Boraindenes as versatile precursors to benzannulated boron heterocycles
Wieprecht, Nele; Krummenacher, Ivo; Wüst, Leonie; Michel, Maximilian; Neder, Marco; Häfner, Andreas; Karg, Jordan; Braunschweig, Holger; Chemical Science  (2025) –; doi:10.1039/D5SC08526H

data_1576371
_publ_section_title
;
 Boraindenes as versatile precursors to benzannulated boron heterocycles
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D5SC08526H
_journal_year                    2025
_chemical_formula_moiety         'C38 H35 B Si'
_chemical_formula_sum            'C38 H35 B Si'
_chemical_formula_weight         530.56
_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             2025-02-04
_audit_creation_method           'CIF-fill 1.5r (K.Radacki, 2005-25)'
_audit_update_record
;
2025-11-03 deposited with the CCDC.	2025-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                85.654(2)
_cell_angle_beta                 83.431(2)
_cell_angle_gamma                73.428(2)
_cell_formula_units_Z            2
_cell_length_a                   7.24980(10)
_cell_length_b                   12.1524(3)
_cell_length_c                   18.0762(4)
_cell_measurement_reflns_used    10601
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.4180
_cell_measurement_theta_min      3.7790
_cell_volume                     1514.83(6)
_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-2019/2 (Sheldrick, 2019)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_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 0.991
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w     95.00 129.00   0.50    0.14    --   84.76  15.00  90.00   68
  2  \w     40.00  82.00   0.50    0.14    --   58.55  15.00  30.00   84
  3  \w     51.00  85.00   0.50    0.14    --   84.76  15.00  90.00   68
  4  \w     50.00 109.00   0.50    0.14    --   84.76  15.00  30.00  118
  5  \w     51.00 135.00   0.50    0.14    --   84.76  15.00 -30.00  168
  6  \w     53.00 133.00   0.50    0.14    --   84.76  15.00-120.00  160
  7  \w     40.00  66.00   0.50    0.14    --   58.55  15.00-180.00   52
  8  \w     24.00  69.00   0.50    0.14    --   58.55-126.00 -60.00   90
  9  \w     41.00  66.00   0.50    0.14    --   77.01-124.00 -31.00   50
 10  \w     58.00  83.00   0.50    0.14    --   84.76-124.00 -31.00   50
 11  \w     49.00  97.00   0.50    0.14    --   71.30-124.00 -31.00   96
 12  \w     30.00  57.00   0.50    0.14    --   58.55-124.00 -31.00   54
 13  \w     36.00  90.00   0.50    0.14    --   77.01-112.00   0.00  108
 14  \w     40.00  93.00   0.50    0.14    --   84.76-112.00  60.00  106
 15  \w     34.00  63.00   0.50    0.14    --   77.01 -95.00 150.00   58
 16  \w     32.00  91.00   0.50    0.14    --   77.01-112.00  90.00  118
 17  \w     66.00  92.00   0.50    0.14    --   84.76 -95.00 150.00   52
 18  \w     17.00  66.00   0.50    0.14    --   58.55 -95.00   0.00   98
 19  \w     32.00  65.00   0.50    0.14    --   71.30 -95.00  30.00   66
 20  \w     44.00  91.00   0.50    0.14    --   84.76 -95.00  90.00   94
 21  \w     65.00  90.00   0.50    0.14    --   84.76 -95.00  60.00   50
 22  \w     53.00  91.00   0.50    0.14    --   84.76 -95.00  30.00   76
 23  \w     67.00  92.00   0.50    0.14    --   84.76 -95.00 -30.00   50
 24  \w     29.00  77.00   0.50    0.14    --   71.30 -95.00-120.00   96
 25  \w     19.00  63.00   0.50    0.14    --   58.55 -95.00-150.00   88
 26  \w     44.00  70.00   0.50    0.14    --   84.76 -95.00-180.00   52
 27  \w     45.00  92.00   0.50    0.14    --   84.76 -95.00-150.00   94
 28  \w     67.00  92.00   0.50    0.14    --   84.76 -95.00-120.00   50
 29  \w     43.00  86.00   0.50    0.14    --   84.76 -95.00 120.00   86
 30  \w    -62.00 -26.00   0.50    0.14    --  -69.61 126.00 120.00   72
 31  \w    -97.00 -69.00   0.50    0.14    --  -79.50 117.00 141.30   56
 32  \w    -59.00 -34.00   0.50    0.14    --  -69.61 124.00  47.00   50
 33  \w    -55.00 -30.00   0.50    0.14    --  -60.24 124.00  47.00   50
 34  \w    -89.00 -64.00   0.50    0.14    --  -76.45 124.00  47.00   50
 35  \w    -68.00 -42.00   0.50    0.14    --  -76.45 112.00-150.00   52
 36  \w    -69.00 -44.00   0.50    0.14    --  -76.45 112.00-180.00   50
 37  \w   -104.00 -78.00   0.50    0.14    --  -60.24 -15.00-180.00   52
 38  \w   -127.00 -41.00   0.50    0.14    --  -76.45 -15.00 -30.00  172
 39  \w   -126.00 -41.00   0.50    0.14    --  -76.45 -15.00  60.00  170
;
_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      0.0123764000
_diffrn_orient_matrix_UB_12      0.0279165000
_diffrn_orient_matrix_UB_13      -0.0846784000
_diffrn_orient_matrix_UB_21      -0.0760717000
_diffrn_orient_matrix_UB_22      -0.1028968000
_diffrn_orient_matrix_UB_23      -0.0117497000
_diffrn_orient_matrix_UB_31      -0.2090008000
_diffrn_orient_matrix_UB_32      0.0785024000
_diffrn_orient_matrix_UB_33      0.0081493000
_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  0.0373
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20374
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.265
_diffrn_reflns_theta_min         3.799
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    0.852
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39877
_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            'clear light yellow'
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_description       plate
_exptl_crystal_F_000             564
_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          0.270
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         5922
_refine_ls_number_restraints     428
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0924P)^2^+0.5406P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1617
_refine_ls_wR_factor_ref         0.1726
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4592
_reflns_number_total             5922
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc08526h2.cif
_cod_data_source_block           E-7Tol
_cod_database_code               1576371
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_min   0.803
_shelx_estimated_absorpt_t_max   0.951
_shelx_res_checksum              71428