Hexadentate poly-Lewis acids based on the bowl-shaped tribenzotriquinacene.
Franke, Maurice; Klingsiek, Maximilian J.; Buth, Julian; Lamm, Jan-Hendrik; Neumann, Beate; Stammler, Hans-Georg; Mitzel, Norbert W.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 7751–7762; doi:10.1039/d4dt00379a

data_7715246
_publ_section_title
;
 Hexadentate poly-Lewis acids based on the bowl-shaped
 tribenzotriquinacene.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7751
_journal_page_last               7762
_journal_paper_doi               10.1039/d4dt00379a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         '2(C31 H28 Br6), 1.5(C7 H8)'
_chemical_formula_sum            'C72.5 H68 Br12'
_chemical_formula_weight         1898.19
_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             2023-12-11
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.11.24 svn.r209d9fb2 for OlexSys, GUI svn.r6869)
;
_audit_update_record
;
2024-01-16 deposited with the CCDC.	2024-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.226(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.0157(3)
_cell_length_b                   20.0868(4)
_cell_length_c                   19.9871(3)
_cell_measurement_reflns_used    23009
_cell_measurement_temperature    100.02(10)
_cell_measurement_theta_max      31.1900
_cell_measurement_theta_min      2.1420
_cell_volume                     7015.6(2)
_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-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (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      100.02(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.924
_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      6.00  95.00   1.00   55.50    --   26.03  57.00 -30.00   89
  2  \w    -43.00  47.00   1.00   55.50    --   26.03 -57.00-180.00   90
  3  \w    -46.00  52.00   1.00   55.50    --   26.03 -38.00  60.00   98
  4  \w     -4.00  42.00   1.00   55.50    --   26.03  77.00 -60.00   46
  5  \w      6.00  95.00   1.00   55.50    --   26.03  57.00  60.00   89
  6  \w     -4.00  42.00   1.00   55.50    --   26.03  77.00-180.00   46
  7  \w     -4.00  42.00   1.00   55.50    --   26.03  77.00 -30.00   46
  8  \w    -15.00  68.00   1.00   55.50    --   26.03 -99.00  60.00   83
  9  \w    -46.00 -17.00   1.00   55.50    --   26.03 -38.00 -90.00   29
;
_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      0.0026525000
_diffrn_orient_matrix_UB_12      0.0349174000
_diffrn_orient_matrix_UB_13      0.0057553000
_diffrn_orient_matrix_UB_21      -0.0374696000
_diffrn_orient_matrix_UB_22      0.0003344000
_diffrn_orient_matrix_UB_23      -0.0004058000
_diffrn_orient_matrix_UB_31      0.0154045000
_diffrn_orient_matrix_UB_32      -0.0052582000
_diffrn_orient_matrix_UB_33      0.0381790000
_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  0.0485
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            105349
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.201
_diffrn_reflns_theta_min         1.502
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.892
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.638
_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    1.797
_exptl_crystal_description       block
_exptl_crystal_F_000             3692
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.062
_refine_diff_density_max         1.467
_refine_diff_density_min         -1.045
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     801
_refine_ls_number_reflns         22899
_refine_ls_number_restraints     164
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+10.9976P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0818
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17003
_reflns_number_total             22899
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00379a2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7715245--7715251.cif.'
_cod_original_formula_sum        'C72.50 H68 Br12'
_cod_database_code               7715246
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C31 H28 Br6'
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_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. Restrained distances
 C75-C74 \\sim C74-C73 \\sim C73-C72 \\sim C72-C71 \\sim C71-C70 \\sim C70-C75
 with sigma of 0.02
 C75-C71 \\sim C75-C73 \\sim C70-C72 \\sim C74-C70 \\sim C73-C71 \\sim C74-C72
 with sigma of 0.04
 C76-C70 \\sim C76-C74
 with sigma of 0.04
3. Restrained planarity
 C70, C71, C72, C73, C74, C75, C76
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C70 \\sim C71 \\sim C72 \\sim C73 \\sim C74 \\sim C75 \\sim C76: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C73) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C75)
\\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(C76) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C70, C71, C72, C73, C74, C75, C76
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C70(0.5) H70(0.5) C71(0.5) H71(0.5) C72(0.5) H72(0.5) C73(0.5)
 H73(0.5) C74(0.5) H74(0.5) C75(0.5) C76(0.5) H76A(0.5) H76B(0.5) H76C(0.5)
7.a Ternary CH refined with riding coordinates:
 C1(H1), C32(H32)
7.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C24(H24A,H24B), C26(H26A,H26B), C27(H27A,H27B), C29(H29A,
 H29B), C30(H30A,H30B), C54(H54A,H54B), C55(H55A,H55B), C57(H57A,H57B),
 C58(H58A,H58B), C60(H60A,H60B), C61(H61A,H61B)
7.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C11(H11), C14(H14), C18(H18), C21(H21), C35(H35), C38(H38),
 C42(H42), C45(H45), C49(H49), C52(H52), C63(H63), C64(H64), C65(H65), C66(H66),
  C67(H67), C70(H70), C71(H71), C72(H72), C73(H73), C74(H74)
7.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C28(H28A,H28B,H28C), C31(H31A,H31B,H31C), C56(H56A,H56B,
 H56C), C59(H59A,H59B,H59C), C62(H62A,H62B,H62C), C69(H69A,H69B,H69C), C76(H76A,
 H76B,H76C)
;
_shelx_res_checksum              94370
_olex2_date_sample_data_collection 2021-02-11
_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 1.444
_oxdiff_exptl_absorpt_empirical_full_min 0.875