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_7715778
_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         'C30 H32 B2 N2, C6 H6'
_chemical_formula_sum            'C36 H38 B2 N2'
_chemical_formula_weight         520.30
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-01
_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                 103.080(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.53870(10)
_cell_length_b                   20.1073(2)
_cell_length_c                   14.4086(2)
_cell_measurement_reflns_used    26703
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.7800
_cell_measurement_theta_min      3.7800
_cell_volume                     2974.04(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.104a (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      100.00(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   -110.00 -18.00   1.00    1.50    --  -38.50 -37.00 -30.00   92
  2  \w    -64.00  30.00   1.00    1.50    --  -38.50  57.00 150.00   94
  3  \w    -21.00  73.00   1.00    1.50    --   42.70 -77.00   0.00   94
  4  \w     12.00  42.00   1.00    1.50    --   42.70  80.00-168.23   30
  5  \w     18.00 111.00   1.00    1.50    --   42.70  57.00  30.00   93
  6  \w     12.00  42.00   1.00    1.50    --   42.70  78.00-122.42   30
  7  \w     11.00  42.00   1.00    1.50    --   42.70  81.00 -63.47   31
  8  \w     11.00  42.00   1.00    1.50    --   42.70  82.00  99.97   31
  9  \w     18.00 111.00   1.00    1.50    --   42.70  57.00-180.00   93
 10  \w     15.00 112.00   1.00    1.50    --   42.70  68.00  82.62   97
 11  \w      9.00 120.00   1.00    1.50    --   42.70  19.00 -90.00  111
 12  \w     15.00 112.00   1.00    1.50    --   42.70  67.00 -79.15   97
 13  \w    -21.00  73.00   1.00    1.50    --   42.70 -77.00-120.00   94
 14  \w     14.00 112.00   1.00    1.50    --   42.70  70.00 119.21   98
 15  \w      4.00  80.00   1.00    1.50    --   42.70 -97.00 158.00   76
 16  \w     11.00  42.00   1.00    1.50    --   42.70  81.00  -0.63   31
 17  \w     84.00 178.00   1.00    6.50    --  111.00  63.00 111.11   94
 18  \w     83.00 178.00   1.00    6.50    --  111.00  70.00  93.10   95
 19  \w     84.00 178.00   1.00    6.50    --  111.00  66.00-117.70   94
 20  \w     42.00 122.00   1.00    6.50    --  111.00-137.00-136.63   80
 21  \w     83.00 178.00   1.00    6.50    --  111.00  68.00 -83.45   95
 22  \w     85.00 178.00   1.00    6.50    --  111.00  61.00 120.00   93
 23  \w     41.00 113.00   1.00    6.50    --  111.00-125.00  30.00   72
 24  \w     87.00 178.00   1.00    6.50    --  111.00  54.00-123.12   91
 25  \w     85.00 178.00   1.00    6.50    --  111.00  61.00 -90.00   93
 26  \w     84.00 111.00   1.00    6.50    --  111.00  63.00 -59.70   27
 27  \w     85.00 112.00   1.00    6.50    --  111.00  60.00 -45.82   27
 28  \w     86.00 114.00   1.00    6.50    --  111.00  56.00  48.19   28
 29  \w    119.00 150.00   1.00    6.50    --  111.00  63.00 128.65   31
 30  \w     84.00 116.00   1.00    6.50    --  111.00  63.00 128.65   32
 31  \w     87.00 140.00   1.00    6.50    --  111.00  50.00 -86.96   53
 32  \w     42.00 113.00   1.00    6.50    --  111.00-125.00  60.00   71
 33  \w     83.00 110.00   1.00    6.50    --  111.00  70.00 130.63   27
 34  \w     89.00 150.00   1.00    6.50    --  111.00  45.00-180.00   61
 35  \w    151.00 178.00   1.00    6.50    --  111.00  68.00  67.80   27
 36  \w     85.00 111.00   1.00    6.50    --  111.00  61.00-150.00   26
 37  \w     85.00 113.00   1.00    6.50    --  111.00  61.00  90.00   28
 38  \w     85.00 160.00   1.00    6.50    --  111.00  61.00 150.00   75
 39  \w     85.00 112.00   1.00    6.50    --  111.00  61.00  30.00   27
 40  \w     82.00 172.00   1.00    6.50    --  111.00  71.00 -25.58   90
 41  \w     86.00 131.00   1.00    6.50    --  111.00  55.00  59.13   45
 42  \w     85.00 124.00   1.00    6.50    --  111.00  61.00   0.00   39
 43  \w     85.00 166.00   1.00    6.50    --  111.00  61.00 -30.00   81
 44  \w     85.00 111.00   1.00    6.50    --  111.00  61.00-180.00   26
 45  \w    130.00 177.00   1.00    6.50    --  111.00  61.00-180.00   47
 46  \w     32.00 107.00   1.00    6.50    --  111.00 -94.00  90.00   75
 47  \w     42.00 113.00   1.00    6.50    --  111.00-125.00 -60.00   71
 48  \w     86.00 111.00   1.00    6.50    --  111.00  61.00  60.00   25
 49  \w    124.00 177.00   1.00    6.50    --  111.00  61.00  60.00   53
 50  \w     89.00 133.00   1.00    6.50    --  111.00  45.00-120.00   44
 51  \w     83.00 110.00   1.00    6.50    --  111.00  68.00  67.80   27
 52  \w    153.00 178.00   1.00    6.50    --  111.00  63.00-169.28   25
 53  \w     85.00 111.00   1.00    6.50    --  111.00  61.00 -66.02   26
 54  \w     84.00 115.00   1.00    6.50    --  111.00  63.00-169.28   31
 55  \w    110.00 141.00   1.00    6.50    --  111.00 -77.00 -60.00   31
 56  \w     44.00 136.00   1.00    6.50    --  111.00 -61.00  90.00   92
 57  \w     49.00  94.00   1.00    6.50    --  111.00-125.00 -90.00   45
 58  \w     43.00  94.00   1.00    6.50    --  111.00 -77.00 -60.00   51
 59  \w     85.00 173.00   1.00    6.50    --  111.00  61.00  14.57   88
;
_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      -0.0761415000
_diffrn_orient_matrix_UB_12      -0.0602848000
_diffrn_orient_matrix_UB_13      -0.0501189000
_diffrn_orient_matrix_UB_21      0.1284499000
_diffrn_orient_matrix_UB_22      -0.0389461000
_diffrn_orient_matrix_UB_23      0.0107805000
_diffrn_orient_matrix_UB_31      -0.0152079000
_diffrn_orient_matrix_UB_32      -0.0268217000
_diffrn_orient_matrix_UB_33      0.0970368000
_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  0.0355
_diffrn_reflns_av_unetI/netI     0.0150
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            65556
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.453
_diffrn_reflns_theta_min         3.841
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.496
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.710
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.104a (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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.194
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         6218
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0412
_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^)+(0.0551P)^2^+0.9626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1067
_refine_ls_wR_factor_ref         0.1114
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5463
_reflns_number_total             6218
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00782d2.cif
_cod_data_source_block           3cx2Pym
_cod_depositor_comments
'Adding full bibliography for 7715770--7715781.cif.'
_cod_original_cell_volume        2974.03(6)
_cod_database_code               7715778
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C36H38B2N2
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.899
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C19(H19A,H19B), C23(H23A,H23B), C25(H25A,H25B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7), C8(H8), C10(H10), C12(H12), C13(H13), C14(H14),
 C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34),
  C35(H35), C36(H36)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C24(H24A,H24B,H24C), C26(H26A,H26B,
 H26C)
;
_shelx_res_checksum              34835
_olex2_date_sample_data_collection 2021-04-30
_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 1.125
_oxdiff_exptl_absorpt_empirical_full_min 0.887