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_7250945
_publ_section_title
;
 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, 1.5(C10 H6 O6 S2), F6 P, 3(H2 O) '
_chemical_formula_sum            'C45 H47 F6 N8 O12 P S3'
_chemical_formula_weight         1133.06
_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   mixed
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc2nv7tl
_audit_creation_date             2019-01-18
_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                77.3840(10)
_cell_angle_beta                 86.6340(10)
_cell_angle_gamma                61.5670(10)
_cell_formula_units_Z            2
_cell_length_a                   13.5033(6)
_cell_length_b                   13.5926(6)
_cell_length_c                   16.9599(7)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.27
_cell_measurement_theta_min      2.32
_cell_volume                     2667.6(2)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.01
_diffrn_measured_fraction_theta_full 0.998
_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  0.0453
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            39097
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.385
_diffrn_reflns_theta_min         2.318
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.256
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6448
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1384 before and 0.0537 after correction.
The Ratio of minimum to maximum transmission is 0.8653.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorle
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_description       block
_exptl_crystal_F_000             1378
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
TITL mo_h18100701_0m_aP -1         R = 0.15
CELL   13.5033   13.5926   16.9599     77.38     86.63     61.57
SPGR P-1
C101 0.579 1.002 0.185 !       4.36 eA-3
Q102 0.404 0.793 0.284 !       3.53 eA-3
Q103 0.875 0.670 0.114 !       3.13 eA-3
Q104 0.502 0.809 0.228 !       3.07 eA-3
C105 0.043 0.463 0.493 !       2.80 eA-3
C106 0.700 0.845 0.077 !       2.69 eA-3
C107 0.530 0.922 0.061 !       2.23 eA-3
C108 0.112 0.411 0.472 !       2.00 eA-3
Q109 0.509 0.887 0.183 !       1.86 eA-3
C110 0.625 0.011 0.154 !       1.79 eA-3
C111 0.567 0.019 0.006 !       1.70 eA-3
Q112 0.690 0.035 0.175 !       1.58 eA-3
C113 0.667 0.865 0.138 !       1.57 eA-3
Q114 0.987 0.891 0.077 !       1.52 eA-3
Q115 0.971 0.598 0.110 !       1.25 eA-3
Q116 0.096 0.879 0.063 !       1.17 eA-3
Q117 0.967 0.670 0.222 !       1.16 eA-3
Q118 0.901 0.751 0.168 !       1.10 eA-3
Q119 0.334 0.757 0.192 !       1.05 eA-3
Q120 0.545 0.607 0.357 !       0.94 eA-3
Q121 0.115 0.592 0.191 !       0.94 eA-3
Q122 0.952 0.397 0.316 !       0.87 eA-3
Q123 0.937 0.608 0.154 !       0.87 eA-3
Q124 0.144 0.937 0.019 !       0.84 eA-3
Q125 0.950 0.501 0.149 !       0.82 eA-3
Q126 0.997 0.565 0.231 !       0.80 eA-3
Q127 0.693 0.301 0.084 !       0.79 eA-3
Q128 0.048 0.615 0.113 !       0.77 eA-3
Q129 0.860 0.082 0.411 !       0.76 eA-3
Q130 0.357 0.121 0.312 !       0.72 eA-3
Q131 0.250 0.930 0.405 !       0.72 eA-3
Q132 0.299 0.685 0.427 !       0.72 eA-3
Q133 0.880 0.323 0.503 !       0.69 eA-3
Q134 0.247 0.035 0.190 !       0.69 eA-3
Q135 0.809 0.033 0.030 !       0.69 eA-3
Q136 0.753 0.441 0.330 !       0.67 eA-3
Q137 0.627 0.892 0.469 !       0.67 eA-3
Q138 0.919 0.785 0.485 !       0.67 eA-3
Q139 0.702 0.302 0.175 !       0.67 eA-3
Q140 0.406 0.999 0.314 !       0.67 eA-3
Q141 0.059 0.946 0.437 !       0.66 eA-3
Q142 0.340 0.330 0.355 !       0.66 eA-3
Q143 0.154 0.250 0.331 !       0.65 eA-3
Q144 0.109 0.837 0.250 !       0.65 eA-3
Q145 0.389 0.115 0.053 !       0.64 eA-3
Q146 0.137 0.300 0.186 !       0.64 eA-3
Q147 0.812 0.747 0.291 !       0.63 eA-3
Q148 0.377 0.510 0.031 !       0.63 eA-3
Q149 0.487 0.211 0.488 !       0.62 eA-3
Q150 0.063 0.261 0.011 !       0.61 eA-3
Q151 0.376 0.501 0.503 !       0.61 eA-3
Q152 0.385 0.657 0.059 !       0.58 eA-3
Q153 0.739 0.979 0.311 !       0.58 eA-3
Q154 0.477 0.310 0.090 !       0.57 eA-3
Q155 0.252 0.047 0.095 !       0.56 eA-3
Q156 0.067 0.047 0.237 !       0.56 eA-3
Q157 0.738 0.983 0.408 !       0.55 eA-3
Q158 0.497 0.214 0.045 !       0.55 eA-3
Q159 0.265 0.392 0.140 !       0.55 eA-3
Q160 0.510 0.720 0.433 !       0.55 eA-3
Q161 0.639 0.306 0.438 !       0.54 eA-3
Q162 0.921 0.315 0.046 !       0.54 eA-3
Q163 0.109 0.802 0.105 !       0.54 eA-3
Q164 0.803 0.344 0.344 !       0.54 eA-3
Q165 0.909 0.947 0.247 !       0.53 eA-3
Q166 0.287 0.713 0.312 !       0.53 eA-3
Q167 0.939 0.897 0.267 !       0.53 eA-3
Q168 0.672 0.191 0.355 !       0.53 eA-3
Q169 0.593 0.738 0.458 !       0.52 eA-3
Q170 0.875 0.138 0.235 !       0.52 eA-3
Q171 0.872 0.155 0.403 !       0.52 eA-3
;
_refine_diff_density_max         1.439
_refine_diff_density_min         -0.885
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     713
_refine_ls_number_reflns         9768
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.237
_refine_ls_R_factor_all          0.0952
_refine_ls_R_factor_gt           0.0706
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0814P)^2^+5.5353P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1780
_refine_ls_wR_factor_ref         0.1964
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7155
_reflns_number_total             9768
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra05896a2.cif
_cod_data_source_block           mo_h18100701_0m_a_sq
_cod_database_code               7250945
_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 O(H,H) groups
2. Restrained distances
 F6-F3
 1.6 with sigma of 0.02
 C42-C41
 1.5 with sigma of 0.02
 C41-C45
 1.4 with sigma of 0.02
 H16D-O7
 3 with sigma of 0.02
 H16D-H16C
 1.35 with sigma of 0.02
 P1-F5 \\sim P1-F5A \\sim P1-F3 \\sim P1-F3A \\sim P1-F6 \\sim P1-F6A \\sim
P1-F2 \\sim P1-F4
 with sigma of 0.02
3. Rigid bond restraints
 C42, C43
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C41, C42
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
Uanis(F3) \\sim Ueq, Uanis(F3A) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
5. Others
 Sof(F3A)=Sof(F5A)=Sof(F6A)=1-FVAR(1)
 Sof(F3)=Sof(F5)=Sof(F6)=FVAR(1)
6.a Free rotating group:
 O10(H10A,H10B), O15(H15A,H15B), O16(H16C,H16D)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B), C12(H12A,H12B), C16(H16A,H16B), C20(H20A,H20B),
 C24(H24A,H24B)
6.c Aromatic/amide H refined with riding coordinates:
 C32(H32), C33(H33), C34(H34), C37(H37), C38(H38), C39(H39), C42(H42),
 C43(H43), C45(H45), C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11),
  C13(H13), C14(H14), C15(H15), C17(H17), C18(H18), C19(H19), C21(H21),
 C22(H22), C23(H23), C26(H26), C27(H27), C28(H28), C30(H30)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'