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_1574017
_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         'C74 H116 B2 Li2 N2 O4 S2'
_chemical_formula_sum            'C74 H116 B2 Li2 N2 O4 S2'
_chemical_formula_weight         1197.30
_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   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-10-12
_audit_creation_method           'CIF-fill 1.4o (K.Radacki, 2005-23)'
_audit_update_record
;
2024-10-18 deposited with the CCDC.	2025-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                82.383(2)
_cell_angle_beta                 79.577(2)
_cell_angle_gamma                68.461(2)
_cell_formula_units_Z            1
_cell_length_a                   10.5609(3)
_cell_length_b                   13.0367(4)
_cell_length_c                   14.8835(4)
_cell_measurement_reflns_used    21793
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.4510
_cell_measurement_theta_min      3.0280
_cell_volume                     1869.70(10)
_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 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 0.993
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w     30.00  56.00   0.50    0.20    --   18.00  60.00-134.62   52
  2  \w     16.00  43.00   0.50    0.20    --    6.00  65.00  -3.83   54
  3  \w     34.00  60.00   0.50    0.20    --   22.00  58.00 -95.84   52
  4  \w     30.00  56.00   0.50    0.20    --   18.00  60.00  33.68   52
  5  \w     30.00  56.00   0.50    0.20    --   18.00  60.00  68.11   52
  6  \w     30.00  56.00   0.50    0.20    --   18.00  60.00 175.65   52
  7  \w     48.00  83.00   0.50    0.20    --   34.00  51.00 129.13   70
  8  \w     34.00  60.00   0.50    0.20    --   22.00  59.00 104.27   52
  9  \w     56.00  91.00   0.50    0.20    --   42.00  50.00  53.85   70
 10  \w     48.00 135.00   0.50    0.20    --   84.34  15.00  90.00  174
 11  \w     48.00 135.00   0.50    0.20    --   84.34  15.00 150.00  174
 12  \w     48.00 135.00   0.50    0.20    --   84.34  15.00 -30.00  174
 13  \w     48.00 135.00   0.50    0.20    --   84.34  15.00 -90.00  174
 14  \w     48.00 135.00   0.50    0.20    --   84.34  15.00-150.00  174
 15  \w     94.00 129.00   0.50    0.20    --   80.33  50.00 -49.50   70
 16  \w     48.00 135.00   0.50    0.20    --   84.34  15.00   0.00  174
 17  \w     42.00  92.00   0.50    0.20    --   84.34 -95.00   0.00  100
 18  \w     31.00  93.00   0.50    0.20    --   76.32-112.00  90.00  124
 19  \w     31.00  93.00   0.50    0.20    --   76.32-112.00  30.00  124
 20  \w     31.00  93.00   0.50    0.20    --   76.32-112.00-120.00  124
 21  \w     42.00  92.00   0.50    0.20    --   84.34 -95.00-180.00  100
 22  \w     42.00  92.00   0.50    0.20    --   84.34 -95.00-120.00  100
 23  \w     42.00  92.00   0.50    0.20    --   84.34 -95.00 -60.00  100
 24  \w     42.00  92.00   0.50    0.20    --   84.34 -95.00  30.00  100
 25  \w     42.00  92.00   0.50    0.20    --   84.34 -95.00  90.00  100
 26  \w     42.00  92.00   0.50    0.20    --   84.34 -95.00 150.00  100
 27  \w    -92.00 -31.00   0.50    0.20    --  -76.37 112.00  90.00  122
 28  \w    -97.00 -33.00   0.50    0.20    --  -79.50 115.00 114.74  128
 29  \w    -97.00 -22.00   0.50    0.20    --  -69.54 126.00  30.00  150
 30  \w    -92.00 -31.00   0.50    0.20    --  -76.37 112.00   0.00  122
 31  \w    -45.00 -18.00   0.50    0.20    --  -14.00 132.00  60.02   54
 32  \w    -92.00 -31.00   0.50    0.20    --  -76.37 112.00  30.00  122
 33  \w    -92.00 -31.00   0.50    0.20    --  -76.37 112.00  60.00  122
 34  \w   -101.00 -33.00   0.50    0.20    --  -79.50 125.00-101.52  136
 35  \w    -88.00 -14.00   0.50    0.20    --  -60.16 126.00-180.00  148
 36  \w    -92.00 -31.00   0.50    0.20    --  -76.37 112.00-150.00  122
 37  \w    -92.00 -31.00   0.50    0.20    --  -76.37 112.00-120.00  122
 38  \w    -79.00 -43.00   0.50    0.20    --  -30.00 -46.00-100.64   72
 39  \w    -91.00 -56.00   0.50    0.20    --  -42.00 -48.00 -37.87   70
 40  \w    -94.00 -59.00   0.50    0.20    --  -46.00 -51.00 127.73   70
 41  \w    -94.00 -59.00   0.50    0.20    --  -46.00 -51.00 169.68   70
 42  \w   -124.00 -92.00   0.50    0.20    --  -79.50 -63.00 129.28   64
 43  \w   -121.00 -86.00   0.50    0.20    --  -74.00 -57.00  63.85   70
 44  \w   -125.00 -90.00   0.50    0.20    --  -78.00 -58.00  83.08   70
 45  \w   -117.00 -83.00   0.50    0.20    --  -70.00 -56.00 156.69   68
 46  \w   -116.00 -85.00   0.50    0.20    --  -70.00 -59.00  44.17   62
 47  \w   -127.00 -92.00   0.50    0.20    --  -79.50 -55.00 113.46   70
 48  \w   -117.00 -83.00   0.50    0.20    --  -70.00 -56.00 -24.50   68
 49  \w   -121.00 -86.00   0.50    0.20    --  -74.00 -55.00   0.69   70
 50  \w   -122.00 -87.00   0.50    0.20    --  -74.00 -54.00  94.54   70
 51  \w   -118.00 -83.00   0.50    0.20    --  -70.00 -54.00 -43.39   70
 52  \w   -127.00 -92.00   0.50    0.20    --  -79.50 -54.00 -82.34   70
 53  \w   -121.00 -86.00   0.50    0.20    --  -74.00 -57.00-115.65   70
 54  \w   -128.00 -93.00   0.50    0.20    --  -79.50 -51.00-146.52   70
 55  \w   -121.00 -86.00   0.50    0.20    --  -74.00 -58.00-178.51   70
 56  \w   -128.00 -93.00   0.50    0.20    --  -79.50 -51.00-168.11   70
 57  \w   -102.00 -67.00   0.50    0.20    --  -54.00 -52.00-149.63   70
 58  \w   -111.00 -76.00   0.50    0.20    --  -62.00 -50.00 -95.68   70
 59  \w   -128.00 -93.00   0.50    0.20    --  -79.50 -51.00  40.51   70
 60  \w   -107.00 -72.00   0.50    0.20    --  -58.00 -49.00  47.96   70
 61  \w   -115.00 -80.00   0.50    0.20    --  -66.00 -50.00 110.69   70
 62  \w   -122.00 -87.00   0.50    0.20    --  -74.00 -52.00 132.00   70
 63  \w   -128.00 -93.00   0.50    0.20    --  -79.50 -49.00  91.62   70
 64  \w   -124.00 -86.00   0.50    0.20    --  -74.00 -43.00   6.83   76
 65  \w   -128.00 -90.00   0.50    0.20    --  -78.00 -42.00  -3.87   76
 66  \w   -115.00 -80.00   0.50    0.20    --  -66.00 -47.00 -72.03   70
 67  \w   -129.00 -93.00   0.50    0.20    --  -79.50 -48.00-134.13   72
 68  \w   -130.00 -91.00   0.50    0.20    --  -79.50 -41.00-118.33   78
 69  \w   -126.00 -92.00   0.50    0.20    --  -79.50-123.00-157.98   68
 70  \w   -125.00 -84.00   0.50    0.20    --  -79.50-139.00  58.14   82
;
_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      0.0164353000
_diffrn_orient_matrix_UB_12      -0.1220585000
_diffrn_orient_matrix_UB_13      0.0265010000
_diffrn_orient_matrix_UB_21      -0.1276674000
_diffrn_orient_matrix_UB_22      0.0360125000
_diffrn_orient_matrix_UB_23      0.0735248000
_diffrn_orient_matrix_UB_31      -0.0924225000
_diffrn_orient_matrix_UB_32      0.0054278000
_diffrn_orient_matrix_UB_33      -0.0708973000
_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  0.0529
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            48954
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.784
_diffrn_reflns_theta_min         3.027
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    0.980
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61338
_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            block
_exptl_crystal_density_diffrn    1.063
_exptl_crystal_description       red
_exptl_crystal_F_000             654
_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_size_max          0.170
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.090
_refine_diff_density_max         1.008
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         7406
_refine_ls_number_restraints     480
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0586
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1119P)^2^+0.4826P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1620
_refine_ls_wR_factor_ref         0.1664
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6548
_reflns_number_total             7406
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc00154d2.cif
_cod_data_source_block           Li(1-S)
_cod_depositor_comments
'Adding full bibliography for 1574010--1574019.cif.'
_cod_database_code               1574017
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.851
_shelx_estimated_absorpt_t_max   0.917
_shelx_res_checksum              71345
_shelx_fab_checksum              49618