Molecular engineering of porous organic cages for iodine capture and fluorescence detection.
Liu, Shuangbin; Xiang, Yuanke; Chen, Xinqi; Gao, Haofeng; Yang, Xiaoran; Li, Jinmei; Fan, Jianxian; Liu, Ziyuan; He, Tianwei; Qiu, Li; Chemical communications (Cambridge, England) 61 (2025) 19124–19127; doi:10.1039/d5cc05062f

data_7135152
_publ_section_title
;
 Molecular engineering of porous organic cages for iodine capture and
 fluorescence detection.
;
_journal_issue                   96
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              19124
_journal_page_last               19127
_journal_paper_doi               10.1039/d5cc05062f
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C69 H60 N6 O3, 4(C H Cl3)'
_chemical_formula_sum            'C73 H64 Cl12 N6 O3'
_chemical_formula_weight         1498.70
_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     direct
_audit_creation_date             2025-10-31
_audit_creation_method
;
FinalCif V89 by Daniel Kratzert, Freiburg 2025,
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2025-10-31 deposited with the CCDC.	2025-11-03 downloaded from the CCDC.
;
_cell_angle_alpha                93.004(2)
_cell_angle_beta                 90.221(2)
_cell_angle_gamma                92.104(2)
_cell_formula_units_Z            4
_cell_length_a                   10.5020(7)
_cell_length_b                   17.3670(13)
_cell_length_c                   38.680(3)
_cell_measurement_reflns_used    9690
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      26.08
_cell_measurement_theta_min      2.36
_cell_volume                     7040.2(9)
_computing_cell_refinement       'SAINT V8.40B'
_computing_data_collection
'Bruker BIS V6.2.16/2021-10-22 && APEX4 2022.1-1'
_computing_data_reduction        'SAINT V8.40B'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE dual wavelength Mo/Cu'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1064
_diffrn_reflns_av_unetI/netI     0.0793
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            165598
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.808
_diffrn_reflns_theta_min         1.920
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.524
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1259 before and 0.0933 after correction.
The Ratio of minimum to maximum transmission is 0.7915.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_description       block
_exptl_crystal_F_000             3088
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.174
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1880
_refine_ls_number_reflns         29967
_refine_ls_number_restraints     1598
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.1217
_refine_ls_R_factor_gt           0.0744
_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^)+(0.0243P)^2^+18.5580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1351
_refine_ls_wR_factor_ref         0.1572
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20216
_reflns_number_total             29967
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc05062f2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7135151--7135152.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7135152
_shelx_shelxl_version_number     2018/3
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_estimated_absorpt_t_min   0.902
_shelx_estimated_absorpt_t_max   0.949
_olex2_diffrn_ambient_temperature_device 'Oxford Cryostream 800'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, H124 of C124, H111 of C111, H130 of C130, H133 of C133,
  H134 of C134, H121 of C121, H109 of C109, H112 of C112, H115 of C115, H122 of
  C122, H123 of C123, H119 of C119, H118 of C118, H114 of C114, H126 of C126,
  H127 of C127, H129 of C129, H136 of C136, H138 of C138, H141 of C141, H144 of
  C144, H43 of C43, H142 of C142, H148 of C148, H137 of C137, H60 of C60, H65
  of C65, H69 of C69, H61 of C61, H52 of C52, H67 of C67, H68 of C68, H44 of
  C44, H64 of C64, H57 of C57, H55 of C55, H45 of C45, H58 of C58, H53 of C53,
  H49 of C49, H51 of C51, H41 of C41, H48 of C48, H85 of C85, H87 of C87, H95
  of C95, H96 of C96, H94 of C94, H84 of C84, H88 of C88, H91 of C91, H92 of
  C92, H82 of C82, H140 of C140, H145 of C145, H143 of C143, H13 of C13, H17 of
  C17, H14 of C14, H23 of C23, H11 of C11, H24 of C24, H25 of C25, H21 of C21,
  H16 of C16, H20 of C20, H38 of C38, H40 of C40, H139 of C139
 At 1.5 times of:
  All C(H,H,H) groups, H149 of C149, H147 of C147
2. Restrained distances
 Cl11-C142 \\sim Cl26-C147
 with sigma of 0.02
 Cl19-C143 \\sim Cl27-C143
 with sigma of 0.02
 Cl20-C143 \\sim Cl1F-C143
 with sigma of 0.02
 Cl8-C141 \\sim Cl8A-C148
 with sigma of 0.02
 Cl21-C143 \\sim Cl1G-C143
 with sigma of 0.02
 Cl9-C141 \\sim Cl9A-C148
 with sigma of 0.02
 C143-H143 \\sim C143-H14C
 with sigma of 0.02
 Cl10-C142 \\sim Cl1B-C147
 with sigma of 0.02
 Cl7-C141 \\sim Cl7A-C148
 with sigma of 0.02
 Cl12-C142 \\sim Cl1A-C147
 with sigma of 0.02
 C141-H141 \\sim C148-H148
 with sigma of 0.02
 C142-H142 \\sim C147-H147
 with sigma of 0.02
 Cl15-C144 \\sim Cl1E-C149
 with sigma of 0.02
 Cl13-C144 \\sim Cl-C149
 with sigma of 0.02
 Cl14-C144 \\sim Cl1D-C149
 with sigma of 0.02
 C144-H144 \\sim C149-H149
 with sigma of 0.02
 Cl11-Cl10 \\sim Cl26-Cl1B
 with sigma of 0.04
 Cl23-C43 \\sim Cl23-C43A
 with sigma of 0.02
 Cl12-Cl10 \\sim Cl1A-Cl1B
 with sigma of 0.04
 Cl24-C43 \\sim Cl25-C43A
 with sigma of 0.02
 Cl11-Cl12 \\sim Cl26-Cl1A
 with sigma of 0.04
 Cl22-C43 \\sim Cl1C-C43A
 with sigma of 0.02
 C43-H43 \\sim C43A-H43A
 with sigma of 0.02
 Cl23-Cl24 \\sim Cl23-Cl25
 with sigma of 0.04
 Cl23-Cl22 \\sim Cl23-Cl1C
 with sigma of 0.04
 Cl24-Cl22 \\sim Cl25-Cl1C
 with sigma of 0.04
 Cl15-Cl13 \\sim Cl1E-Cl
 with sigma of 0.04
 Cl15-Cl14 \\sim Cl1E-Cl1D
 with sigma of 0.04
 Cl13-Cl14 \\sim Cl-Cl1D
 with sigma of 0.04
 Cl8-Cl9 \\sim Cl8A-Cl9A
 with sigma of 0.04
 Cl8-Cl7 \\sim Cl8A-Cl7A
 with sigma of 0.04
 Cl9-Cl7 \\sim Cl9A-Cl7A
 with sigma of 0.04
 Cl19-Cl20 \\sim Cl27-Cl1F
 with sigma of 0.04
 Cl19-Cl21 \\sim Cl27-Cl1G
 with sigma of 0.04
 Cl20-Cl21 \\sim Cl1F-Cl1G
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(Cl21) \\sim Ueq, Uanis(C147) \\sim Ueq, Uanis(Cl1A) \\sim Ueq,
Uanis(C149) \\sim Ueq, Uanis(C144) \\sim Ueq, Uanis(Cl1D) \\sim Ueq,
Uanis(Cl1E) \\sim Ueq, Uanis(Cl) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.01
Uanis(C147) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
Uanis(C148) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
Uanis(Cl1A) \\sim Ueq, Uanis(Cl1B) \\sim Ueq, Uanis(C147) \\sim Ueq,
Uanis(Cl10) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.01
Uanis(C43A) \\sim Ueq, Uanis(Cl25) \\sim Ueq, Uanis(Cl1C) \\sim Ueq,
Uanis(Cl7A) \\sim Ueq, Uanis(Cl8A) \\sim Ueq, Uanis(Cl9A) \\sim Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.01
Uanis(C43A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
Uanis(Cl25) \\sim Ueq, Uanis(Cl1C) \\sim Ueq, Uanis(Cl22) \\sim Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.001
5. Others
 Sof(Cl1A)=Sof(Cl1B)=Sof(Cl26)=Sof(C147)=Sof(H147)=1-FVAR(1)
 Sof(Cl10)=Sof(Cl11)=Sof(Cl12)=Sof(C142)=Sof(H142)=FVAR(1)
 Sof(Cl1C)=Sof(Cl25)=Sof(C43A)=Sof(H43A)=1-FVAR(2)
 Sof(Cl22)=Sof(Cl24)=Sof(C43)=Sof(H43)=FVAR(2)
 Sof(Cl)=Sof(Cl1D)=Sof(Cl1E)=Sof(C149)=Sof(H149)=1-FVAR(3)
 Sof(Cl13)=Sof(Cl14)=Sof(Cl15)=Sof(C144)=Sof(H144)=FVAR(3)
 Sof(Cl7A)=Sof(Cl8A)=Sof(Cl9A)=Sof(C148)=Sof(H148)=1-FVAR(4)
 Sof(Cl7)=Sof(Cl8)=Sof(Cl9)=Sof(C141)=Sof(H141)=FVAR(4)
 Sof(Cl1F)=Sof(Cl1G)=Sof(Cl27)=Sof(H14C)=1-FVAR(5)
 Sof(H143)=Sof(Cl19)=Sof(Cl20)=Sof(Cl21)=FVAR(5)
6.a Riding coordinates:
 C143(H143), C147(H147), C149(H149)
6.b Ternary CH refined with riding coordinates:
 C139(H139), C140(H140), C145(H145), C43(H43), C43A(H43A), C141(H141),
 C142(H142), C144(H144)
6.c Secondary CH2 refined with riding coordinates:
 C10(H10N,H10O), C26(H26A,H26B), C35(H35A,H35B), C37(H37A,H37B), C54(H54A,
 H54B), C146(H14A,H14B), C76(H76A,H76B), C78(H78A,H78B), C80(H80A,H80B),
 C97(H97A,H97B), C105(H10A,H10B), C107(H10I,H10J)
6.d Aromatic/amide H refined with riding coordinates:
 C11(H11), C13(H13), C14(H14), C16(H16), C17(H17), C20(H20), C21(H21),
 C23(H23), C24(H24), C25(H25), C38(H38), C40(H40), C41(H41), C44(H44), C45(H45),
  C48(H48), C49(H49), C51(H51), C52(H52), C53(H53), C55(H55), C57(H57),
 C58(H58), C60(H60), C61(H61), C64(H64), C65(H65), C67(H67), C68(H68), C69(H69),
  C82(H82), C84(H84), C85(H85), C87(H87), C88(H88), C91(H91), C92(H92),
 C94(H94), C95(H95), C96(H96), C109(H109), C111(H111), C112(H112), C114(H114),
 C115(H115), C118(H118), C119(H119), C121(H121), C122(H122), C123(H123),
 C124(H124), C126(H126), C127(H127), C129(H129), C130(H130), C133(H133),
 C134(H134), C136(H136), C137(H137), C138(H138)
6.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C33(H33A,H33B,H33C),
 C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C77(H77A,H77B,H77C), C79(H79A,H79B,
 H79C), C81(H81A,H81B,H81C), C104(H10C,H10D,H10E), C106(H10K,H10L,H10M),
 C108(H10F,H10G,H10H)
;
_shelx_res_checksum              33436