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_1576370
_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         'C37 H33 B Si'
_chemical_formula_sum            'C37 H33 B Si'
_chemical_formula_weight         516.53
_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             2024-09-20
_audit_creation_method           'CIF-fill 1.5e (K.Radacki, 2005-23)'
_audit_update_record
;
2025-11-03 deposited with the CCDC.	2025-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                81.3640(10)
_cell_angle_beta                 85.9170(10)
_cell_angle_gamma                75.3270(10)
_cell_formula_units_Z            2
_cell_length_a                   7.21830(10)
_cell_length_b                   11.1905(2)
_cell_length_c                   18.6492(3)
_cell_measurement_reflns_used    10385
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.0430
_cell_measurement_theta_min      4.1230
_cell_volume                     1439.90(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 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 0.989
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w     58.00 102.00   0.50    0.05    --   76.88  15.00 -60.00   88
  2  \w     89.00 119.00   0.50    0.05    --   76.88  15.00   0.00   60
  3  \w     46.00  71.00   0.50    0.05    --   76.88  15.00   0.00   50
  4  \w     22.00  47.00   0.50    0.05    --   58.63-126.00 120.00   50
  5  \w     67.00  92.00   0.50    0.05    --   80.80-105.00 100.55   50
  6  \w     45.00  98.00   0.50    0.05    --   80.80-115.00 -36.34  106
  7  \w     47.00  73.00   0.50    0.05    --   58.63-126.00 -90.00   52
  8  \w    -68.00 -31.00   0.50    0.05    --  -60.27 -15.00 -90.00   74
  9  \w   -105.00 -45.00   0.50    0.05    --  -69.75 -15.00-150.00  120
 10  \w   -106.00 -49.00   0.50    0.05    --  -60.27 -15.00-180.00  114
 11  \w   -106.00 -74.00   0.50    0.05    --  -60.27 -15.00 -90.00   64
 12  \w   -117.00 -92.00   0.50    0.05    --  -69.75 -15.00 -60.00   50
 13  \w    -73.00 -46.00   0.50    0.05    --  -75.18 -15.00 -90.00   54
 14  \w    -64.00 -37.00   0.50    0.05    --  -69.75 -15.00 -60.00   54
 15  \w   -111.00 -58.00   0.50    0.05    --  -75.18 -15.00   0.00  106
 16  \w   -119.00 -47.00   0.50    0.05    --  -75.18 -15.00  60.00  144
 17  \w   -100.00 -47.00   0.50    0.05    --  -75.18 -15.00 120.00  106
 18  \w    -90.00 -64.00   0.50    0.05    --  -69.75 -15.00 150.00   52
 19  \w    -70.00 -40.00   0.50    0.05    --  -75.18 112.00 -30.00   60
 20  \w   -101.00 -55.00   0.50    0.05    --  -78.50 129.00   3.29   92
 21  \w   -102.00 -35.00   0.50    0.05    --  -78.50 129.00 -23.45  134
 22  \w    -98.00 -72.00   0.50    0.05    --  -78.50 121.00-127.81   52
 23  \w    -94.00 -35.00   0.50    0.05    --  -69.75 126.00  30.00  118
 24  \w    -62.00 -36.00   0.50    0.05    --  -69.75 126.00  90.00   52
 25  \w    -61.00 -35.00   0.50    0.05    --  -78.50 127.00 116.27   52
 26  \w    -97.00 -46.00   0.50    0.05    --  -78.50 120.00 151.11  102
 27  \w   -100.00 -71.00   0.50    0.05    --  -78.50 127.00 116.27   58
 28  \w    -96.00 -40.00   0.50    0.05    --  -78.50 116.00  70.06  112
 29  \w    -95.00 -69.00   0.50    0.05    --  -78.50 116.00  97.18   52
 30  \w    -87.00 -33.00   0.50    0.05    --  -75.18 112.00 120.00  108
 31  \w    -97.00 -48.00   0.50    0.05    --  -78.50 120.00 -68.27   98
 32  \w    -64.00 -38.00   0.50    0.05    --  -75.18 112.00 -60.00   52
 33  \w    -64.00 -38.00   0.50    0.05    --  -78.50 121.00-127.81   52
 34  \w    -78.00 -34.00   0.50    0.05    --  -75.18 112.00-150.00   88
 35  \w    -95.00 -43.00   0.50    0.05    --  -78.50 119.00-175.84  104
;
_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      0.1093263000
_diffrn_orient_matrix_UB_12      -0.0192810000
_diffrn_orient_matrix_UB_13      0.0704816000
_diffrn_orient_matrix_UB_21      -0.1671684000
_diffrn_orient_matrix_UB_22      0.0941143000
_diffrn_orient_matrix_UB_23      0.0323799000
_diffrn_orient_matrix_UB_31      -0.0939856000
_diffrn_orient_matrix_UB_32      -0.1068145000
_diffrn_orient_matrix_UB_33      0.0312031000
_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  0.0276
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16901
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.615
_diffrn_reflns_theta_min         4.123
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    0.883
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80514
_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    1.191
_exptl_crystal_description       plate
_exptl_crystal_F_000             548
_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          0.290
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         5434
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0485P)^2^+0.3994P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1016
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4813
_reflns_number_total             5434
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc08526h2.cif
_cod_data_source_block           E-7Ph
_cod_database_code               1576370
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.784
_shelx_estimated_absorpt_t_max   0.957
_shelx_res_checksum              31621