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_7715771
_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         'C66 H10 B4 F40, 2.5(C6 H6)'
_chemical_formula_sum            'C81 H25 B4 F40'
_chemical_formula_weight         1801.25
_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             2020-07-10
_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                80.332(5)
_cell_angle_beta                 71.304(6)
_cell_angle_gamma                69.470(6)
_cell_formula_units_Z            2
_cell_length_a                   12.7646(9)
_cell_length_b                   16.0907(10)
_cell_length_c                   19.4943(13)
_cell_measurement_reflns_used    4881
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      74.0930
_cell_measurement_theta_min      2.9040
_cell_volume                     3544.8(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (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 0.991
_diffrn_measured_fraction_theta_max 0.962
_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    -87.00 -18.00   1.00   30.00    --  -38.50 125.00-180.00   69
  2  \w   -109.00 -21.00   1.00   30.00    --  -38.50 -38.00 -60.00   88
  3  \w    -63.00  38.00   1.00   30.00    --  -38.50  19.00 120.00  101
  4  \w    -63.00 -11.00   1.00   30.00    --  -38.50 125.00  90.00   52
  5  \w     61.00  96.00   1.00   30.00    --   42.89-125.00-180.00   35
  6  \w     67.00 112.00   1.00   30.00    --  106.24-125.00  60.00   45
  7  \w    131.00 157.00   1.00   30.00    --  106.24 125.00   0.00   26
  8  \w     35.00 127.00   1.00   30.00    --  106.24 -30.00  90.00   92
  9  \w     80.00 106.00   1.00   30.00    --  106.24 -94.00 -90.00   26
 10  \w     45.00 106.00   1.00   30.00    --  106.24 -94.00 150.00   61
 11  \w     90.00 175.00   1.00   30.00    --  106.24  45.00  30.00   85
 12  \w     52.00 107.00   1.00   30.00    --  106.24 -94.00-150.00   55
 13  \w     68.00 112.00   1.00   30.00    --  106.24-125.00 150.00   44
 14  \w     30.00 141.00   1.00   30.00    --  106.24 -15.00-150.00  111
 15  \w     27.00 105.00   1.00   30.00    --  106.24 -94.00  60.00   78
 16  \w     41.00 131.00   1.00   30.00    --  106.24 -61.00-120.00   90
 17  \w     43.00 122.00   1.00   30.00    --  106.24 -30.00   0.00   79
;
_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      0.0887016000
_diffrn_orient_matrix_UB_12      0.0019928000
_diffrn_orient_matrix_UB_13      0.0373114000
_diffrn_orient_matrix_UB_21      -0.0243648000
_diffrn_orient_matrix_UB_22      -0.0783474000
_diffrn_orient_matrix_UB_23      0.0525824000
_diffrn_orient_matrix_UB_31      0.0979686000
_diffrn_orient_matrix_UB_32      -0.0659614000
_diffrn_orient_matrix_UB_33      -0.0532041000
_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  0.0853
_diffrn_reflns_av_unetI/netI     0.0664
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25292
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.137
_diffrn_reflns_theta_min         2.938
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.545
_exptl_absorpt_correction_T_max  0.85137
_exptl_absorpt_correction_T_min  0.84978
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_description       plate
_exptl_crystal_F_000             1782
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.144
_exptl_crystal_size_min          0.043
_exptl_crystal_size_rad          0.070
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       0.00066(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1128
_refine_ls_number_reflns         14816
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.944
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0592
_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^)+(0.1027P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1479
_refine_ls_wR_factor_ref         0.1563
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10457
_reflns_number_total             14816
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9746\% 
around [-0.00 -0.00 1.00] (reciprocal) or [-0.42 -0.07 0.91] (direct)
;
_cod_data_source_file            d4dt00782d2.cif
_cod_data_source_block           4d
_cod_depositor_comments
'Adding full bibliography for 7715770--7715781.cif.'
_cod_database_code               7715771
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C81H25B4F40
_shelx_estimated_absorpt_t_max   0.937
_shelx_estimated_absorpt_t_min   0.646
_diffrn_oxdiff_digest_frames
;
016228cc1fddda8a03cd02aff376df1d87011375134
;
_diffrn_oxdiff_digest_hkl
;
013eb8c1fa3947f6fdd3a3365643270599f5bf
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6029(10)
 0.3971(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7), C8(H8), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C17(H17), C67(H67), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72),
  C73(H73), C74(H74), C75(H75), C76(H76), C77(H77), C78(H78), C79(H79),
 C80(H80), C81(H81)
;
_shelx_res_checksum              86583
_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 4.552
_oxdiff_exptl_absorpt_empirical_full_min 0.269
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2