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_7715781
_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         'C36 H38 B2 N2'
_chemical_formula_sum            'C36 H38 B2 N2'
_chemical_formula_weight         520.365
_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'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-01
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2024.02.25 svn.r851e31b8 for OlexSys, GUI svn.r6933)
;
_audit_update_record
;
2024-03-04 deposited with the CCDC.	2024-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.959(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8924(3)
_cell_length_b                   16.8358(3)
_cell_length_c                   16.0803(3)
_cell_measurement_reflns_used    26180
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      36.3860
_cell_measurement_theta_min      2.7320
_cell_volume                     3006.55(12)
_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 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 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 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9936
_diffrn_measured_fraction_theta_max 0.9608
_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    -19.00  58.00   1.00   32.00    --   35.84 -38.00  60.00   77
  2  \w     -5.00  76.00   1.00   32.00    --   35.84 -99.00  60.00   81
  3  \w     17.00 104.00   1.00   32.00    --   35.84  57.00 120.00   87
  4  \w     15.00  55.00   1.00   32.00    --   35.84  38.00 -30.00   40
  5  \w      2.00  31.00   1.00   32.00    --   35.84  87.00  64.09   29
  6  \w      2.00  31.00   1.00   32.00    --   35.84  86.00-131.73   29
  7  \w    -33.00  41.00   1.00   32.00    --   35.84 -57.00 -30.00   74
  8  \w    -13.00  76.00   1.00   32.00    --   35.84 -99.00-150.00   89
  9  \w      8.00  36.00   1.00   32.00    --   35.84  75.00-171.99   28
 10  \w     -2.00  98.00   1.00   32.00    --   35.84  19.00 -90.00  100
 11  \w    -29.00  64.00   1.00   32.00    --   35.84 -77.00 -90.00   93
 12  \w      6.00  42.00   1.00   32.00    --   35.84  80.00 -22.35   36
 13  \w     17.00 106.00   1.00   32.00    --   35.84  46.00  56.00   89
 14  \w      4.00  91.00   1.00   32.00    --   35.84  19.00  30.00   87
 15  \w      2.00  30.00   1.00   32.00    --   35.84  86.00 -75.35   28
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0041900000
_diffrn_orient_matrix_UB_12      -0.0230400000
_diffrn_orient_matrix_UB_13      -0.0379487000
_diffrn_orient_matrix_UB_21      -0.0628077000
_diffrn_orient_matrix_UB_22      0.0075225000
_diffrn_orient_matrix_UB_23      -0.0183732000
_diffrn_orient_matrix_UB_31      0.0108792000
_diffrn_orient_matrix_UB_32      0.0344644000
_diffrn_orient_matrix_UB_33      -0.0212966000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.9936
_diffrn_reflns_Laue_measured_fraction_max 0.9608
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            95727
_diffrn_reflns_point_group_measured_fraction_full 0.9936
_diffrn_reflns_point_group_measured_fraction_max 0.9608
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         36.87
_diffrn_reflns_theta_min         2.77
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.454
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (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    1.150
_exptl_crystal_description       block
_exptl_crystal_F_000             1112.340
_exptl_crystal_size_max          0.326
_exptl_crystal_size_mid          0.311
_exptl_crystal_size_min          0.178
_refine_diff_density_max         0.3759
_refine_diff_density_min         -0.2401
_refine_diff_density_rms         0.0554
_refine_ls_d_res_high            0.5922
_refine_ls_d_res_low             7.3428
_refine_ls_goodness_of_fit_ref   1.0827
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     703
_refine_ls_number_reflns         14575
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0827
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          -0.0004
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0193P)^2^+0.2498P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0680
_refine_ls_wR_factor_ref         0.0751
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              18
_reflns_limit_h_min              -19
_reflns_limit_k_max              28
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                11136
_reflns_number_total             14575
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt00782d2.cif
_cod_data_source_block           3cx2Py
_cod_depositor_comments
'Adding full bibliography for 7715770--7715781.cif.'
_cod_database_code               7715781
_chemical_oxdiff_formula         'C144 H152 B8 N8 '
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     35.41
_olex2_refinement_description
;
;
_olex2_refine_details
;
Refinement using NoSpherA2, an implementation of
NOn-SPHERical Atom-form-factors in Olex2.
Please cite:
F. Kleemiss et al. Chem. Sci. DOI 10.1039/D0SC05526C - 2021
NoSpherA2 implementation of HAR makes use of
tailor-made aspherical atomic form factors calculated
on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from
spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF
wavefunction - either Hartree-Fock or DFT using selected funtionals
 - for a fragment of the crystal.
This fragment can be embedded in an electrostatic crystal field by employing cluster charges
or modelled using implicit solvation models, depending on the software used.
The following options were used:
   SOFTWARE:       ORCA 5.0
   PARTITIONING:   NoSpherA2
   INT ACCURACY:   Normal
   METHOD:         M062X
   BASIS SET:      def2-TZVPP
   CHARGE:         0
   MULTIPLICITY:   1
   DATE:           2024-02-28_16-03-23
;
_olex2_date_sample_data_collection 2021-04-08
_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 1.088
_oxdiff_exptl_absorpt_empirical_full_min 0.897