Boroles from alumoles: accessing boroles with alkyl-substituted backbones <i>via</i> transtrielation.
Bohlen, Josina L.; Endres, Lukas; Drescher, Regina; Radacki, Krzysztof; Dietz, Maximilian; Krummenacher, Ivo; Braunschweig, Holger; Chemical science 14 (2023) 9010–9015; doi:10.1039/d3sc02668j

data_1569552
_publ_section_title
;
 Boroles from alumoles: accessing boroles with alkyl-substituted backbones
 <i>via</i> transtrielation.
;
_journal_issue                   34
_journal_name_full               'Chemical science'
_journal_page_first              9010
_journal_page_last               9015
_journal_paper_doi               10.1039/d3sc02668j
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C38 H56 B N'
_chemical_formula_sum            'C38 H56 B N'
_chemical_formula_weight         537.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-02-27
_audit_creation_method           'CIF-fill 1.3q (K.Radacki, 2005-22)'
_audit_update_record
;
2023-05-15 deposited with the CCDC.	2023-07-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.4760(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9907(2)
_cell_length_b                   10.55440(10)
_cell_length_c                   18.3576(2)
_cell_measurement_reflns_used    14735
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.6260
_cell_measurement_theta_min      4.8340
_cell_volume                     3271.00(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.68a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.68a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.68a (Rigaku OD, 2022)'
_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 0.994
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w   -122.00 -93.00   0.50    0.36    --  -79.50 -48.00 177.34   58
  2  \w   -128.00 -98.00   0.50    0.36    --  -79.50 -52.00 142.79   60
  3  \w   -101.00 -69.00   0.50    0.36    --  -54.00 -52.00 -11.07   64
  4  \w   -124.00 -99.00   0.50    0.36    --  -79.50 -65.00 -72.76   50
  5  \w   -107.00 -75.00   0.50    0.36    --  -62.00 -52.00-137.20   64
  6  \w    -68.00 -39.00   0.50    0.36    --  -22.00 -48.00-107.93   58
  7  \w    -78.00 -52.00   0.50    0.36    --  -79.50 111.00 -50.39   52
  8  \w    -85.00 -60.00   0.50    0.36    --  -69.45 130.00-132.00   50
  9  \w    -54.00 -20.00   0.50    0.36    --  -59.96 130.00-132.00   68
 10  \w    -61.00 -35.00   0.50    0.36    --  -76.35 130.00-132.00   52
 11  \w   -101.00 -67.00   0.50    0.36    --  -76.35 130.00-132.00   68
 12  \w    -97.00 -66.00   0.50    0.36    --  -78.00 114.00 130.94   62
 13  \w   -124.00 -98.00   0.50    0.36    --  -79.50-120.00 103.62   52
 14  \w     25.00  70.00   0.50    0.36    --   58.28-130.00 155.00   90
 15  \w     38.00  63.00   0.50    0.36    --   71.14-130.00 155.00   50
 16  \w     36.00  62.00   0.50    0.36    --   82.28-130.00 155.00   52
 17  \w     72.00  97.00   0.50    0.36    --   82.28-130.00 155.00   50
 18  \w     46.00 100.00   0.50    0.36    --   85.25-123.00 167.39  108
 19  \w     57.00  98.00   0.50    0.36    --   85.25-133.00 127.48   82
 20  \w     42.00  69.00   0.50    0.36    --   85.25-128.00 -20.28   54
 21  \w     62.00  99.00   0.50    0.36    --   85.25-121.00 -66.70   74
 22  \w     40.00  87.00   0.50    0.36    --   85.25-137.00-103.96   94
 23  \w     48.00  81.00   0.50    0.36    --   85.25-128.00-133.48   66
 24  \w     51.00  93.00   0.50    0.36    --   85.25-102.00-172.64   84
 25  \w     39.00  92.00   0.50    0.36    --   82.28-112.00-180.00  106
 26  \w     64.00  92.00   0.50    0.36    --   85.25-100.00-151.34   56
 27  \w     66.00  92.00   0.50    0.36    --   85.25 -99.00-127.20   52
 28  \w     65.00  91.00   0.50    0.36    --   85.25 -98.00 -63.67   52
 29  \w     65.00  91.00   0.50    0.36    --   85.25-100.00 -70.09   52
 30  \w     43.00  90.00   0.50    0.36    --   82.28 -95.00-120.00   94
 31  \w     46.00  71.00   0.50    0.36    --   85.25-105.00 -44.53   50
 32  \w     41.00  67.00   0.50    0.36    --   85.25-108.00  -5.32   52
 33  \w     20.00  59.00   0.50    0.36    --   58.28 -95.00  60.00   78
 34  \w     58.00  84.00   0.50    0.36    --   85.25  14.00  65.38   52
 35  \w     99.00 124.00   0.50    0.36    --   85.25  52.00 166.59   50
 36  \w     98.00 131.00   0.50    0.36    --   85.25  57.00  52.78   66
 37  \w     87.00 135.00   0.50    0.36    --   85.25  15.00 116.95   96
 38  \w     99.00 124.00   0.50    0.36    --   85.25  54.00  19.76   50
 39  \w     98.00 128.00   0.50    0.36    --   85.25  14.00  65.38   60
 40  \w     99.00 130.00   0.50    0.36    --   85.25  63.00 -46.56   62
 41  \w    101.00 132.00   0.50    0.36    --   85.25  47.00-106.90   62
 42  \w    102.00 127.00   0.50    0.36    --   85.25  60.00-151.38   50
 43  \w    102.00 127.00   0.50    0.36    --   85.25 116.00 -64.82   50
 44  \w    100.00 127.00   0.50    0.36    --   85.25 134.00  19.78   54
 45  \w    103.00 129.00   0.50    0.36    --   85.25 122.00-145.54   52
;
_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      -0.0055210000
_diffrn_orient_matrix_UB_12      -0.1431105000
_diffrn_orient_matrix_UB_13      -0.0163019000
_diffrn_orient_matrix_UB_21      0.0467705000
_diffrn_orient_matrix_UB_22      -0.0281399000
_diffrn_orient_matrix_UB_23      0.0751334000
_diffrn_orient_matrix_UB_31      -0.0781542000
_diffrn_orient_matrix_UB_32      -0.0066793000
_diffrn_orient_matrix_UB_33      0.0349358000
_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  0.0291
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37012
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.358
_diffrn_reflns_theta_min         4.841
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    0.448
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.775
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.42.68a (Rigaku Oxford Diffraction, 2022) 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            'clear light orange'
_exptl_crystal_density_diffrn    1.092
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_preparation
;
 Crystals were grown from saturated solution of C6D6 at 20 \%C. 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          0.220
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.278
_refine_diff_density_min         -0.198
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         6637
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0586P)^2^+0.8946P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1063
_refine_ls_wR_factor_ref         0.1110
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5692
_reflns_number_total             6637
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02668j2.cif
_cod_data_source_block           5a
_cod_depositor_comments
'Adding full bibliography for 1569551--1569553.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1569552
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.908
_shelx_estimated_absorpt_t_max   0.961
_shelx_res_checksum              81180