Tetraimidazolium macrocycle: a versatile building block and precursor for box-type coordination cages
Wang, Fang; Hua, Kai; RSC Advances 15 (2025) 36704–36709; doi:10.1039/D5RA05896A

data_7250943
_publ_section_title
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 Tetraimidazolium macrocycle: a versatile building block and precursor for
 box-type coordination cages
;
_journal_issue                   44
_journal_name_full               'RSC Advances'
_journal_page_first              36704
_journal_page_last               36709
_journal_paper_doi               10.1039/D5RA05896A
_journal_volume                  15
_journal_year                    2025
_chemical_formula_moiety
'	C30 H32 N8, 2(C10 H6 O6 S2), 2(C2 H3 N), 5(H2 O)'
_chemical_formula_sum            'C54 H60 N10 O17 S4'
_chemical_formula_weight         1249.36
_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.cc2nv7vm
_audit_creation_date             2019-01-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2025-06-28 deposited with the CCDC.	2025-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                103.076(2)
_cell_angle_beta                 93.461(2)
_cell_angle_gamma                91.759(2)
_cell_formula_units_Z            2
_cell_length_a                   13.1874(10)
_cell_length_b                   13.5426(9)
_cell_length_c                   16.6450(11)
_cell_measurement_reflns_used    9885
_cell_measurement_temperature    166(2)
_cell_measurement_theta_max      25.33
_cell_measurement_theta_min      2.33
_cell_volume                     2887.3(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      166.0
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            49194
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.387
_diffrn_reflns_theta_min         2.205
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.245
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.7030
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0824 before and 0.0648 after correction.
The Ratio of minimum to maximum transmission is 0.9434.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless??
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_description       block
_exptl_crystal_F_000             1308.0
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.966
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     788
_refine_ls_number_reflns         10444
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_gt           0.0821
_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^)+(0.0395P)^2^+25.9738P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2112
_refine_ls_wR_factor_ref         0.2204
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8437
_reflns_number_total             10444
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra05896a2.cif
_cod_data_source_block           mo_h19012701_0m_a
_cod_original_formula_sum        '	C54 H60 N10 O17 S4'
_cod_database_code               7250943
_shelx_shelxl_version_number     2018/3
_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, All O(H,H) groups
2.a Free rotating group:
 O14(H14A,H14B), O16(H16A,H16B), O13(H13A,H13B), O15(H15C,H15D)
2.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C22(H22A,H22B), C7(H7A,H7B), C15(H15A,H15B), C30(H30A,H30B),
 C26(H26A,H26B)
2.c Aromatic/amide H refined with riding coordinates:
 C23(H23), C14(H14), C25(H25), C39(H39), C43(H43), C10(H10), C2(H2), C49(H49),
 C13(H13), C33(H33), C24(H24), C38(H38), C34(H34), C37(H37), C44(H44), C48(H48),
  C3(H3), C42(H42), C47(H47), C12(H12), C4(H4), C27(H27), C9(H9), C18(H18),
 C29(H29), C28(H28), C8(H8), C32(H32), C5(H5), C17(H17), C19(H19), C20(H20)
2.d Idealised Me refined as rotating group:
 C51(H51A,H51B,H51C), C53(H53A,H53B,H53C)
;
_shelx_res_checksum              6382
_olex2_submission_special_instructions 'No special instructions were received'