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_1574408
_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 As B N2 O, 0.5 (C7 H8)'
_chemical_formula_sum            'C25.5 H32 As B N2 O'
_chemical_formula_weight         468.26
_chemical_name_common            (SIMes)BH2(ASCO)
_chemical_name_systematic        7
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Photo-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   geom
_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                 90.683(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.5069(4)
_cell_length_b                   18.7077(16)
_cell_length_c                   17.6728(7)
_cell_measurement_reflns_used    6247
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.0430
_cell_measurement_theta_min      3.4340
_cell_volume                     2481.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.142a (Rigaku OD, 2024)'
_computing_data_collection
;
 CrysAlisPro system (CCD 41.118a 64-bit (release 23-09-2021))
;
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w     15.00  81.00   0.60    7.00    --   61.01-115.00 169.00  110
  2  \w    -83.00 -17.00   0.60    7.00    --  -61.92 115.00-101.00  110
  3  \w    -93.00 -27.00   0.60    7.00    --  -72.66 115.00-101.00  110
  4  \w     28.00  94.00   0.60    7.00    --   74.07-115.00 169.00  110
  5  \w    -97.00 -31.00   0.60    7.00    --  -76.30 115.00-101.00  110
  6  \w     32.00  98.00   0.60    7.00    --   78.44-115.00 169.00  110
  7  \w     28.00  55.00   0.60    7.00    --   14.00  60.00  17.51   45
  8  \w    -95.00 -60.80   0.60    7.00    --  -46.00 -39.00 156.47   57
  9  \w   -105.00 -75.00   0.60    7.00    --  -58.00 -50.00-112.84   50
 10  \w     20.00  65.00   0.60    7.00    --   61.01 -95.00 -30.00   75
 11  \w     20.00  65.00   0.60    7.00    --   61.01 -95.00-150.00   75
 12  \w   -114.00 -83.40   0.60    7.00    --  -66.00 -46.00 -26.81   51
 13  \w   -113.00 -83.00   0.60    7.00    --  -66.00 -47.00  11.25   50
 14  \w   -117.00 -87.00   0.60    7.00    --  -70.00 -47.00-148.79   50
 15  \w   -113.00 -87.80   0.60    7.00    --  -70.00 -59.00 -44.82   42
 16  \w   -115.00 -86.80   0.60    7.00    --  -70.00 -58.00-114.87   47
 17  \w   -118.00 -92.80   0.60    7.00    --  -74.00 -61.00 165.37   42
 18  \w   -118.00 -91.60   0.60    7.00    --  -74.00 -47.00   4.35   44
 19  \w   -118.00 -91.00   0.60    7.00    --  -74.00 -58.00  97.21   45
 20  \w   -116.00 -90.80   0.60    7.00    --  -74.00 -55.00-101.72   42
 21  \w    -94.00 -67.00   0.60    7.00    --  -76.30 112.00 150.00   45
 22  \w    -85.00 -31.00   0.60    7.00    --  -76.30 112.00-150.00   90
 23  \w   -100.00 -37.00   0.60    7.00    --  -79.50 115.00 167.30  105
 24  \w   -111.00 -74.40   0.60    7.00    --  -79.50 -20.00  58.80   61
 25  \w   -122.00 -95.00   0.60    7.00    --  -79.50 -43.00 -63.15   45
 26  \w   -124.00 -97.00   0.60    7.00    --  -79.50 -52.00  47.46   45
 27  \w   -123.00 -96.60   0.60    7.00    --  -79.50 -49.00 177.67   44
 28  \w   -126.00 -96.00   0.60    7.00    --  -79.50 -45.00 -22.61   50
 29  \w   -127.00-100.00   0.60    7.00    --  -79.50 -39.00 154.09   45
 30  \w     43.00  97.00   0.60    7.00    --   81.85-108.00 -92.47   90
;
_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      -0.0959978000
_diffrn_orient_matrix_UB_12      -0.0673600000
_diffrn_orient_matrix_UB_13      0.0288535000
_diffrn_orient_matrix_UB_21      0.0957555000
_diffrn_orient_matrix_UB_22      -0.0453574000
_diffrn_orient_matrix_UB_23      -0.0596968000
_diffrn_orient_matrix_UB_31      0.1539040000
_diffrn_orient_matrix_UB_32      -0.0135730000
_diffrn_orient_matrix_UB_33      0.0565981000
_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  0.0666
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20863
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        65.089
_diffrn_reflns_theta_max         65.089
_diffrn_reflns_theta_min         3.440
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    1.982
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.869
_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            colourless
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_description       plate
_exptl_crystal_F_000             980
_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'
_exptl_crystal_size_max          0.085
_exptl_crystal_size_mid          0.032
_exptl_crystal_size_min          0.017
_refine_diff_density_max         0.828
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.317
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         4222
_refine_ls_number_restraints     560
_refine_ls_restrained_S_all      1.317
_refine_ls_R_factor_all          0.1611
_refine_ls_R_factor_gt           0.1157
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3318
_refine_ls_wR_factor_ref         0.3669
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2474
_reflns_number_total             4222
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc01996f2.cif
_cod_data_source_block           MaDi151_MaJu_auto_a
_cod_depositor_comments
'Adding full bibliography for 1574408--1574414.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1574408
_shelx_shelxl_version_number     2019/2
_shelx_res_checksum              22594