Host-guest chemistry of tridentate Lewis acids based on tribenzotriquinacene.
Franke, Maurice; Ens, Tobin; Mix, Andreas; Neumann, Beate; Stammler, Hans-Georg; Mitzel, Norbert W.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 11970–11980; doi:10.1039/d4dt01558d

data_7716493
_publ_section_title
;
 Host-guest chemistry of tridentate Lewis acids based on
 tribenzotriquinacene.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11970
_journal_page_last               11980
_journal_paper_doi               10.1039/d4dt01558d
_journal_volume                  53
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C70 H88 B3 N3, 3(C6 H6)'
_chemical_formula_sum            'C88 H106 B3 N3'
_chemical_formula_weight         1238.18
_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             2021-08-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2024-04-02 deposited with the CCDC.	2024-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.397(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.4550(6)
_cell_length_b                   11.6294(4)
_cell_length_c                   25.6412(12)
_cell_measurement_reflns_used    10291
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      76.2370
_cell_measurement_theta_min      3.4360
_cell_volume                     3674.2(3)
_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 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    'SHELXT 2018/2 (Sheldrick, 2018)'
_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 0.990
_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    -58.00  13.00   1.00    6.00    --  -38.50  37.00-180.00   71
  2  \w    -89.00  47.00   1.00    6.00    --  -38.50   0.00 -60.00  136
  3  \w     12.00  81.00   1.00    6.00    --   42.70 -99.00-120.00   69
  4  \w     28.00  89.00   1.00    6.00    --   42.70-125.00  90.00   61
  5  \w     26.00  79.00   1.00    6.00    --   42.70  37.00  30.00   53
  6  \w     26.00  69.00   1.00    6.00    --   42.70  57.00 -30.00   43
  7  \w     59.00  84.00   1.00   32.00    --  111.00 -94.00-120.00   25
  8  \w    135.00 167.00   1.00   32.00    --  111.00  77.00 120.00   32
  9  \w     90.00 178.00   1.00   32.00    --  111.00  45.00 -90.00   88
 10  \w     85.00 112.00   1.00   32.00    --  111.00  61.00   0.00   27
 11  \w    116.00 175.00   1.00   32.00    --  111.00  77.00  90.00   59
 12  \w     85.00 111.00   1.00   32.00    --  111.00  61.00 -30.00   26
 13  \w    126.00 177.00   1.00   32.00    --  111.00  61.00 -30.00   51
 14  \w     46.00 105.00   1.00   32.00    --  111.00 -94.00 -60.00   59
 15  \w    104.00 172.00   1.00   32.00    --  111.00  77.00  60.00   68
 16  \w     43.00 101.00   1.00   32.00    --  111.00-125.00 -60.00   58
 17  \w     89.00 115.00   1.00   32.00    --  111.00  45.00 -30.00   26
 18  \w     91.00 177.00   1.00   32.00    --  111.00  30.00-150.00   86
 19  \w     89.00 115.00   1.00   32.00    --  111.00  45.00 -60.00   26
 20  \w     41.00 111.00   1.00   32.00    --  111.00-125.00-150.00   70
 21  \w     85.00 111.00   1.00   32.00    --  111.00  61.00 -90.00   26
 22  \w     89.00 115.00   1.00   32.00    --  111.00  45.00   0.00   26
 23  \w     85.00 111.00   1.00   32.00    --  111.00  61.00 -60.00   26
 24  \w     41.00  99.00   1.00   32.00    --  111.00-125.00-180.00   58
 25  \w     92.00 152.00   1.00   32.00    --  111.00  45.00  30.00   60
 26  \w     43.00  78.00   1.00   32.00    --  111.00-125.00 150.00   35
 27  \w     90.00 158.00   1.00   32.00    --  111.00  30.00 -30.00   68
 28  \w     90.00 116.00   1.00   32.00    --  111.00  30.00   0.00   26
 29  \w    137.00 169.00   1.00   32.00    --  111.00  59.00  -5.06   32
 30  \w     86.00 113.00   1.00   32.00    --  111.00  61.00  30.00   27
 31  \w    136.00 167.00   1.00   32.00    --  111.00  77.00-150.00   31
 32  \w     85.00 111.00   1.00   32.00    --  111.00  59.00  -5.06   26
;
_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      -0.0717232000
_diffrn_orient_matrix_UB_12      -0.0669324000
_diffrn_orient_matrix_UB_13      -0.0438080000
_diffrn_orient_matrix_UB_21      0.0697152000
_diffrn_orient_matrix_UB_22      0.0443263000
_diffrn_orient_matrix_UB_23      -0.0406972000
_diffrn_orient_matrix_UB_31      0.0750527000
_diffrn_orient_matrix_UB_32      -0.1053596000
_diffrn_orient_matrix_UB_33      0.0105034000
_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  0.0570
_diffrn_reflns_av_unetI/netI     0.0768
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            36522
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.591
_diffrn_reflns_theta_min         3.485
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.469
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.863
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_description       plate
_exptl_crystal_F_000             1340
_exptl_crystal_size_max          0.219
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.011
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.4(10)
_refine_ls_extinction_coef       0.00223(13)
_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   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1009
_refine_ls_number_reflns         15024
_refine_ls_number_restraints     230
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0756
_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^)+(0.0224P)^2^+4.6959P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1569
_refine_ls_wR_factor_ref         0.1677
_reflns_Friedel_coverage         0.864
_reflns_Friedel_fraction_full    0.979
_reflns_Friedel_fraction_max     0.947
_reflns_number_gt                12498
_reflns_number_total             15024
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01558d2.cif
_cod_data_source_block           5x3Py
_cod_depositor_comments
'Adding full bibliography for 7716492--7716494.cif.'
_cod_database_code               7716493
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C58 H72 B2 N2'
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.904
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6(10)
 0.4(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Restrained distances
 C58B-B3 \\sim C62B-B3
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C58 \\sim C58B \\sim C59 \\sim C59B \\sim C60 \\sim C60B \\sim C61 \\sim C61B
\\sim C62 \\sim C62B \\sim C63 \\sim C63B \\sim C64 \\sim C64B \\sim C65 \\sim
C65B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
2A
5. Others
 Sof(C58B)=Sof(H58B)=Sof(C59B)=Sof(H59C)=Sof(H59D)=Sof(C60B)=Sof(H60C)=
 Sof(H60D)=Sof(C61B)=Sof(H61C)=Sof(H61D)=Sof(C62B)=Sof(H62B)=Sof(C63B)=
 Sof(H63C)=Sof(H63D)=Sof(C64B)=Sof(H64C)=Sof(H64D)=Sof(C65B)=Sof(H65C)=
 Sof(H65D)=Sof(C66B)=Sof(H66B)=Sof(C67B)=Sof(H67B)=Sof(C68B)=Sof(H68B)=
 Sof(C69B)=Sof(H69B)=Sof(C70B)=Sof(H70B)=Sof(C86B)=Sof(H86B)=Sof(C85B)=
 Sof(H85B)=Sof(C84B)=Sof(H84B)=Sof(C83B)=Sof(H83B)=Sof(C88B)=Sof(H88B)=
 Sof(C87B)=Sof(H87B)=1-FVAR(1)
 Sof(C58)=Sof(H58)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(C60)=Sof(H60A)=Sof(H60B)=
 Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(C62)=Sof(H62)=Sof(C63)=Sof(H63A)=Sof(H63B)=
 Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(C66)=Sof(H66)=
 Sof(C67)=Sof(H67)=Sof(C68)=Sof(H68)=Sof(C69)=Sof(H69)=Sof(C70)=Sof(H70)=
 Sof(C83)=Sof(H83)=Sof(C84)=Sof(H84)=Sof(C85)=Sof(H85)=Sof(C86)=Sof(H86)=
 Sof(C87)=Sof(H87)=Sof(C88)=Sof(H88)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C1(H1), C32(H32), C36(H36), C45(H45), C49(H49), C58(H58), C58B(H58B),
 C62(H62), C62B(H62B)
6.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,
 H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B),
 C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C37(H37A,H37B), C38(H38A,H38B),
  C39(H39A,H39B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C50(H50A,
 H50B), C51(H51A,H51B), C52(H52A,H52B), C59(H59A,H59B), C59B(H59C,H59D),
 C60(H60A,H60B), C60B(H60C,H60D), C61(H61A,H61B), C61B(H61C,H61D), C63(H63A,
 H63B), C63B(H63C,H63D), C64(H64A,H64B), C64B(H64C,H64D), C65(H65A,H65B),
 C65B(H65C,H65D)
6.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C11(H11), C12(H12), C13(H13), C14(H14),
 C18(H18), C19(H19), C20(H20), C21(H21), C40(H40), C41(H41), C42(H42), C43(H43),
  C44(H44), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C66(H66),
 C66B(H66B), C67(H67), C67B(H67B), C68(H68), C68B(H68B), C69(H69), C69B(H69B),
 C70(H70), C70B(H70B), C77(H77), C78(H78), C79(H79), C80(H80), C81(H81),
 C82(H82), C71(H71), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76), C83(H83),
  C84(H84), C85(H85), C86(H86), C87(H87), C88(H88), C86B(H86B), C85B(H85B),
 C84B(H84B), C83B(H83B), C88B(H88B), C87B(H87B)
6.d Fitted hexagon refined as free rotating group:
 C86B(C85B,C84B,C83B,C88B,C87B)
;
_shelx_res_checksum              92537
_olex2_date_sample_data_collection 2021-08-02
_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 1.158
_oxdiff_exptl_absorpt_empirical_full_min 0.872