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_1574018
_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_absolute_configuration unk
_chemical_formula_moiety         'C70 H108 B2 Li4 N2 O3 S2'
_chemical_formula_sum            'C70 H108 B2 Li4 N2 O3 S2'
_chemical_formula_weight         1139.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-07-24
_audit_creation_method           'CIF-fill 1.4m (K.Radacki, 2005-23)'
_audit_update_record
;
2024-10-18 deposited with the CCDC.	2025-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.0250(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.65140(10)
_cell_length_b                   21.0348(2)
_cell_length_c                   16.8392(2)
_cell_measurement_reflns_used    37160
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.8920
_cell_measurement_theta_min      2.7240
_cell_volume                     3626.22(7)
_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 1.000
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w     48.00 135.00   0.50    0.20    --   84.34  15.00  60.00  174
  2  \w     34.00  84.00   0.50    0.20    --   76.32 -95.00-120.00  100
  3  \w     31.00  93.00   0.50    0.20    --   76.32-112.00-180.00  124
  4  \w     38.00 109.00   0.50    0.20    --   58.45  15.00   0.00  142
  5  \w    -97.00 -22.00   0.50    0.20    --  -69.54 126.00-180.00  150
  6  \w    -92.00 -31.00   0.50    0.20    --  -76.37 112.00  30.00  122
  7  \w     16.00  66.00   0.50    0.20    --   58.45 -95.00 -60.00  100
  8  \w     48.00 135.00   0.50    0.20    --   84.34  15.00 120.00  174
  9  \w     34.00  84.00   0.50    0.20    --   76.32 -95.00 -60.00  100
 10  \w     40.00 127.00   0.50    0.20    --   76.32  15.00-150.00  174
 11  \w    -97.00 -22.00   0.50    0.20    --  -69.54 126.00 120.00  150
 12  \w     24.00  99.00   0.50    0.20    --   71.26-126.00 150.00  150
 13  \w     39.00  93.00   0.50    0.20    --   84.34-112.00  60.00  108
 14  \w   -127.00 -40.00   0.50    0.20    --  -76.37 -15.00 -90.00  174
 15  \w     16.00  66.00   0.50    0.20    --   58.45 -95.00-150.00  100
 16  \w     38.00 109.00   0.50    0.20    --   58.45  15.00 -60.00  142
 17  \w   -127.00 -40.00   0.50    0.20    --  -76.37 -15.00   0.00  174
 18  \w     34.00  84.00   0.50    0.20    --   76.32 -95.00   0.00  100
 19  \w     31.00  93.00   0.50    0.20    --   76.32-112.00-120.00  124
 20  \w     39.00  93.00   0.50    0.20    --   84.34-112.00 120.00  108
 21  \w     48.00 135.00   0.50    0.20    --   84.34  15.00-120.00  174
 22  \w   -120.00 -34.00   0.50    0.20    --  -69.54 -15.00  90.00  172
 23  \w   -110.00 -31.00   0.50    0.20    --  -60.16 -15.00  30.00  158
 24  \w    -92.00 -31.00   0.50    0.20    --  -76.37 112.00 -30.00  122
 25  \w     48.00 135.00   0.50    0.20    --   84.34  15.00 -30.00  174
 26  \w     16.00  66.00   0.50    0.20    --   58.45 -95.00 -30.00  100
 27  \w     16.00  66.00   0.50    0.20    --   58.45 -95.00  90.00  100
 28  \w     31.00  93.00   0.50    0.20    --   76.32-112.00   0.00  124
;
_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      0.1339847000
_diffrn_orient_matrix_UB_12      -0.0330828000
_diffrn_orient_matrix_UB_13      0.0180466000
_diffrn_orient_matrix_UB_21      0.0128395000
_diffrn_orient_matrix_UB_22      0.0029626000
_diffrn_orient_matrix_UB_23      0.0933558000
_diffrn_orient_matrix_UB_31      -0.0672286000
_diffrn_orient_matrix_UB_32      -0.0652578000
_diffrn_orient_matrix_UB_33      -0.0049660000
_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  0.0273
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            57318
_diffrn_reflns_point_group_measured_fraction_full 0.911
_diffrn_reflns_point_group_measured_fraction_max 0.860
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.810
_diffrn_reflns_theta_min         2.730
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    0.974
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.590
_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            yellow
_exptl_crystal_density_diffrn    1.043
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_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          0.241
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.089
_refine_diff_density_max         0.200
_refine_diff_density_min         -0.170
_refine_diff_density_rms         0.030
_refine_ls_abs_structure_details 'Refined as an inversion twin.'
_refine_ls_abs_structure_Flack   0.435(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     909
_refine_ls_number_reflns         12842
_refine_ls_number_restraints     781
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0288
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0469P)^2^+0.5862P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0763
_reflns_Friedel_coverage         0.727
_reflns_Friedel_fraction_full    0.816
_reflns_Friedel_fraction_max     0.746
_reflns_number_gt                12591
_reflns_number_total             12842
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc00154d2.cif
_cod_data_source_block           Li2(1-S)
_cod_depositor_comments
'Adding full bibliography for 1574010--1574019.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1574018
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              90639
_shelx_fab_checksum              37494