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_1572076
_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         'C30 H27 B O'
_chemical_formula_sum            'C30 H27 B O'
_chemical_formula_weight         414.32
_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_date             2024-04-10
_audit_creation_method           'CIF-fill 1.4u (K.Radacki, 2005-23)'
_audit_update_record
;
2024-06-05 deposited with the CCDC.	2024-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.511(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9933(2)
_cell_length_b                   12.0387(2)
_cell_length_c                   17.7494(3)
_cell_measurement_reflns_used    10233
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.3090
_cell_measurement_theta_min      4.2370
_cell_volume                     2252.18(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 0.975
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w   -118.00 -86.00   0.50    0.39    --  -69.77 -15.00 -60.00   64
  2  \w    -72.00 -34.00   0.50    0.39    --  -69.77 -15.00 -60.00   76
  3  \w    -71.00 -41.00   0.50    0.39    --  -76.38 -15.00 -30.00   60
  4  \w   -127.00 -77.00   0.50    0.39    --  -76.38 -15.00 -30.00  100
  5  \w   -108.00 -65.00   0.50    0.39    --  -60.28 -15.00  90.00   86
  6  \w   -108.00 -51.00   0.50    0.39    --  -76.38 -15.00-120.00  114
  7  \w   -125.00 -43.00   0.50    0.39    --  -76.38 -15.00-180.00  164
  8  \w    -74.00 -48.00   0.50    0.39    --  -76.38 112.00-180.00   52
  9  \w    -97.00 -33.00   0.50    0.39    --  -79.50 116.00-156.28  128
 10  \w    -97.00 -48.00   0.50    0.39    --  -79.50 116.00  31.76   98
 11  \w    -97.00 -37.00   0.50    0.39    --  -79.50 115.00 132.32  120
 12  \w    -60.00 -31.00   0.50    0.39    --  -76.38 112.00  90.00   58
 13  \w    -55.00 -26.00   0.50    0.39    --  -60.28 126.00  30.00   58
 14  \w     48.00 126.00   0.50    0.39    --   84.40  15.00 120.00  156
 15  \w     48.00 103.00   0.50    0.39    --   84.40  15.00 -90.00  110
 16  \w     65.00 135.00   0.50    0.39    --   84.40  15.00-180.00  140
 17  \w     25.00  51.00   0.50    0.39    --   71.40-126.00-150.00   52
 18  \w     20.00  54.00   0.50    0.39    --   58.64-126.00   0.00   68
 19  \w     31.00  56.00   0.50    0.39    --   71.40 -95.00  60.00   50
 20  \w     30.00  56.00   0.50    0.39    --   71.40 -95.00 120.00   52
 21  \w     32.00  93.00   0.50    0.39    --   76.43-112.00  30.00  122
 22  \w     48.00  93.00   0.50    0.39    --   76.43-112.00 -30.00   90
 23  \w     66.00  92.00   0.50    0.39    --   84.40 -95.00  60.00   52
 24  \w     25.00  52.00   0.50    0.39    --   58.64 -95.00   0.00   54
 25  \w     16.00  55.00   0.50    0.39    --   58.64 -95.00 -60.00   78
 26  \w     16.00  56.00   0.50    0.39    --   58.64 -95.00-150.00   80
 27  \w     65.00  92.00   0.50    0.39    --   84.40 -95.00-180.00   54
 28  \w     66.00  92.00   0.50    0.39    --   84.40 -95.00 -60.00   52
 29  \w     50.00  92.00   0.50    0.39    --   84.40 -95.00 -90.00   84
 30  \w     42.00  74.00   0.50    0.39    --   84.40 -95.00 -30.00   64
 31  \w     67.00  92.00   0.50    0.39    --   84.40 -95.00-120.00   50
 32  \w     63.00  88.00   0.50    0.39    --   84.40 -95.00-150.00   50
 33  \w     51.00  92.00   0.50    0.39    --   84.40 -95.00   0.00   82
 34  \w     42.00  92.00   0.50    0.39    --   84.40 -95.00  30.00  100
 35  \w     46.00  92.00   0.50    0.39    --   84.40 -95.00 120.00   92
;
_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      -0.1315611000
_diffrn_orient_matrix_UB_12      -0.0158334000
_diffrn_orient_matrix_UB_13      -0.0593324000
_diffrn_orient_matrix_UB_21      0.0011947000
_diffrn_orient_matrix_UB_22      -0.1232576000
_diffrn_orient_matrix_UB_23      0.0236733000
_diffrn_orient_matrix_UB_31      -0.0635432000
_diffrn_orient_matrix_UB_32      0.0309284000
_diffrn_orient_matrix_UB_33      0.0641081000
_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  0.0525
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26463
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.946
_diffrn_reflns_theta_min         4.260
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19585
_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 colourless'
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_description       plate
_exptl_crystal_F_000             880
_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          0.310
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.216
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         4516
_refine_ls_number_restraints     220
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0704P)^2^+0.4380P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1189
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3658
_reflns_number_total             4516
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03817g2.cif
_cod_data_source_block           1-THF
_cod_depositor_comments
'Adding full bibliography for 1572071--1572079.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1572076
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.850
_shelx_estimated_absorpt_t_max   0.948
_shelx_res_checksum              24230