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_7250942
_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 H4 N), 9(H2 O)'
_chemical_formula_sum            'C54 H70 N10 O21 S4'
_chemical_formula_weight         1323.4
_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.cc2nv7sk
_audit_creation_date             2018-10-03
_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                106.084(4)
_cell_angle_beta                 93.193(4)
_cell_angle_gamma                91.577(4)
_cell_formula_units_Z            1
_cell_length_a                   9.9900(12)
_cell_length_b                   11.5725(14)
_cell_length_c                   13.5773(17)
_cell_measurement_reflns_used    7265
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.40
_cell_measurement_theta_min      2.49
_cell_volume                     1504.4(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      153.04
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0660
_diffrn_reflns_av_unetI/netI     0.0737
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16014
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.401
_diffrn_reflns_theta_min         2.491
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.244
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4028
_exptl_absorpt_correction_type   ??multi-scan'
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1499 before and 0.0928 after correction.
The Ratio of minimum to maximum transmission is 0.5405.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_description       bulk
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.640
_refine_diff_density_min         -1.037
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       0.012(3)
_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   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         5515
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.527
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0685
_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^)+(0.0959P)^2^+2.0058P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1772
_refine_ls_wR_factor_ref         0.1944
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4290
_reflns_number_total             5515
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra05896a2.cif
_cod_data_source_block           mo_h18092504_0m_a
_cod_database_code               7250942
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.988
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H8BA,H8BB} of O8B, {H8AA,H8AB} of O8A, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, {H11A,H11B} of O11, {H9C,H9D} of O9, {H10A,H10B} of
  O10W, {H10C,H10D} of O10B
2. Restrained distances
 N1B-C1B = N1A-C1A
 1.16 with sigma of 0.005
 C2B-C1B = C2A-C1A
 1.47 with sigma of 0.005
 H6-H8AB
 2.1 with sigma of 0.005
 N1B-N2
 3 with sigma of 0.02
 N1B-N3
 3 with sigma of 0.02
 H10D-H10C
 3 with sigma of 0.02
 H10D-O10B
 0.87 with sigma of 0.02
 O10B-H10C
 0.87 with sigma of 0.02
 N1A-C2A = N1B-C2B
 2.63 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
N1B \\sim C1B \\sim C2B \\sim N1A \\sim C1A \\sim C2A: within 3.8A with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O8A) = Uanis(O8B)
4. Others
 Fixed Sof: O8B(0.5) H8BA(0.5) H8BB(0.5) O10B(0.5) H10C(0.5) H10D(0.5)
 N1B(0.5) C1B(0.5) H1BA(0.5) C2B(0.5) H2BA(0.5) H2BB(0.5) H2BC(0.5) O8A(0.5)
 H8AA(0.5) H8AB(0.5) N1A(0.5) C1A(0.5) H1AA(0.5) C2A(0.5) H2AA(0.5) H2AB(0.5)
 H2AC(0.5)
5.a Riding coordinates:
 O8B(H8BA,H8BB), O8A(H8AA,H8AB)
5.b Free rotating group:
 O11(H11A,H11B), O9(H9C,H9D), O10W(H10A,H10B), O10B(H10C,H10D)
5.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C5(H5A,H5B), C9(H9A,H9B)
5.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C14(H14),
 C15(H15), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23),
 C1B(H1BA), C1A(H1AA)
5.e Idealised Me refined as rotating group:
 C2B(H2BA,H2BB,H2BC), C2A(H2AA,H2AB,H2AC)
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_shelx_res_checksum              21777
_olex2_submission_special_instructions 'No special instructions were received'