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_7135151
_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         'C57 H54 N8 O3, 2(C H Cl3)'
_chemical_formula_sum            'C59 H56 Cl6 N8 O3'
_chemical_formula_weight         1137.81
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-10-23
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-10-31 deposited with the CCDC.	2025-11-03 downloaded from the CCDC.
;
_cell_angle_alpha                89.732(4)
_cell_angle_beta                 74.207(4)
_cell_angle_gamma                89.827(4)
_cell_formula_units_Z            4
_cell_length_a                   15.1639(16)
_cell_length_b                   18.904(2)
_cell_length_c                   20.266(2)
_cell_measurement_reflns_used    9860
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.24
_cell_volume                     5590.0(10)
_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 2025/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.985
_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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0826
_diffrn_reflns_av_unetI/netI     0.0737
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            112790
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.567
_diffrn_reflns_theta_min         1.957
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.360
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6205
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1271 before and 0.0941 after correction.
The Ratio of minimum to maximum transmission is 0.8321.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_description       plate
_exptl_crystal_F_000             2368
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1579
_refine_ls_number_reflns         28120
_refine_ls_number_restraints     667
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1112
_refine_ls_R_factor_gt           0.0778
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1066P)^2^+7.1152P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1910
_refine_ls_wR_factor_ref         0.2198
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20761
_reflns_number_total             28120
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc05062f2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7135151--7135152.cif.'
_cod_original_cell_volume        5590.1(10)
_cod_database_code               7135151
_shelx_shelxl_version_number     2025/1
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6221(10)
 0.3779(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl2 \\sim Cl3 \\sim C115 \\sim Cl1A \\sim Cl2A \\sim Cl3A \\sim C119
\\sim Cl1B \\sim Cl2B \\sim Cl3B \\sim C124: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
Cl4 \\sim Cl5 \\sim Cl6 \\sim C118 \\sim Cl4A \\sim Cl5A \\sim Cl6A \\sim C120
\\sim Cl4B \\sim Cl5B \\sim Cl6B \\sim C123: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
Cl7 \\sim Cl8 \\sim Cl9 \\sim C117 \\sim Cl7A \\sim Cl8A \\sim Cl9A \\sim C121:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Cl10 \\sim Cl11 \\sim Cl12 \\sim C116 \\sim Cl13 \\sim Cl14 \\sim Cl15 \\sim
C122: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
2A
Uanis(Cl11) = Uanis(Cl14)
Uanis(Cl10) = Uanis(Cl13)
4. Same fragment restrains
{Cl1A, Cl2A, Cl3A, C119} sigma for 1-2: 0.01, 1-3: 0.01
{Cl1B, Cl2B, Cl3B, C124} sigma for 1-2: 0.01, 1-3: 0.01
as in
{Cl1, Cl2, Cl3, C115}
{Cl4A, Cl5A, Cl6A, C120} sigma for 1-2: 0.01, 1-3: 0.01
{Cl4B, Cl5B, Cl6B, C123} sigma for 1-2: 0.01, 1-3: 0.01
as in
{Cl4, Cl5, Cl6, C118}
{Cl7A, Cl8A, Cl9A, C121} sigma for 1-2: 0.01, 1-3: 0.01
as in
{Cl7, Cl8, Cl9, C117}
{Cl13, Cl14, Cl15, C122} sigma for 1-2: 0.01, 1-3: 0.01
as in
{Cl10, Cl11, Cl12, C116}
5. Others
 1*[Sof(Cl1)+Sof(Cl2)+Sof(Cl3)+Sof(C115)+Sof(H115)]+1*[Sof(Cl1A)+Sof(Cl2A)+
 Sof(Cl3A)+Sof(C119)+Sof(H119)]+1*[Sof(Cl1B)+Sof(Cl2B)+Sof(Cl3B)+Sof(C124)+
 Sof(H124)]=1 with esd of 0
 Sof(Cl1)=Sof(Cl2)=Sof(Cl3)=Sof(C115)=Sof(H115)=FVAR(1)
 Sof(Cl7A)=Sof(Cl8A)=Sof(Cl9A)=Sof(C121)=Sof(H121)=1-FVAR(2)
 Sof(Cl7)=Sof(Cl8)=Sof(Cl9)=Sof(C117)=Sof(H117)=FVAR(2)
 Sof(Cl13)=Sof(Cl14)=Sof(Cl15)=Sof(C122)=Sof(H122)=1-FVAR(3)
 Sof(Cl10)=Sof(Cl11)=Sof(Cl12)=Sof(C116)=Sof(H116)=FVAR(3)
 Sof(Cl1A)=Sof(Cl2A)=Sof(Cl3A)=Sof(C119)=Sof(H119)=FVAR(4)
 Sof(Cl1B)=Sof(Cl2B)=Sof(Cl3B)=Sof(C124)=Sof(H124)=FVAR(5)
 Fixed Sof: Cl4(0.43898) Cl5(0.43898) Cl6(0.43898) C118(0.43898) H118(0.43898)
 Cl4A(0.50924) Cl5A(0.50924) Cl6A(0.50924) C120(0.50924) H120(0.50924)
 Cl4B(0.05178) Cl5B(0.05178) Cl6B(0.05178) C123(0.05178) H123(0.05178)
6.a Ternary CH refined with riding coordinates:
 C115(H115), C118(H118), C117(H117), C116(H116), C119(H119), C120(H120),
 C121(H121), C122(H122), C124(H124), C123(H123)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B),
 C21(H21A,H21B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B),
  C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B), C75(H75A,
 H75B), C76(H76A,H76B), C77(H77A,H77B), C78(H78A,H78B), C94(H94A,H94B),
 C95(H95A,H95B), C96(H96A,H96B), C97(H97A,H97B), C113(H11A,H11B), C114(H11C,
 H11D)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C12(H12), C13(H13), C15(H15),
 C16(H16), C17(H17), C22(H22), C24(H24), C25(H25), C27(H27), C28(H28), C31(H31),
  C32(H32), C34(H34), C35(H35), C36(H36), C41(H41), C43(H43), C44(H44),
 C46(H46), C47(H47), C50(H50), C51(H51), C53(H53), C54(H54), C55(H55), C60(H60),
  C62(H62), C63(H63), C65(H65), C66(H66), C69(H69), C70(H70), C72(H72),
 C73(H73), C74(H74), C79(H79), C81(H81), C82(H82), C84(H84), C85(H85), C88(H88),
  C89(H89), C91(H91), C92(H92), C93(H93), C98(H98), C100(H100), C101(H101),
 C103(H103), C104(H104), C107(H107), C108(H108), C110(H110), C111(H111),
 C112(H112)
;
_shelx_res_checksum              26252
_olex2_diffrn_ambient_temperature_device 'Oxford Cryostream 800'
_olex2_submission_special_instructions 'No special instructions were received'