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_7250944
_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         'C60 H56 Ag4 N16, 4(C24 H20 B), 10(C2 H3 N)'
_chemical_formula_sum            'C176 H166 Ag4 B4 N26'
_chemical_formula_weight         3120.06
_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   geom
_audit_block_doi                 10.5517/ccdc.csd.cc2nv7wn
_audit_creation_date             2018-09-30
_audit_creation_method
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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.
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_cell_angle_alpha                83.5650(10)
_cell_angle_beta                 75.8980(10)
_cell_angle_gamma                69.6420(10)
_cell_formula_units_Z            1
_cell_length_a                   14.7897(5)
_cell_length_b                   16.4560(5)
_cell_length_c                   17.2188(6)
_cell_measurement_reflns_used    9923
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.32
_cell_measurement_theta_min      2.31
_cell_volume                     3808.8(2)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       '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      153.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_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  0.0486
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            47222
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.355
_diffrn_reflns_theta_min         2.310
_exptl_absorpt_coefficient_mu    0.567
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0816 before and 0.0596 after correction.
The Ratio of minimum to maximum transmission is 0.9159.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_description       block
_exptl_crystal_F_000             1612
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.070
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     986
_refine_ls_number_reflns         13902
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0337P)^2^+2.7855P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0927
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11059
_reflns_number_total             13902
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra05896a2.cif
_cod_data_source_block           h18093003
_cod_database_code               7250944
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.972
_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 C(H,H,H,H,H,H) groups
2. Restrained distances
 N1A-C1A = N2A-C3A
 1.16 with sigma of 0.02
 C4A-C3A = C1A-C0AA
 1.47 with sigma of 0.005
 C34A-C33 \\sim C34-C33
 with sigma of 0.02
 N11-C34 \\sim N11A-C34A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C3A) \\sim Ueq, Uanis(N2A) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(N10)
\\sim Ueq, Uanis(C0AA) \\sim Ueq, Uanis(C1A) \\sim Ueq, Uanis(N1A) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N11A) = Uanis(N11)
Uanis(C34A) = Uanis(C34)
4. Rigid body (RIGU) restrains
 C4A, C3A, N2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H33D)=Sof(H33E)=Sof(H33F)=Sof(N11A)=Sof(C34A)=1-FVAR(1)
 Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C34)=Sof(N11)=FVAR(1)
 Fixed Sof: C3A(0.5) C1A(0.5) N1A(0.5) N2A(0.5) C4A(0.5) H4AA(0.5) H4AB(0.5)
 H4AC(0.5) C0AA(0.5) H0AA(0.5) H0AB(0.5) H0AC(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C19(H19A,H19B), C1(H1A,H1B), C9(H9A,H9B), C23(H23A,H23B),
 C15(H15A,H15B)
6.b Aromatic/amide H refined with riding coordinates:
 C68(H68), C75(H75), C69(H69), C71(H71), C81(H81), C62(H62), C65(H65),
 C70(H70), C16(H16), C63(H63), C6(H6), C56(H56), C74(H74), C18(H18), C38(H38),
 C26(H26), C72(H72), C41(H41), C2(H2), C28(H28), C80(H80), C82(H82), C39(H39),
 C4(H4), C21(H21), C64(H64), C27(H27), C22(H22), C59(H59), C25(H25), C76(H76),
 C66(H66), C83(H83), C44(H44), C84(H84), C8(H8), C11(H11), C77(H77), C78(H78),
 C45(H45), C42(H42), C40(H40), C57(H57), C60(H60), C50(H50), C14(H14), C13(H13),
  C58(H58), C47(H47), C48(H48), C12(H12), C46(H46), C51(H51), C53(H53),
 C52(H52), C54(H54)
6.c Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C33(H33A,H33B,H33C), C33(H33D,H33E,H33F), C31(H31A,H31B,
 H31C), C29(H29A,H29B,H29C), C4A(H4AA,H4AB,H4AC), C0AA(H0AA,H0AB,H0AC)
;
_shelx_res_checksum              79898
_olex2_submission_special_instructions 'No special instructions were received'