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_7715772
_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         'C40 H40 B2 N2'
_chemical_formula_sum            'C40 H40 B2 N2'
_chemical_formula_weight         570.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2021-01-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2024-03-04 deposited with the CCDC.	2024-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.198(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3734(3)
_cell_length_b                   19.5963(5)
_cell_length_c                   15.8553(3)
_cell_measurement_reflns_used    8593
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      76.4320
_cell_measurement_theta_min      3.5840
_cell_volume                     3150.30(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.986
_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    -72.00  39.00   1.00   11.00    --  -38.50  19.00-120.00  111
  2  \w   -110.00 -18.00   1.00   11.00    --  -38.50 -38.00  60.00   92
  3  \w     18.00 111.00   1.00   11.00    --   42.70  57.00   0.00   93
  4  \w     27.00  97.00   1.00   11.00    --   42.70-125.00 -60.00   70
  5  \w     85.00 178.00   1.00   30.00    --  111.00  61.00  60.00   93
  6  \w     32.00 151.00   1.00   30.00    --  111.00 -15.00 150.00  119
  7  \w     97.00 178.00   1.00   30.00    --  111.00 125.00-150.00   81
  8  \w     31.00 107.00   1.00   30.00    --  111.00 -94.00-150.00   76
  9  \w     41.00 113.00   1.00   30.00    --  111.00-125.00-150.00   72
 10  \w     31.00 107.00   1.00   30.00    --  111.00 -94.00-120.00   76
 11  \w     41.00 133.00   1.00   30.00    --  111.00 -45.00 -90.00   92
 12  \w     38.00 132.00   1.00   30.00    --  111.00 -30.00  60.00   94
 13  \w    -59.00  33.00   1.00   11.00    --  -38.50  38.00 120.00   92
 14  \w     18.00 111.00   1.00   11.00    --   42.70  57.00-120.00   93
 15  \w     18.00 111.00   1.00   11.00    --   42.70  57.00-180.00   93
 16  \w     89.00 132.00   1.00   30.00    --  111.00  45.00   0.00   43
 17  \w     71.00 178.00   1.00   30.00    --  111.00  15.00 -60.00  107
 18  \w     71.00 178.00   1.00   30.00    --  111.00  15.00-150.00  107
;
_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      -0.1418175000
_diffrn_orient_matrix_UB_12      -0.0280964000
_diffrn_orient_matrix_UB_13      -0.0170126000
_diffrn_orient_matrix_UB_21      0.0028397000
_diffrn_orient_matrix_UB_22      0.0020456000
_diffrn_orient_matrix_UB_23      0.0975324000
_diffrn_orient_matrix_UB_31      -0.0544074000
_diffrn_orient_matrix_UB_32      0.0733841000
_diffrn_orient_matrix_UB_33      -0.0091546000
_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  0.0408
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30802
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.778
_diffrn_reflns_theta_min         3.636
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.514
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.901
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_description       plate
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.156
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.185
_refine_diff_density_rms         0.034
_refine_ls_extinction_coef       0.00034(8)
_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   1.013
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     558
_refine_ls_number_reflns         6535
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0460P)^2^+0.7857P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.1048
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5057
_reflns_number_total             6535
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00782d2.cif
_cod_data_source_block           3axTMEDA
_cod_depositor_comments
'Adding full bibliography for 7715770--7715781.cif.'
_cod_original_cell_volume        3150.28(13)
_cod_database_code               7715772
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C148 H140 B8 N20 '
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.924
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
;
_shelx_res_checksum              45354
_olex2_date_sample_data_collection 2021-01-12
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.322
_oxdiff_exptl_absorpt_empirical_full_min 0.846