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_1574411
_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         'C37 H49 B12 N2 P S'
_chemical_formula_sum            'C37 H49 B12 N2 P S'
_chemical_formula_weight         714.53
_chemical_name_common            (SIMes)[BP(H)B(H)(C2B10H10Me)C(C12H8)S]
_chemical_name_systematic        6
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-02-23
_audit_creation_method           'CIF-fill 1.3q (K.Radacki, 2005-22)'
_audit_update_record
;
2025-03-03 deposited with the CCDC.	2025-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.2580(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.8665(2)
_cell_length_b                   8.27010(10)
_cell_length_c                   23.3283(2)
_cell_measurement_reflns_used    16044
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.1100
_cell_measurement_theta_min      3.7750
_cell_volume                     4025.68(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.68a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.68a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.68a (Rigaku OD, 2022)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w     99.00 125.00   0.50    0.60    --   85.25  56.00 123.36   52
  2  \w     95.00 127.00   0.50    0.60    --   85.25 137.00 -37.93   64
  3  \w    102.00 131.00   0.50    0.60    --   85.25 122.00 -69.75   58
  4  \w    101.00 126.00   0.50    0.60    --   85.25 118.00 -56.34   50
  5  \w    102.00 132.00   0.50    0.60    --   85.25  52.00-120.34   60
  6  \w     99.00 124.00   0.50    0.60    --   85.25  56.00-106.75   50
  7  \w    100.00 126.00   0.50    0.60    --   85.25  50.00 -42.83   52
  8  \w    100.00 128.00   0.50    0.60    --   85.25  50.00 -19.91   56
  9  \w    100.00 131.00   0.50    0.60    --   85.25  47.00  76.06   62
 10  \w     86.00 112.00   0.50    0.60    --   85.25  24.00  73.46   52
 11  \w     98.00 123.00   0.50    0.60    --   85.25  55.00  24.26   50
 12  \w    104.00 130.00   0.50    0.60    --   85.25  45.00 -65.19   52
 13  \w     98.00 124.00   0.50    0.60    --   85.25  44.00-138.12   52
 14  \w     72.00  98.00   0.50    0.60    --   58.57  15.00-120.00   52
 15  \w     50.00  77.00   0.50    0.60    --   85.25 -76.00 -50.90   54
 16  \w     69.00  97.00   0.50    0.60    --   85.25-116.00-133.08   56
 17  \w     46.00  98.00   0.50    0.60    --   85.25-117.00-175.65  104
 18  \w     50.00  76.00   0.50    0.60    --   85.25-136.00-171.83   52
 19  \w     42.00  99.00   0.50    0.60    --   85.25-126.00  94.85  114
 20  \w     53.00  99.00   0.50    0.60    --   85.25-124.00 124.95   92
 21  \w     43.00  68.00   0.50    0.60    --   82.28-114.00 119.00   50
 22  \w     42.00  93.00   0.50    0.60    --   85.25 -97.00 118.10  102
 23  \w     45.00  91.00   0.50    0.60    --   71.34-114.00 119.00   92
 24  \w     59.00  90.00   0.50    0.60    --   85.25 -92.00 173.47   62
 25  \w     22.00  47.00   0.50    0.60    --   58.57-114.00 119.00   50
 26  \w     53.00  83.00   0.50    0.60    --   85.25 -89.00  12.08   60
 27  \w     43.00  68.00   0.50    0.60    --   85.25 -95.00 -10.24   50
 28  \w     47.00  91.00   0.50    0.60    --   85.25-102.00-117.73   88
 29  \w     51.00  92.00   0.50    0.60    --   85.25-100.00-146.02   82
 30  \w     48.00  75.00   0.50    0.60    --   85.25 -85.00-111.04   54
 31  \w    -52.00 -17.00   0.50    0.60    --  -60.16 114.00-150.00   70
 32  \w    -88.00 -63.00   0.50    0.60    --  -76.35 114.00-150.00   50
 33  \w    -84.00 -25.00   0.50    0.60    --  -69.76 114.00-150.00  118
 34  \w    -88.00 -39.00   0.50    0.60    --  -74.00 104.00 146.36   98
 35  \w    -79.00 -53.00   0.50    0.60    --  -79.50  88.00 165.21   52
 36  \w   -125.00 -91.00   0.50    0.60    --  -79.50 -61.00 149.26   68
 37  \w   -102.00 -74.00   0.50    0.60    --  -58.00 -52.00-163.50   56
 38  \w   -118.00 -91.00   0.50    0.60    --  -74.00 -57.00-175.54   54
 39  \w   -127.00-101.00   0.50    0.60    --  -79.50 -52.00 -83.31   52
 40  \w   -118.00 -89.00   0.50    0.60    --  -70.00 -46.00 -71.19   58
 41  \w    -95.00 -60.00   0.50    0.60    --  -46.00 -42.00  74.12   70
 42  \w   -124.00 -84.00   0.50    0.60    --  -79.50-138.00 -59.60   80
;
_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      0.0197631000
_diffrn_orient_matrix_UB_12      -0.1767365000
_diffrn_orient_matrix_UB_13      -0.0111683000
_diffrn_orient_matrix_UB_21      0.0711157000
_diffrn_orient_matrix_UB_22      0.0485850000
_diffrn_orient_matrix_UB_23      0.0043886000
_diffrn_orient_matrix_UB_31      -0.0010362000
_diffrn_orient_matrix_UB_32      -0.0334858000
_diffrn_orient_matrix_UB_33      0.0649347000
_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  0.0370
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            43845
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.387
_diffrn_reflns_theta_min         3.790
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    1.297
_exptl_absorpt_correction_T_max  0.896
_exptl_absorpt_correction_T_min  0.371
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.42.68a (Rigaku Oxford Diffraction, 2022) 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    1.179
_exptl_crystal_description       plate
_exptl_crystal_F_000             1504
_exptl_crystal_preparation
;
 Crystals were grown from saturated solution. 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'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         8197
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0484P)^2^+2.0816P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1081
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6821
_reflns_number_total             8197
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc01996f2.cif
_cod_data_source_block           MaJu054_MaJu_autored_a
_cod_depositor_comments
'Adding full bibliography for 1574408--1574414.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1574411
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.781
_shelx_estimated_absorpt_t_max   0.975
_shelx_res_checksum              6814