Guest-adaptive hydrogen-bonded dimerization of a C3-symmetric tribenzotriquinacene molecular bowl
Yang, Tian-Shu; Duan, Xiao-Fang; Yin, Fan; Cai, Li-Xuan; Zhou, Li-Peng; Hu, Shao-Jun; Guo, Xiao-Qing; Sun, Qing-Fu; CrystEngComm 27 (2025) 2025–2032; doi:10.1039/D5CE00038F

data_7250046
_publ_section_title
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 Guest-adaptive hydrogen-bonded dimerization of a C3-symmetric
 tribenzotriquinacene molecular bowl
;
_journal_issue                   13
_journal_name_full               CrystEngComm
_journal_page_first              2025
_journal_page_last               2032
_journal_paper_doi               10.1039/D5CE00038F
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety
'C59 H55 N15 O3, 3(C3 H3), C H Cl3, H2 O, 1.2[CHCl3]'
_chemical_formula_sum            'C70.2 H68.2 Cl6.6 N15 O4'
_chemical_formula_weight         1419.96
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc2m1483
_audit_creation_date             2025-02-12
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-02-12 deposited with the CCDC.	2025-02-27 downloaded from the CCDC.
;
_cell_angle_alpha                70.136(2)
_cell_angle_beta                 79.294(2)
_cell_angle_gamma                85.330(2)
_cell_formula_units_Z            2
_cell_length_a                   14.2295(3)
_cell_length_b                   15.4768(3)
_cell_length_c                   17.3417(4)
_cell_measurement_reflns_used    19965
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      55.9950
_cell_measurement_theta_min      2.3890
_cell_volume                     3528.67(14)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            46596
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         56.017
_diffrn_reflns_theta_min         2.389
_exptl_absorpt_coefficient_mu    1.924
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_description       block
_exptl_crystal_F_000             1477
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.7
_exptl_crystal_size_min          0.6
_refine_diff_density_max         1.060
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     838
_refine_ls_number_reflns         13676
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1149
_refine_ls_R_factor_gt           0.0881
_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^)+(0.1711P)^2^+3.1247P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2705
_refine_ls_wR_factor_ref         0.2954
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9502
_reflns_number_total             13676
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00038f2.cif
_cod_data_source_block           Ph
_cod_depositor_comments
'Adding full bibliography for 7250046--7250051.cif.'
_cod_original_formula_sum        'C70.20 H68.20 Cl6.60 N15 O4'
_cod_database_code               7250046
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O4-H4A \\sim O4-H4B
 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C23(H23), C40(H40), C57(H57), C63(H63)
3.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C13(H13), C15(H15), C19(H19), C20(H20), C21(H21),
 C27(H27), C29(H29), C30(H30), C32(H32), C36(H36), C37(H37), C38(H38), C44(H44),
  C46(H46), C47(H47), C49(H49), C53(H53), C54(H54), C55(H55), N9(H9), C60(H60),
 C61(H61), C62(H62), C64(H64), C65(H65), C66(H66), C67(H67), C68(H68), C69(H69)
3.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C24(H24A,
 H24B,H24C), C25(H25A,H25B,H25C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C),
 C58(H58A,H58B,H58C), C59(H59A,H59B,H59C)
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_smtbx_masks_special_details
;
A solvent mask was calculated and 135 electrons were 
found in a volume of 515\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
1.2[CHCl3] per formula unit 
which account for 139 electrons 
per unit cell.
;
_shelx_res_checksum              8971
_shelx_fab_checksum              31599
_olex2_submission_special_instructions 'No special instructions were received'