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_1574412
_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         'C55 H53 As B2 N2'
_chemical_formula_sum            'C55 H53 As B2 N2'
_chemical_formula_weight         838.53
_chemical_name_common            (SIMes)BH2(As-C4BPh5)
_chemical_name_systematic        8
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_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                61.329(2)
_cell_angle_beta                 73.8450(10)
_cell_angle_gamma                64.999(2)
_cell_formula_units_Z            2
_cell_length_a                   13.8895(2)
_cell_length_b                   14.0251(2)
_cell_length_c                   14.5748(2)
_cell_measurement_reflns_used    30113
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.6690
_cell_measurement_theta_min      3.5220
_cell_volume                     2247.48(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.96a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.96a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.96a (Rigaku OD, 2021)'
_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 0.993
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w    -47.00  -8.00   0.60    1.00    --  -26.00 117.00  73.62   65
  2  \w    -95.00 -60.80   0.60    1.00    --  -46.00 -47.00 -48.55   57
  3  \w    -95.00 -60.80   0.60    1.00    --  -46.00 -49.00 -14.93   57
  4  \w   -107.00 -73.40   0.60    1.00    --  -58.00 -49.00 102.08   56
  5  \w   -107.00 -73.40   0.60    1.00    --  -58.00 -50.00  43.24   56
  6  \w   -111.00 -77.40   0.60    1.00    --  -62.00 -49.00 166.09   56
  7  \w   -119.00 -85.40   0.60    1.00    --  -70.00 -47.00  24.80   56
  8  \w   -118.00 -84.40   0.60    1.00    --  -70.00 -54.00-104.84   56
  9  \w   -120.00 -83.40   0.60    1.00    --  -70.00 -43.00  87.45   61
 10  \w    -97.00 -33.40   0.60    1.00    --  -78.00 114.00-112.85  106
 11  \w    -97.00 -33.40   0.60    1.00    --  -78.00 114.00 -78.02  106
 12  \w    -98.00 -32.00   0.60    1.00    --  -79.50 120.00  31.77  110
 13  \w   -126.00 -89.40   0.60    1.00    --  -79.50-131.00-136.85   61
 14  \w   -129.00 -93.00   0.60    1.00    --  -79.50 -47.00  51.24   60
 15  \w   -126.00 -86.40   0.60    1.00    --  -79.50-136.00 -52.73   66
 16  \w   -102.00 -33.00   0.60    1.00    --  -79.50 132.00  70.24  115
 17  \w   -125.00 -92.00   0.60    1.00    --  -79.50 -61.00 160.49   55
 18  \w   -127.00 -93.40   0.60    1.00    --  -79.50 -55.00 171.57   56
 19  \w    -97.00 -34.00   0.60    1.00    --  -79.50 115.00 179.43  105
 20  \w   -125.00 -92.00   0.60    1.00    --  -79.50 -60.00-129.64   55
 21  \w    -97.00 -34.00   0.60    1.00    --  -79.50 116.00-107.33  105
 22  \w   -126.00 -96.00   0.60    1.00    --  -79.50-117.00 -17.25   50
 23  \w   -128.00 -94.40   0.60    1.00    --  -79.50 -50.00 -30.58   56
 24  \w    -96.00 -34.80   0.60    1.00    --  -79.50 114.00 121.01  102
 25  \w   -125.00 -92.00   0.60    1.00    --  -79.50 -60.00  79.56   55
 26  \w   -125.00 -92.00   0.60    1.00    --  -79.50 -61.00 -46.19   55
 27  \w   -126.00 -92.40   0.60    1.00    --  -79.50-125.00 109.29   56
 28  \w    -92.00 -35.00   0.60    1.00    --  -79.50 102.00  33.13   95
 29  \w   -126.00 -87.00   0.60    1.00    --  -79.50-132.00  33.74   65
 30  \w   -126.00 -92.40   0.60    1.00    --  -79.50 -58.00  12.23   56
 31  \w   -128.00 -94.40   0.60    1.00    --  -79.50 -52.00  96.64   56
 32  \w   -126.00 -93.00   0.60    1.00    --  -79.50-120.00 136.74   55
 33  \w     40.00  88.60   0.60    1.00    --   82.35 -95.00  30.00   81
 34  \w     40.00  88.60   0.60    1.00    --   82.35 -95.00-150.00   81
 35  \w     40.00  88.60   0.60    1.00    --   82.35 -95.00  60.00   81
 36  \w     40.00  88.60   0.60    1.00    --   82.35 -95.00   0.00   81
 37  \w     37.00  91.60   0.60    1.00    --   82.35-112.00  30.00   91
 38  \w     46.00 133.00   0.60    1.00    --   82.35  15.00   0.00  145
 39  \w     40.00  88.60   0.60    1.00    --   82.35 -95.00 120.00   81
 40  \w     40.00  88.60   0.60    1.00    --   82.35 -95.00  90.00   81
 41  \w     40.00  88.60   0.60    1.00    --   82.35 -95.00 150.00   81
 42  \w     37.00  91.60   0.60    1.00    --   82.35-112.00 -60.00   91
 43  \w     97.00 130.00   0.60    1.00    --   85.25  60.00-107.90   55
 44  \w    100.00 130.00   0.60    1.00    --   85.25 119.00  -9.92   50
 45  \w     98.00 134.60   0.60    1.00    --   85.25  43.00 142.25   61
 46  \w     98.00 131.60   0.60    1.00    --   85.25  55.00-150.77   56
 47  \w     42.00  93.00   0.60    1.00    --   85.25 -97.00 -30.83   85
 48  \w     43.00  91.00   0.60    1.00    --   85.25 -94.00-118.03   80
 49  \w     38.00  98.00   0.60    1.00    --   85.25-120.00 161.31  100
 50  \w    101.00 131.00   0.60    1.00    --   85.25 118.00 -32.38   50
 51  \w     96.00 135.60   0.60    1.00    --   85.25  34.00-172.23   66
 52  \w     99.00 132.60   0.60    1.00    --   85.25  52.00  36.46   56
 53  \w     45.00  93.00   0.60    1.00    --   85.25 -97.00 179.12   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      -0.0254390000
_diffrn_orient_matrix_UB_12      0.0917089000
_diffrn_orient_matrix_UB_13      0.0410645000
_diffrn_orient_matrix_UB_21      -0.1158653000
_diffrn_orient_matrix_UB_22      0.0014261000
_diffrn_orient_matrix_UB_23      0.0335106000
_diffrn_orient_matrix_UB_31      0.0323022000
_diffrn_orient_matrix_UB_32      -0.0967359000
_diffrn_orient_matrix_UB_33      0.1088113000
_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  0.0196
_diffrn_reflns_av_unetI/netI     0.0113
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            41801
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.071
_diffrn_reflns_theta_min         3.472
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    1.308
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.729
_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            yellow
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_description       block
_exptl_crystal_F_000             880.0
_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          0.189
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.051
_refine_diff_density_max         1.528
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     735
_refine_ls_number_reflns         8445
_refine_ls_number_restraints     1071
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0710P)^2^+2.2178P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1253
_refine_ls_wR_factor_ref         0.1264
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8021
_reflns_number_total             8445
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc01996f2.cif
_cod_data_source_block           MaDi240_MaJu_a
_cod_depositor_comments
'Adding full bibliography for 1574408--1574414.cif.'
_cod_database_code               1574412
_shelx_shelxl_version_number     2019/2
_shelx_res_checksum              26808