full bibliography for 1574408--1574414.cif.'
_cod_original_cell_volume        3828.04(7)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1574413
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_min   0.553
_shelx_estimated_absorpt_t_max   0.872
_shelx_res_checksum              9446