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_1574010
_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         'C30 H42 B N O'
_chemical_formula_sum            'C30 H42 B N O'
_chemical_formula_weight         443.45
_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             2023-02-16
_audit_creation_method           'CIF-fill 1.3q (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                 95.7630(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.15680(10)
_cell_length_b                   11.11500(10)
_cell_length_c                   26.1678(3)
_cell_measurement_reflns_used    18057
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.0080
_cell_measurement_theta_min      3.3890
_cell_volume                     2649.84(5)
_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 0.989
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w     56.00  84.00   0.50    0.05    --   85.25-133.00 -32.15   56
  2  \w     38.00  93.00   0.50    0.05    --   85.25-136.00 -47.17  110
  3  \w     39.00  93.00   0.50    0.05    --   85.25-132.00 -71.91  108
  4  \w     54.00 102.00   0.50    0.05    --   85.25-131.00 -86.71   96
  5  \w     48.00  74.00   0.50    0.05    --   85.25-135.00-129.03   52
  6  \w     43.00  69.00   0.50    0.05    --   85.25-126.00-124.43   52
  7  \w     61.00  86.00   0.50    0.05    --   58.57-126.00-120.00   50
  8  \w     41.00  91.00   0.50    0.05    --   85.25-107.00 -11.43  100
  9  \w     60.00  86.00   0.50    0.05    --   85.25-127.00  59.69   52
 10  \w     40.00  89.00   0.50    0.05    --   85.25-104.00 -40.82   98
 11  \w     40.00  65.00   0.50    0.05    --   85.25-108.00  61.79   50
 12  \w     41.00  70.00   0.50    0.05    --   85.25-129.00 132.92   58
 13  \w     74.00  99.00   0.50    0.05    --   85.25-122.00 172.47   50
 14  \w     59.00  85.00   0.50    0.05    --   85.25-101.00 172.07   52
 15  \w     42.00  90.00   0.50    0.05    --   85.25 -99.00  64.08   96
 16  \w     49.00  75.00   0.50    0.05    --   85.25 -92.00  62.70   52
 17  \w     47.00  86.00   0.50    0.05    --   85.25 -85.00  -4.98   78
 18  \w     44.00  69.00   0.50    0.05    --   85.25 -73.00  66.39   50
 19  \w     59.00  85.00   0.50    0.05    --   85.25 -86.00 -43.12   52
 20  \w     62.00  89.00   0.50    0.05    --   85.25 -92.00 -80.07   54
 21  \w     45.00  70.00   0.50    0.05    --   85.25 -75.00-138.20   50
 22  \w    104.00 129.00   0.50    0.05    --   85.25 114.00 -53.87   50
 23  \w    102.00 127.00   0.50    0.05    --   85.25 116.00-155.26   50
 24  \w    105.00 131.00   0.50    0.05    --   85.25 122.00   8.82   52
 25  \w    102.00 132.00   0.50    0.05    --   85.25 116.00 175.95   60
 26  \w    103.00 128.00   0.50    0.05    --   85.25  66.00  65.38   50
 27  \w     99.00 124.00   0.50    0.05    --   85.25  63.00 154.55   50
 28  \w     90.00 118.00   0.50    0.05    --   82.28  15.00  60.00   56
 29  \w     96.00 136.00   0.50    0.05    --   85.25  23.00 -61.99   80
 30  \w    106.00 134.00   0.50    0.05    --   85.25  51.00-153.71   56
 31  \w     99.00 124.00   0.50    0.05    --   85.25  47.00-178.12   50
 32  \w   -100.00 -63.00   0.50    0.05    --  -50.00 -45.00 -26.57   74
 33  \w   -128.00-100.00   0.50    0.05    --  -79.50 -51.00  86.30   56
 34  \w   -122.00 -92.00   0.50    0.05    --  -79.50 -63.00 123.44   60
 35  \w   -101.00 -69.00   0.50    0.05    --  -54.00 -50.00 117.67   64
 36  \w   -111.00 -85.00   0.50    0.05    --  -62.00 -48.00  91.45   52
 37  \w    -99.00 -63.00   0.50    0.05    --  -50.00 -46.00 172.88   72
 38  \w   -118.00 -92.00   0.50    0.05    --  -79.50 -61.00  52.66   52
 39  \w   -119.00 -87.00   0.50    0.05    --  -74.00 -60.00 -23.09   64
 40  \w   -119.00 -93.00   0.50    0.05    --  -79.50 -63.00-179.63   52
 41  \w   -125.00 -99.00   0.50    0.05    --  -79.50-114.00  89.39   52
 42  \w   -126.00 -90.00   0.50    0.05    --  -79.50-135.00 177.28   72
;
_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      0.1193276000
_diffrn_orient_matrix_UB_12      0.0907891000
_diffrn_orient_matrix_UB_13      -0.0115834000
_diffrn_orient_matrix_UB_21      0.0494476000
_diffrn_orient_matrix_UB_22      0.0104371000
_diffrn_orient_matrix_UB_23      0.0578792000
_diffrn_orient_matrix_UB_31      0.1090495000
_diffrn_orient_matrix_UB_32      -0.1042234000
_diffrn_orient_matrix_UB_33      -0.0043353000
_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  0.0391
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            28398
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.493
_diffrn_reflns_theta_min         3.395
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    0.490
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76125
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021) Empirical 
 absorption correction using spherical harmonics, implemented in SCALE3 
 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.112
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_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_size_max          0.460
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         5435
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0781P)^2^+0.7187P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1338
_refine_ls_wR_factor_ref         0.1388
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4671
_reflns_number_total             5435
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc00154d2.cif
_cod_data_source_block           1-CO
_cod_depositor_comments
'Adding full bibliography for 1574010--1574019.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1574010
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.806
_shelx_estimated_absorpt_t_max   0.939
_shelx_res_checksum              7109