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_7715776
_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_absolute_configuration unk
_chemical_formula_moiety         'C44 H34 B2 N2'
_chemical_formula_sum            'C44 H34 B2 N2'
_chemical_formula_weight         612.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-04
_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                90
_cell_angle_beta                 101.4546(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.17085(16)
_cell_length_b                   18.4947(2)
_cell_length_c                   16.5929(2)
_cell_measurement_reflns_used    37804
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.1320
_cell_measurement_theta_min      3.5810
_cell_volume                     3359.84(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_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      100.01(10)
_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 0.995
_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   -116.00 -15.00   1.00    7.50    --  -38.50 -19.00-120.00  101
  2  \w    -53.00  33.00   1.00    7.50    --  -38.50  37.00 -60.00   86
  3  \w    -57.00  19.00   1.00    7.50    --  -38.50  37.00-120.00   76
  4  \w    -58.00  31.00   1.00    7.50    --  -38.50  37.00  60.00   89
  5  \w     12.00  39.00   1.00    7.50    --   42.70  80.00 -17.54   27
  6  \w     13.00  40.00   1.00    7.50    --   42.70  77.00 -77.86   27
  7  \w     14.00 112.00   1.00    7.50    --   42.70  70.00 131.72   98
  8  \w     28.00  97.00   1.00    7.50    --   42.70-125.00 -30.00   69
  9  \w     21.00  92.00   1.00    7.50    --   42.70  51.00  10.00   71
 10  \w     13.00  38.00   1.00    7.50    --   42.70  77.00-165.55   25
 11  \w     12.00  42.00   1.00    7.50    --   42.70  82.00 103.72   30
 12  \w     13.00  42.00   1.00    7.50    --   42.70  80.00-136.67   29
 13  \w     75.00 103.00   1.00    7.50    --   42.70  57.00  90.00   28
 14  \w     22.00  75.00   1.00    7.50    --   42.70  37.00 -90.00   53
 15  \w     22.00  64.00   1.00    7.50    --   42.70  57.00 -60.00   42
 16  \w     11.00  38.00   1.00    7.50    --   42.70  81.00  34.29   27
 17  \w      7.00  67.00   1.00    7.50    --   42.70 -99.00 120.00   60
 18  \w     18.00  59.00   1.00    7.50    --   42.70  57.00  90.00   41
 19  \w     84.00 178.00   1.00   31.50    --  111.00  66.00 121.95   94
 20  \w     85.00 113.00   1.00   31.50    --  111.00  61.00 -65.58   28
 21  \w     85.00 112.00   1.00   31.50    --  111.00  62.00 141.26   27
 22  \w    128.00 155.00   1.00   31.50    --  111.00  61.00 -10.95   27
 23  \w     84.00 110.00   1.00   31.50    --  111.00  64.00  74.93   26
 24  \w     89.00 116.00   1.00   31.50    --  111.00  45.00 -30.00   27
 25  \w    134.00 176.00   1.00   31.50    --  111.00  64.00  74.93   42
 26  \w     87.00 154.00   1.00   31.50    --  111.00  53.00 -67.43   67
 27  \w     42.00  74.00   1.00   31.50    --  111.00-137.00 -92.37   32
 28  \w     95.00 122.00   1.00   31.50    --  111.00-137.00 -92.37   27
 29  \w     54.00 124.00   1.00   31.50    --  111.00-140.00 -36.18   70
 30  \w     59.00 113.00   1.00   31.50    --  111.00-125.00  30.00   54
 31  \w    125.00 176.00   1.00   31.50    --  111.00  65.00 -41.29   51
 32  \w     85.00 112.00   1.00   31.50    --  111.00  61.00 -10.95   27
 33  \w     86.00 113.00   1.00   31.50    --  111.00  58.00 -92.10   27
 34  \w     84.00 111.00   1.00   31.50    --  111.00  65.00 -41.29   27
 35  \w    117.00 145.00   1.00   31.50    --  111.00  58.00 168.29   28
 36  \w     86.00 174.00   1.00   31.50    --  111.00  55.00 178.69   88
 37  \w     86.00 114.00   1.00   31.50    --  111.00  58.00 168.29   28
 38  \w     56.00 137.00   1.00   31.50    --  111.00 -61.00   0.00   81
 39  \w     83.00 109.00   1.00   31.50    --  111.00  68.00  30.98   26
 40  \w     86.00 112.00   1.00   31.50    --  111.00  56.00  28.72   26
 41  \w     86.00 114.00   1.00   31.50    --  111.00  55.00  73.93   28
 42  \w     58.00 137.00   1.00   31.50    --  111.00 -61.00 120.00   79
 43  \w     86.00 176.00   1.00   31.50    --  111.00  61.00 -60.00   90
 44  \w     89.00 118.00   1.00   31.50    --  111.00  45.00 -90.00   29
 45  \w     85.00 112.00   1.00   31.50    --  111.00  61.00   0.00   27
 46  \w     90.00 115.00   1.00   31.50    --  111.00  45.00-150.00   25
 47  \w     44.00 113.00   1.00   31.50    --  111.00-125.00   0.00   69
 48  \w     85.00 111.00   1.00   31.50    --  111.00  61.00-120.00   26
 49  \w    121.00 177.00   1.00   31.50    --  111.00  61.00-120.00   56
 50  \w     85.00 115.00   1.00   31.50    --  111.00  61.00 120.00   30
 51  \w     85.00 178.00   1.00   31.50    --  111.00  61.00  60.00   93
 52  \w     85.00 112.00   1.00   31.50    --  111.00  61.00 -30.00   27
 53  \w     85.00 112.00   1.00   31.50    --  111.00  61.00  90.00   27
 54  \w     90.00 178.00   1.00   31.50    --  111.00  45.00  30.00   88
 55  \w     85.00 123.00   1.00   31.50    --  111.00  61.00 150.00   38
 56  \w     86.00 143.00   1.00   31.50    --  111.00  61.00 -90.00   57
 57  \w     83.00 175.00   1.00   31.50    --  111.00  70.00-160.15   92
 58  \w    151.00 176.00   1.00   31.50    --  111.00  71.00-146.18   25
 59  \w     83.00 110.00   1.00   31.50    --  111.00  69.00 175.00   27
 60  \w     82.00 108.00   1.00   31.50    --  111.00  71.00-146.18   26
 61  \w     42.00 112.00   1.00   31.50    --  111.00-125.00  60.00   70
 62  \w     36.00  61.00   1.00   31.50    --  111.00 -94.00  60.00   25
 63  \w     41.00 113.00   1.00   31.50    --  111.00-125.00-180.00   72
 64  \w     78.00 106.00   1.00   31.50    --  111.00 -94.00  60.00   28
 65  \w     84.00 114.00   1.00   31.50    --  111.00  64.00 -22.39   30
 66  \w     87.00 113.00   1.00   31.50    --  111.00  52.00  60.34   26
 67  \w     86.00 143.00   1.00   31.50    --  111.00  58.00 108.90   57
;
_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      -0.1297677000
_diffrn_orient_matrix_UB_12      -0.0242056000
_diffrn_orient_matrix_UB_13      0.0063614000
_diffrn_orient_matrix_UB_21      0.0080896000
_diffrn_orient_matrix_UB_22      0.0458966000
_diffrn_orient_matrix_UB_23      0.0783473000
_diffrn_orient_matrix_UB_31      -0.0539496000
_diffrn_orient_matrix_UB_32      0.0651270000
_diffrn_orient_matrix_UB_33      -0.0528932000
_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  0.0290
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            65174
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.326
_diffrn_reflns_theta_min         2.717
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.525
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.773
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
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    1.211
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_exptl_crystal_size_rad          0.050
_refine_diff_density_max         0.527
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.4(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     891
_refine_ls_number_reflns         13796
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0687
_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^)+(0.0880P)^2^+3.0439P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1791
_refine_ls_wR_factor_ref         0.1800
_reflns_Friedel_coverage         0.907
_reflns_Friedel_fraction_full    0.984
_reflns_Friedel_fraction_max     0.963
_reflns_number_gt                13520
_reflns_number_total             13796
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00782d2.cif
_cod_data_source_block           3ax2Py
_cod_depositor_comments
'Adding full bibliography for 7715770--7715781.cif.'
_cod_original_cell_volume        3359.85(8)
_cod_database_code               7715776
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C44H34B2N2
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.921
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     42.10
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6(7)
 0.4(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C62B) = Uanis(C62A)
Uanis(C67B) = Uanis(C67A)
Uanis(C68A) = Uanis(C68B)
Uanis(C61A) = Uanis(C61B)
Uanis(C63A) = Uanis(C63B)
Uanis(C64A) = Uanis(C64B)
Uanis(C65B) = Uanis(C65A)
Uanis(C66B) = Uanis(C66A)
4. Others
 Sof(C61B)=Sof(H61C)=Sof(H61D)=Sof(C62B)=Sof(C63B)=Sof(H63B)=Sof(C64B)=
 Sof(H64B)=Sof(C65B)=Sof(H65B)=Sof(C66B)=Sof(H66B)=Sof(C67B)=Sof(C68B)=
 Sof(H68C)=Sof(H68D)=1-FVAR(1)
 Sof(C61A)=Sof(H61A)=Sof(H61B)=Sof(C62A)=Sof(C63A)=Sof(H63A)=Sof(C64A)=
 Sof(H64A)=Sof(C65A)=Sof(H65A)=Sof(C66A)=Sof(H66A)=Sof(C67A)=Sof(C68A)=
 Sof(H68A)=Sof(H68B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C24(H24A,H24B), C32(H32A,H32B), C39(H39A,H39B), C61A(H61A,
 H61B), C61B(H61C,H61D), C68A(H68A,H68B), C68B(H68C,H68D), C76(H76A,H76B),
 C83(H83A,H83B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7), C8(H8), C10(H10), C12(H12), C13(H13), C14(H14),
 C19(H19), C20(H20), C21(H21), C22(H22), C25(H25), C26(H26), C27(H27), C28(H28),
  C29(H29), C34(H34), C35(H35), C36(H36), C37(H37), C40(H40), C41(H41),
 C42(H42), C43(H43), C44(H44), C47(H47), C50(H50), C51(H51), C52(H52), C54(H54),
  C56(H56), C57(H57), C58(H58), C63A(H63A), C63B(H63B), C64A(H64A), C64B(H64B),
 C65A(H65A), C65B(H65B), C66A(H66A), C66B(H66B), C69(H69), C70(H70), C71(H71),
 C72(H72), C73(H73), C78(H78), C79(H79), C80(H80), C81(H81), C84(H84), C85(H85),
  C86(H86), C87(H87), C88(H88)
;
_shelx_res_checksum              54033
_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 1.121
_oxdiff_exptl_absorpt_empirical_full_min 0.870