Bidentate boron Lewis acids: synthesis by tin boron exchange reaction and host-guest complex formation.
Beckmann, J. Louis; Neumann, Beate; Stammler, Hans-Georg; Lamm, Jan-Hendrik; Mitzel, Norbert W.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 7958–7964; doi:10.1039/d4dt00782d

data_7715777
_publ_section_title
;
 Bidentate boron Lewis acids: synthesis by tin boron exchange reaction and
 host-guest complex formation.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7958
_journal_page_last               7964
_journal_paper_doi               10.1039/d4dt00782d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C46 H12 B2 F20 N2'
_chemical_formula_sum            'C46 H12 B2 F20 N2'
_chemical_formula_weight         994.20
_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
_audit_creation_date             2024-01-31
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.11.24 svn.r209d9fb2 for OlexSys, GUI svn.r6869)
;
_audit_update_record
;
2024-03-04 deposited with the CCDC.	2024-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.696(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0213(2)
_cell_length_b                   15.6580(3)
_cell_length_c                   26.8420(4)
_cell_measurement_reflns_used    16945
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      75.8320
_cell_measurement_theta_min      3.1780
_cell_volume                     3787.38(12)
_computing_cell_refinement       'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.95a 64-bit (release 03-11-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.970
_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   -112.00 -18.00   1.00   12.00    --  -41.83 -57.00   0.00   94
  2  \w    -91.00 -15.00   1.00   12.00    --  -41.83 -57.00 150.00   76
  3  \w    -87.00  -6.00   1.00   12.00    --  -41.83 125.00  90.00   81
  4  \w    -85.00 -16.00   1.00   12.00    --  -41.83 125.00-120.00   69
  5  \w    -80.00 -10.00   1.00   12.00    --  -41.83 -19.00-180.00   70
  6  \w    -93.00 -10.00   1.00   12.00    --  -41.83 -19.00  60.00   83
  7  \w    -66.00  23.00   1.00   12.00    --  -41.83  57.00  60.00   89
  8  \w   -108.00 -16.00   1.00   12.00    --  -41.83 -57.00 -60.00   92
  9  \w   -102.00 -15.00   1.00   12.00    --  -41.83 -57.00  60.00   87
 10  \w     11.00  42.00   1.00   12.00    --   41.83  79.00-168.06   31
 11  \w      9.00  34.00   1.00   12.00    --   41.83  82.00 137.34   25
 12  \w     10.00  35.00   1.00   12.00    --   41.83  79.00  45.18   25
 13  \w     -9.00  42.00   1.00   12.00    --   41.83 -77.00-150.00   51
 14  \w      9.00  38.00   1.00   12.00    --   41.83  82.00 -33.36   29
 15  \w     12.00  42.00   1.00   12.00    --   41.83  76.00 -83.99   30
 16  \w     52.00  83.00   1.00   48.00    --  111.00 -45.00  30.00   31
 17  \w    125.00 176.00   1.00   48.00    --  111.00  61.00  60.00   51
 18  \w     83.00 111.00   1.00   48.00    --  111.00  61.00  30.00   28
 19  \w    133.00 175.00   1.00   48.00    --  111.00  61.00 150.00   42
 20  \w     83.00 110.00   1.00   48.00    --  111.00  61.00 -30.00   27
 21  \w     83.00 113.00   1.00   48.00    --  111.00  61.00 150.00   30
 22  \w     88.00 147.00   1.00   48.00    --  111.00  45.00  90.00   59
 23  \w    126.00 151.00   1.00   48.00    --  111.00  45.00 -60.00   25
 24  \w     83.00 131.00   1.00   48.00    --  111.00  61.00-150.00   48
 25  \w    139.00 174.00   1.00   48.00    --  111.00  61.00-150.00   35
 26  \w     83.00 110.00   1.00   48.00    --  111.00  61.00  60.00   27
 27  \w     39.00 101.00   1.00   48.00    --  111.00 -94.00-150.00   62
 28  \w     83.00 178.00   1.00   48.00    --  111.00  61.00 -60.00   95
 29  \w     83.00 110.00   1.00   48.00    --  111.00  61.00-180.00   27
 30  \w    127.00 176.00   1.00   48.00    --  111.00  61.00-180.00   49
 31  \w    127.00 178.00   1.00   48.00    --  111.00  61.00-120.00   51
 32  \w    124.00 175.00   1.00   48.00    --  111.00  45.00  30.00   51
 33  \w     83.00 109.00   1.00   48.00    --  111.00  61.00-120.00   26
 34  \w    137.00 177.00   1.00   48.00    --  111.00  61.00 120.00   40
 35  \w     83.00 111.00   1.00   48.00    --  111.00  61.00 120.00   28
 36  \w     84.00 109.00   1.00   48.00    --  111.00-111.00-150.00   25
 37  \w     43.00  77.00   1.00   48.00    --  111.00 -94.00  60.00   34
 38  \w     87.00 166.00   1.00   48.00    --  111.00  45.00-150.00   79
 39  \w     87.00 113.00   1.00   48.00    --  111.00  45.00   0.00   26
 40  \w    117.00 158.00   1.00   48.00    --  111.00  45.00   0.00   41
 41  \w     87.00 152.00   1.00   48.00    --  111.00  45.00 120.00   65
 42  \w     87.00 118.00   1.00   48.00    --  111.00  45.00  30.00   31
 43  \w     42.00 109.00   1.00   48.00    --  111.00-111.00  60.00   67
 44  \w     87.00 119.00   1.00   48.00    --  111.00  45.00 -30.00   32
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0020615000
_diffrn_orient_matrix_UB_12      0.0436147000
_diffrn_orient_matrix_UB_13      0.0514192000
_diffrn_orient_matrix_UB_21      -0.0783390000
_diffrn_orient_matrix_UB_22      -0.0785685000
_diffrn_orient_matrix_UB_23      0.0211085000
_diffrn_orient_matrix_UB_31      0.1519006000
_diffrn_orient_matrix_UB_32      -0.0400065000
_diffrn_orient_matrix_UB_33      0.0146574000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            46095
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.831
_diffrn_reflns_theta_min         3.269
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.535
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.897
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.95a (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 red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         7640
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0483P)^2^+1.3339P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.1022
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6294
_reflns_number_total             7640
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00782d2.cif
_cod_data_source_block           3dxPym
_cod_depositor_comments
'Adding full bibliography for 7715770--7715781.cif.'
_cod_database_code               7715777
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C46 H12 B2 F20 N2'
_shelx_estimated_absorpt_t_max   0.862
_shelx_estimated_absorpt_t_min   0.759
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7), C8(H8), C10(H10), C12(H12), C13(H13), C14(H14),
 C43(H43), C44(H44), C45(H45), C46(H46)
;
_shelx_res_checksum              39243
_olex2_date_sample_data_collection 2024-01-30
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.568
_oxdiff_exptl_absorpt_empirical_full_min 0.702