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_1569553
_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         'C39 H58 B N'
_chemical_formula_sum            'C39 H58 B N'
_chemical_formula_weight         551.67
_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             2023-01-30
_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                 96.4030(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1660(2)
_cell_length_b                   10.52710(10)
_cell_length_c                   18.3364(2)
_cell_measurement_reflns_used    18297
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.9700
_cell_measurement_theta_min      4.8470
_cell_volume                     3292.87(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-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 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w   -120.00 -92.00   0.50    0.20    --  -79.50 -63.00 -51.88   56
  2  \w   -105.00 -80.00   0.50    0.20    --  -62.00 -52.00-112.36   50
  3  \w   -119.00 -93.00   0.50    0.20    --  -79.50 -57.00-131.36   52
  4  \w    -99.00 -68.00   0.50    0.20    --  -54.00 -49.00 -32.95   62
  5  \w   -113.00 -81.00   0.50    0.20    --  -66.00 -47.00  17.19   64
  6  \w   -118.00 -92.00   0.50    0.20    --  -74.00 -56.00-158.03   52
  7  \w   -128.00 -96.00   0.50    0.20    --  -79.50 -50.00-175.53   64
  8  \w    -97.00 -55.00   0.50    0.20    --  -79.50 115.00-161.92   84
  9  \w     -6.00  19.00   0.50    0.20    --  -10.00  78.00 131.87   50
 10  \w    -82.00 -56.00   0.50    0.20    --  -69.76 113.00 -83.00   52
 11  \w    -86.00 -61.00   0.50    0.20    --  -76.35 113.00 -83.00   50
 12  \w    -78.00 -18.00   0.50    0.20    --  -60.16 113.00 -83.00  120
 13  \w   -125.00 -87.00   0.50    0.20    --  -79.50-133.00  14.36   76
 14  \w     46.00 100.00   0.50    0.20    --   85.25-125.00 -25.78  108
 15  \w     41.00  81.00   0.50    0.20    --   85.25-138.00-159.93   80
 16  \w     56.00  97.00   0.50    0.20    --   85.25-114.00-114.56   82
 17  \w     75.00 101.00   0.50    0.20    --   85.25-126.00 -44.84   52
 18  \w     38.00  80.00   0.50    0.20    --   85.25-127.00  95.87   84
 19  \w     43.00  86.00   0.50    0.20    --   85.25-123.00 139.72   86
 20  \w     56.00  82.00   0.50    0.20    --   85.25-119.00 110.25   52
 21  \w     66.00  91.00   0.50    0.20    --   82.28-112.00  90.00   50
 22  \w     37.00  62.00   0.50    0.20    --   82.28-112.00  60.00   50
 23  \w     43.00  69.00   0.50    0.20    --   85.25-112.00 -26.16   52
 24  \w     41.00  66.00   0.50    0.20    --   82.28-113.00-175.00   50
 25  \w     67.00  93.00   0.50    0.20    --   85.25-106.00-166.57   52
 26  \w     47.00  78.00   0.50    0.20    --   71.34-113.00-175.00   62
 27  \w     21.00  46.00   0.50    0.20    --   58.57-113.00-175.00   50
 28  \w     43.00  93.00   0.50    0.20    --   85.25 -97.00-163.82  100
 29  \w     64.00  89.00   0.50    0.20    --   82.28 -95.00-120.00   50
 30  \w     60.00  86.00   0.50    0.20    --   85.25 -85.00-134.88   52
 31  \w     19.00  46.00   0.50    0.20    --   58.57 -95.00 -90.00   54
 32  \w     46.00  71.00   0.50    0.20    --   85.25 -82.00-100.99   50
 33  \w     42.00  70.00   0.50    0.20    --   82.28 -95.00 -30.00   56
 34  \w     44.00  70.00   0.50    0.20    --   85.25 -72.00 -33.40   52
 35  \w     46.00  73.00   0.50    0.20    --   85.25 -85.00   9.40   54
 36  \w     51.00  84.00   0.50    0.20    --   85.25 -88.00  29.57   66
 37  \w     42.00  91.00   0.50    0.20    --   85.25 -99.00 156.61   98
 38  \w     99.00 134.00   0.50    0.20    --   85.25  38.00  11.34   70
 39  \w     98.00 127.00   0.50    0.20    --   85.25  53.00-154.12   58
 40  \w    102.00 128.00   0.50    0.20    --   85.25  56.00 -46.09   52
 41  \w    100.00 128.00   0.50    0.20    --   85.25  64.00 116.39   56
 42  \w    104.00 130.00   0.50    0.20    --   85.25 117.00 157.94   52
 43  \w     92.00 117.00   0.50    0.20    --   85.25 135.00  51.19   50
 44  \w     98.00 123.00   0.50    0.20    --   85.25 122.00  16.76   50
 45  \w     96.00 129.00   0.50    0.20    --   85.25 127.00-108.55   66
;
_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      -0.0360101000
_diffrn_orient_matrix_UB_12      0.0918867000
_diffrn_orient_matrix_UB_13      -0.0598767000
_diffrn_orient_matrix_UB_21      0.0092347000
_diffrn_orient_matrix_UB_22      0.1106791000
_diffrn_orient_matrix_UB_23      0.0554133000
_diffrn_orient_matrix_UB_31      0.0822139000
_diffrn_orient_matrix_UB_32      0.0278270000
_diffrn_orient_matrix_UB_33      -0.0220868000
_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  0.0269
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            36724
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.070
_diffrn_reflns_theta_min         4.852
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    0.457
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.799
_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 orange'
_exptl_crystal_density_diffrn    1.113
_exptl_crystal_description       block
_exptl_crystal_F_000             1216
_exptl_crystal_preparation
;
 Crystals were grown from saturated solution. 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          0.170
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.222
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         6242
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0389
_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^)+(0.0497P)^2^+1.0040P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1016
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5531
_reflns_number_total             6242
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02668j2.cif
_cod_data_source_block           6a
_cod_depositor_comments
'Adding full bibliography for 1569551--1569553.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1569553
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_min   0.926
_shelx_estimated_absorpt_t_max   0.973
_shelx_res_checksum              9606