The forgotten borole: synthesis, properties and reactivity of a 1-boraindene.
Wieprecht, Nele; Krummenacher, Ivo; Wüst, Leonie; Michel, Maximilian; Fuchs, Sonja; Nees, Samuel; Härterich, Marcel; Braunschweig, Holger; Chemical science 15 (2024) 12496–12501; doi:10.1039/d4sc03817g

data_1572078
_publ_section_title
;
 The forgotten borole: synthesis, properties and reactivity of a
 1-boraindene.
;
_journal_issue                   31
_journal_name_full               'Chemical science'
_journal_page_first              12496
_journal_page_last               12501
_journal_paper_doi               10.1039/d4sc03817g
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C29 H28 B N Si'
_chemical_formula_sum            'C29 H28 B N Si'
_chemical_formula_weight         429.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           'CIF-fill 1.2y (K.Radacki, 2005-22)'
_audit_update_record
;
2024-06-05 deposited with the CCDC.	2024-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.2250(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0612(2)
_cell_length_b                   11.32090(10)
_cell_length_c                   16.7015(2)
_cell_measurement_reflns_used    11540
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.0590
_cell_measurement_theta_min      3.7900
_cell_volume                     2371.20(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 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 HPA
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HyPix Arc150'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 
   # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
 --------------------------------------------------------------------------
   1  \w     63.00  88.00   0.50    0.50    --   50.00  52.00 -87.16   50
   2  \w     98.00 123.00   0.50    0.50    --   85.25  44.00-114.32   50
   3  \w    101.00 127.00   0.50    0.50    --   85.25  34.00-155.00   52
   4  \w     99.00 125.00   0.50    0.50    --   85.25  42.00-148.69   52
   5  \w     98.00 132.00   0.50    0.50    --   82.31  15.00-180.00   68
   6  \w     93.00 136.00   0.50    0.50    --   85.25  23.00 -89.24   86
   7  \w    107.00 133.00   0.50    0.50    --   82.31  15.00-150.00   52
   8  \w    101.00 126.00   0.50    0.50    --   85.25  65.00  -9.12   50
   9  \w     98.00 131.00   0.50    0.50    --   85.25  55.00 108.31   66
  10  \w     99.00 133.00   0.50    0.50    --   85.25  51.00 163.46   68
  11  \w     52.00  84.00   0.50    0.50    --   85.25 -83.00 168.86   64
  12  \w     38.00  63.00   0.50    0.50    --   58.61-129.00 -28.00   50
  13  \w     34.00  88.00   0.50    0.50    --   71.30-129.00 -28.00  108
  14  \w     79.00 104.00   0.50    0.50    --   85.25-137.00 -49.95   50
  15  \w     40.00  74.00   0.50    0.50    --   85.25-137.00 -49.95   68
  16  \w     39.00  65.00   0.50    0.50    --   85.25-136.00-104.66   52
  17  \w     37.00  69.00   0.50    0.50    --   82.31-129.00 -28.00   64
  18  \w     52.00  82.00   0.50    0.50    --   85.25-116.00   6.71   60
  19  \w     37.00  71.00   0.50    0.50    --   85.25-116.00  -1.18   68
  20  \w     72.00  97.00   0.50    0.50    --   85.25-114.00 -31.65   50
  21  \w     39.00  66.00   0.50    0.50    --   85.25-116.00 -27.26   54
  22  \w     71.00  97.00   0.50    0.50    --   82.31-112.00  30.00   52
  23  \w     42.00 101.00   0.50    0.50    --   85.25-124.00 107.87  118
  24  \w     73.00  99.00   0.50    0.50    --   85.25-124.00 147.39   52
  25  \w     38.00  84.00   0.50    0.50    --   85.25-118.00 149.79   92
  26  \w     60.00  97.00   0.50    0.50    --   82.31-112.00 120.00   74
  27  \w     71.00  97.00   0.50    0.50    --   82.31-112.00  90.00   52
  28  \w     42.00  69.00   0.50    0.50    --   82.31 -95.00  60.00   54
  29  \w     40.00  66.00   0.50    0.50    --   85.25-110.00  29.45   52
  30  \w     67.00  93.00   0.50    0.50    --   85.25-110.00  29.45   52
  31  \w     45.00  87.00   0.50    0.50    --   85.25 -94.00  36.27   84
  32  \w     43.00  68.00   0.50    0.50    --   85.25 -93.00  -2.42   50
  33  \w     68.00  94.00   0.50    0.50    --   85.25 -99.00  -4.43   52
  34  \w     67.00  93.00   0.50    0.50    --   85.25 -95.00 -35.13   52
  35  \w     52.00  90.00   0.50    0.50    --   82.31 -95.00 -60.00   76
  36  \w     45.00  70.00   0.50    0.50    --   85.25 -88.00 -80.05   50
  37  \w    104.00 129.00   0.50    0.50    --   85.25 112.00-124.51   50
  38  \w    100.00 133.00   0.50    0.50    --   85.25 119.00-112.12   66
  39  \w    103.00 134.00   0.50    0.50    --   85.25 115.00-101.23   62
  40  \w    104.00 133.00   0.50    0.50    --   85.25 117.00 156.18   58
  41  \w    -57.00 -16.00   0.50    0.50    --  -60.19 129.00  44.00   82
  42  \w    -89.00 -64.00   0.50    0.50    --  -76.37 129.00  44.00   50
  43  \w    -85.00 -60.00   0.50    0.50    --  -69.72 129.00  44.00   50
  44  \w    -95.00 -69.00   0.50    0.50    --  -79.50 107.00  34.05   52
  45  \w    -93.00 -63.00   0.50    0.50    --  -79.50 108.00  -2.22   60
  46  \w    -61.00 -35.00   0.50    0.50    --  -79.50 108.00  -2.22   52
  47  \w   -114.00 -86.00   0.50    0.50    --  -70.00 -59.00 -31.61   56
  48  \w   -121.00 -93.00   0.50    0.50    --  -79.50 -54.00 -10.09   56
  49  \w   -117.00 -84.00   0.50    0.50    --  -70.00 -56.00 140.36   66
  50  \w   -103.00 -72.00   0.50    0.50    --  -58.00 -48.00  -6.32   62
  51  \w   -128.00 -94.00   0.50    0.50    --  -79.50 -52.00 -63.42   68
  52  \w    -97.00 -67.00   0.50    0.50    --  -50.00 -51.00-162.70   60

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-R'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30697
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.218
_diffrn_reflns_theta_min         3.820
_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  0.82569
_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            colourless
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.066
_refine_diff_density_max         0.344
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         4819
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0661P)^2^+0.8981P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1163
_refine_ls_wR_factor_ref         0.1214
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4182
_reflns_number_total             4819
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03817g2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 1572071--1572079.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1572078
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.843
_shelx_estimated_absorpt_t_max   0.935
_shelx_res_checksum              15321