Harnessing transient CAAC-stabilized mesitylborylenes for chalcogen activation.
Michel, Maximilian; Endres, Lukas; Fantuzzi, Felipe; Krummenacher, Ivo; Braunschweig, Holger; Chemical science 16 (2025) 5632–5639; doi:10.1039/d5sc00154d

data_1574016
_publ_section_title
;
 Harnessing transient CAAC-stabilized mesitylborylenes for chalcogen
 activation.
;
_journal_issue                   13
_journal_name_full               'Chemical science'
_journal_page_first              5632
_journal_page_last               5639
_journal_paper_doi               10.1039/d5sc00154d
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C29 H42 B N S'
_chemical_formula_sum            'C29 H42 B N S'
_chemical_formula_weight         447.50
_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   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-08-19
_audit_creation_method           'CIF-fill 1.3i (K.Radacki, 2005-22)'
_audit_update_record
;
2024-10-18 deposited with the CCDC.	2025-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.3370(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.00600(10)
_cell_length_b                   8.46370(10)
_cell_length_c                   17.39900(10)
_cell_measurement_reflns_used    15831
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.1610
_cell_measurement_theta_min      5.0920
_cell_volume                     2647.07(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_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 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   -124.00 -94.00   0.50    0.30    --  -79.50 -64.00 154.44   60
  2  \w   -125.00 -91.00   0.50    0.30    --  -79.50 -60.00  80.24   68
  3  \w   -125.00 -99.00   0.50    0.30    --  -79.50 -61.00  -4.58   52
  4  \w   -109.00 -70.00   0.50    0.30    --  -58.00 -40.00-100.43   78
  5  \w   -122.00 -96.00   0.50    0.30    --  -79.50 -64.00-172.63   52
  6  \w   -117.00 -85.00   0.50    0.30    --  -70.00 -58.00-132.00   64
  7  \w    -95.00 -60.00   0.50    0.30    --  -46.00 -47.00 -19.66   70
  8  \w   -126.00 -87.00   0.50    0.30    --  -79.50-132.00 -22.74   78
  9  \w    -95.00 -60.00   0.50    0.30    --  -46.00 -49.00 170.66   70
 10  \w    -88.00 -14.00   0.50    0.30    --  -60.16 126.00  60.00  148
 11  \w     81.00 106.00   0.50    0.30    --   85.25-139.00  34.76   50
 12  \w     40.00  90.00   0.50    0.30    --   85.25-121.00  74.83  100
 13  \w     40.00  66.00   0.50    0.30    --   85.25-139.00  34.76   52
 14  \w     56.00  94.00   0.50    0.30    --   85.25-120.00  53.34   76
 15  \w     64.00  94.00   0.50    0.30    --   85.25-130.00 -58.69   60
 16  \w     65.00  96.00   0.50    0.30    --   85.25-120.00 -84.86   62
 17  \w     76.00 101.00   0.50    0.30    --   85.25-128.00 -98.84   50
 18  \w     40.00  66.00   0.50    0.30    --   85.25-114.00-172.26   52
 19  \w     39.00  69.00   0.50    0.30    --   85.25-128.00 -98.84   60
 20  \w     29.00  79.00   0.50    0.30    --   71.26 -95.00-150.00  100
 21  \w     40.00  65.00   0.50    0.30    --   82.35 -95.00-150.00   50
 22  \w     50.00  81.00   0.50    0.30    --   85.25-117.00 -36.13   62
 23  \w     46.00  72.00   0.50    0.30    --   85.25-117.00  60.79   52
 24  \w     49.00  87.00   0.50    0.30    --   85.25 -86.00 146.16   76
 25  \w     63.00  88.00   0.50    0.30    --   82.35 -95.00 120.00   50
 26  \w     43.00  90.00   0.50    0.30    --   85.25 -93.00 102.91   94
 27  \w     61.00  93.00   0.50    0.30    --   85.25-101.00  67.70   64
 28  \w     47.00  83.00   0.50    0.30    --   85.25 -93.00-178.18   72
 29  \w     44.00  69.00   0.50    0.30    --   85.25 -72.00-148.13   50
 30  \w    105.00 130.00   0.50    0.30    --   85.25 111.00  48.02   50
 31  \w     93.00 130.00   0.50    0.30    --   85.25 138.00 121.35   74
 32  \w     96.00 121.00   0.50    0.30    --   85.25 128.00 169.95   50
 33  \w     96.00 131.00   0.50    0.30    --   85.25 128.00 135.49   70
 34  \w    100.00 125.00   0.50    0.30    --   85.25 119.00  61.06   50
 35  \w     95.00 120.00   0.50    0.30    --   85.25 128.00  30.42   50
 36  \w     97.00 132.00   0.50    0.30    --   85.25 129.00  -0.36   70
 37  \w     99.00 129.00   0.50    0.30    --   85.25 140.00-126.08   60
 38  \w     98.00 123.00   0.50    0.30    --   85.25  53.00-164.39   50
 39  \w    107.00 133.00   0.50    0.30    --   85.25  39.00-141.40   52
 40  \w     85.00 110.00   0.50    0.30    --   85.25  24.00-145.53   50
 41  \w     97.00 122.00   0.50    0.30    --   85.25  41.00  74.00   50
 42  \w     97.00 122.00   0.50    0.30    --   85.25  39.00 122.64   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      -0.0349992000
_diffrn_orient_matrix_UB_12      -0.1528292000
_diffrn_orient_matrix_UB_13      -0.0336974000
_diffrn_orient_matrix_UB_21      0.0249303000
_diffrn_orient_matrix_UB_22      0.0455728000
_diffrn_orient_matrix_UB_23      -0.0802852000
_diffrn_orient_matrix_UB_31      0.0741405000
_diffrn_orient_matrix_UB_32      -0.0876952000
_diffrn_orient_matrix_UB_33      0.0169740000
_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  0.0228
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28964
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.369
_diffrn_reflns_theta_min         4.921
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    1.182
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.906
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.41.112a (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            orange
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_description       block
_exptl_crystal_F_000             976
_exptl_crystal_preparation
;
 Crystalls were grown from saturated solution of Hexane at -30 \%C. 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_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         5457
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0524P)^2^+0.9437P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1016
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4961
_reflns_number_total             5457
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc00154d2.cif
_cod_data_source_block           1-S
_cod_depositor_comments
'Adding full bibliography for 1574010--1574019.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1574016
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.891
_shelx_estimated_absorpt_t_max   0.911
_shelx_res_checksum              77463