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_1569551
_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         '0.97(C22 H33 B) 0.03(C22 H32 B Br)'
_chemical_formula_sum            'C22 H32.97 B Br0.03'
_chemical_formula_weight         310.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-03-10
_audit_creation_method           'CIF-fill 1.3r (K.Radacki, 2005-23)'
_audit_update_record
;
2023-05-15 deposited with the CCDC.	2023-07-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.359(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.7239(7)
_cell_length_b                   9.0900(5)
_cell_length_c                   11.1927(8)
_cell_measurement_reflns_used    2150
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.3850
_cell_measurement_theta_min      4.5550
_cell_volume                     981.18(11)
_computing_cell_refinement       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_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 0.982
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w     16.00  64.60   0.60    5.00    --   58.57 -95.00 -90.00   81
  2  \w     16.00  64.60   0.60    5.00    --   58.57 -95.00-180.00   81
  3  \w    -88.00 -15.40   0.60    5.00    --  -60.16 126.00-150.00  121
  4  \w    -88.00 -15.40   0.60    5.00    --  -60.16 126.00 -60.00  121
  5  \w     29.00  77.60   0.60    5.00    --   71.34 -95.00  60.00   81
  6  \w     29.00  77.60   0.60    5.00    --   71.34 -95.00 -30.00   81
  7  \w    -92.00 -32.00   0.60    5.00    --  -76.35 112.00 150.00  100
  8  \w   -127.00 -40.00   0.60    5.00    --  -76.35 -15.00 -30.00  145
  9  \w     46.00 133.00   0.60    5.00    --   82.28  15.00-180.00  145
 10  \w     37.00  91.60   0.60    5.00    --   82.28-112.00 -60.00   91
 11  \w     37.00  91.60   0.60    5.00    --   82.28-112.00-180.00   91
 12  \w     37.00  91.60   0.60    5.00    --   82.28-112.00-150.00   91
 13  \w     37.00  91.60   0.60    5.00    --   82.28-112.00 150.00   91
 14  \w     46.00 133.00   0.60    5.00    --   82.28  15.00  90.00  145
 15  \w     45.00  72.00   0.60    5.00    --   82.28 -95.00 -60.00   45
 16  \w     41.00  80.00   0.60    5.00    --   82.28 -95.00-150.00   65
 17  \w     53.00  98.00   0.60    5.00    --   82.28  15.00-120.00   75
 18  \w     40.00  65.20   0.60    5.00    --   82.28 -95.00  60.00   42
 19  \w     47.00  85.40   0.60    5.00    --   82.28-112.00 -90.00   64
 20  \w     53.00  79.40   0.60    5.00    --   82.28 -95.00 -90.00   44
 21  \w     37.00  79.60   0.60    5.00    --   82.28-112.00  90.00   71
;
_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      0.0107011000
_diffrn_orient_matrix_UB_12      -0.0362238000
_diffrn_orient_matrix_UB_13      0.1352619000
_diffrn_orient_matrix_UB_21      0.1198063000
_diffrn_orient_matrix_UB_22      -0.1073284000
_diffrn_orient_matrix_UB_23      -0.0132099000
_diffrn_orient_matrix_UB_31      0.1052288000
_diffrn_orient_matrix_UB_32      0.1259383000
_diffrn_orient_matrix_UB_33      0.0281188000
_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  0.0407
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9056
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.587
_diffrn_reflns_theta_min         4.585
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    0.488
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.959
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.42.84a (Rigaku Oxford Diffraction, 2023) 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 red'
_exptl_crystal_density_diffrn    1.052
_exptl_crystal_description       block
_exptl_crystal_F_000             342
_exptl_crystal_preparation
;
 Crystals were grown from saturated solution of hexane at -30 \%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          0.070
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         2030
_refine_ls_number_restraints     222
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.1138
_refine_ls_R_factor_gt           0.0809
_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^)+(0.1018P)^2^+1.3674P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2164
_refine_ls_wR_factor_ref         0.2398
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1358
_reflns_number_total             2030
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02668j2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 1569551--1569553.cif.'
_cod_original_cell_volume        981.18(12)
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               1569551
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_min   0.967
_shelx_estimated_absorpt_t_max   0.990
_shelx_res_checksum              39104