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_7715774
_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         'C52 H18 B2 F20 N2, C6 H6'
_chemical_formula_sum            'C58 H24 B2 F20 N2'
_chemical_formula_weight         1150.41
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-27
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2024-03-04 deposited with the CCDC.	2024-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                105.644(5)
_cell_angle_beta                 96.165(5)
_cell_angle_gamma                108.009(5)
_cell_formula_units_Z            2
_cell_length_a                   11.3707(7)
_cell_length_b                   12.0641(7)
_cell_length_c                   19.7225(10)
_cell_measurement_reflns_used    3373
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      76.1390
_cell_measurement_theta_min      3.9730
_cell_volume                     2423.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.77a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.77a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.77a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -59.00  32.00   1.00    5.00    --  -38.50  38.00-120.00   91
  2  \w    -56.00  24.00   1.00    5.00    --  -38.50  38.00 150.00   80
  3  \w    -54.00 -24.00   1.00    5.00    --  -38.50 -19.00 -60.00   30
  4  \w     18.00  44.00   1.00    5.00    --   42.89  57.00   0.00   26
  5  \w     13.00  42.00   1.00    5.00    --   42.89  82.00   0.18   29
  6  \w     50.00  81.00   1.00    5.00    --   42.89  57.00  90.00   31
  7  \w     22.00  59.00   1.00    5.00    --   42.89  38.00   0.00   37
  8  \w     15.00  42.00   1.00    5.00    --   42.89  78.00 -80.18   27
  9  \w     23.00  49.00   1.00    5.00    --   42.89  38.00  90.00   26
 10  \w     38.00  87.00   1.00    5.00    --   42.89-122.00 -45.00   49
 11  \w     49.00  87.00   1.00    5.00    --   42.89  57.00   0.00   38
 12  \w     82.00 108.00   1.00   20.00    --  111.00  73.00  36.17   26
 13  \w     82.00 108.00   1.00   20.00    --  111.00  72.00 -54.99   26
 14  \w    120.00 178.00   1.00   20.00    --  111.00  73.00  36.17   58
 15  \w     88.00 176.00   1.00   20.00    --  111.00  47.00   8.66   88
 16  \w     86.00 112.00   1.00   20.00    --  111.00  57.00 -10.69   26
 17  \w    142.00 168.00   1.00   20.00    --  111.00  57.00 -79.15   26
 18  \w    151.00 176.00   1.00   20.00    --  111.00  56.00  11.94   25
 19  \w    127.00 153.00   1.00   20.00    --  111.00  45.00 -90.00   26
 20  \w     91.00 177.00   1.00   20.00    --  111.00  43.00 -48.41   86
 21  \w     89.00 115.00   1.00   20.00    --  111.00  45.00 -90.00   26
 22  \w     77.00 104.00   1.00   20.00    --  111.00 -94.00  30.00   27
 23  \w     41.00 112.00   1.00   20.00    --  111.00-125.00 150.00   71
 24  \w     74.00 136.00   1.00   20.00    --  111.00 -61.00 -60.00   62
 25  \w     85.00 111.00   1.00   20.00    --  111.00  61.00  30.00   26
 26  \w     85.00 111.00   1.00   20.00    --  111.00  61.00 -90.00   26
 27  \w     91.00 116.00   1.00   20.00    --  111.00  45.00  30.00   25
 28  \w     85.00 110.00   1.00   20.00    --  111.00  61.00 -60.00   25
 29  \w     46.00 130.00   1.00   20.00    --  111.00 -45.00  90.00   84
 30  \w     86.00 112.00   1.00   20.00    --  111.00  61.00-120.00   26
 31  \w    139.00 164.00   1.00   20.00    --  111.00  67.00 -33.80   25
 32  \w     88.00 114.00   1.00   20.00    --  111.00  57.00 -79.15   26
 33  \w     92.00 118.00   1.00   20.00    --  111.00  45.00 -30.00   26
 34  \w     91.00 117.00   1.00   20.00    --  111.00  45.00 -60.00   26
 35  \w     58.00 100.00   1.00   20.00    --  111.00 -94.00 -30.00   42
 36  \w     83.00 109.00   1.00   20.00    --  111.00  67.00 -33.80   26
 37  \w     90.00 116.00   1.00   20.00    --  111.00  30.00   0.00   26
 38  \w     89.00 115.00   1.00   20.00    --  111.00  61.00  60.00   26
 39  \w     92.00 145.00   1.00   20.00    --  111.00  30.00 -60.00   53
 40  \w     90.00 116.00   1.00   20.00    --  111.00  30.00  60.00   26
 41  \w     95.00 121.00   1.00   20.00    --  111.00  45.00-120.00   26
 42  \w     89.00 122.00   1.00   20.00    --  111.00  45.00   0.00   33
 43  \w    124.00 149.00   1.00   20.00    --  111.00  45.00   0.00   25
 44  \w     89.00 116.00   1.00   20.00    --  111.00  45.00  90.00   27
 45  \w     87.00 113.00   1.00   20.00    --  111.00  61.00   0.00   26
 46  \w     84.00 111.00   1.00   20.00    --  111.00  66.00  43.36   27
 47  \w     82.00 107.00   1.00   20.00    --  111.00  74.00  24.58   25
 48  \w     84.00 110.00   1.00   20.00    --  111.00  63.00 -56.11   26
 49  \w     87.00 113.00   1.00   20.00    --  111.00  61.00 -30.00   26
 50  \w     86.00 112.00   1.00   20.00    --  111.00  56.00  11.94   26
 51  \w    -44.00 -18.00   1.00    5.00    --  -38.50 -38.00 -30.00   26
 52  \w   -102.00 -76.00   1.00    5.00    --  -38.50 -38.00  60.00   26
 53  \w    -38.00 -11.00   1.00    5.00    --  -38.50 125.00-120.00   27
 54  \w    -99.00 -73.00   1.00    5.00    --  -38.50 -38.00 -30.00   26
 55  \w     69.00  97.00   1.00    5.00    --   42.89-125.00 -90.00   28
 56  \w    113.00 166.00   1.00   20.00    --  111.00 125.00-150.00   53
 57  \w     72.00  98.00   1.00   20.00    --  111.00-125.00-150.00   26
 58  \w     70.00 109.00   1.00   20.00    --  111.00-112.00 -37.56   39
 59  \w     62.00  92.00   1.00   20.00    --  111.00 -94.00-150.00   30
 60  \w     88.00 113.00   1.00   20.00    --  111.00-125.00  30.00   25
 61  \w     45.00  72.00   1.00   20.00    --  111.00-125.00  30.00   27
 62  \w     59.00 109.00   1.00   20.00    --  111.00-108.00 -74.76   50
 63  \w     85.00 110.00   1.00   20.00    --  111.00-115.00 129.00   25
 64  \w    147.00 173.00   1.00   20.00    --  111.00  77.00-180.00   26
 65  \w     78.00 107.00   1.00   20.00    --  111.00-102.00 138.43   29
;
_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      -0.0187098000
_diffrn_orient_matrix_UB_12      -0.0190757000
_diffrn_orient_matrix_UB_13      -0.0814111000
_diffrn_orient_matrix_UB_21      0.1438904000
_diffrn_orient_matrix_UB_22      0.0594692000
_diffrn_orient_matrix_UB_23      0.0081083000
_diffrn_orient_matrix_UB_31      0.0127474000
_diffrn_orient_matrix_UB_32      -0.1272443000
_diffrn_orient_matrix_UB_33      -0.0135992000
_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  0.1250
_diffrn_reflns_av_unetI/netI     0.1332
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32253
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         4.001
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.289
_exptl_absorpt_correction_T_max  0.90301
_exptl_absorpt_correction_T_min  0.90301
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.77a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_description       plate
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.256
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.026
_exptl_crystal_size_rad          0.052
_refine_diff_density_max         0.286
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     827
_refine_ls_number_reflns         8872
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1279
_refine_ls_R_factor_gt           0.0632
_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^)+(0.0445P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1344
_refine_ls_wR_factor_ref         0.1731
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4899
_reflns_number_total             8872
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00782d2.cif
_cod_data_source_block           3dx2Py
_cod_depositor_comments
'Adding full bibliography for 7715770--7715781.cif.'
_cod_database_code               7715774
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C58H24B2F20N2
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.734
_diffrn_oxdiff_digest_frames
;
013da340ce667e728468c55bfd3bf3f1c3023035bd9
;
_diffrn_oxdiff_digest_hkl
;
0112b5cf0d126f98771e5ec25ff88b652d71fa
;
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid body (RIGU) restrains
 F6, F6B, F7, F7B, F8, F8B, F9, F9B, F10, F10B, C25, C25B, C26, C26B, C27,
 C27B, C28, C28B, C29, C29B, C30, C30B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Others
 Sof(F6B)=Sof(F7B)=Sof(F8B)=Sof(F9B)=Sof(F10B)=Sof(C25B)=Sof(C26B)=Sof(C27B)=
 Sof(C28B)=Sof(C29B)=Sof(C30B)=1-FVAR(1)
 Sof(F6)=Sof(F7)=Sof(F8)=Sof(F9)=Sof(F10)=Sof(C25)=Sof(C26)=Sof(C27)=Sof(C28)=
 Sof(C29)=Sof(C30)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7), C8(H8), C10(H10), C12(H12), C13(H13), C14(H14),
 C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C48(H48), C49(H49), C50(H50),
  C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58)
4.b Fitted hexagon refined as free rotating group:
 C25B(C26B,C27B,C28B,C29B,C30B)
;
_shelx_res_checksum              84029
_olex2_date_sample_data_collection 2020-06-25
_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 2.183
_oxdiff_exptl_absorpt_empirical_full_min 0.464