Neutral anion-detecting organic cages based on anion-π interactions.
Lu, Yuyang; Zhou, Ping; Tang, Hua; Wu, Yating; Kuang, Yueyan; Cao, Ze; Liu, Jiyong; Wu, Guangcheng; Chen, Hongliang; Li, Hao; Chemical science 17 (2026) 5993–6004; doi:10.1039/d5sc08157b

data_1576947
_publ_section_title
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 Neutral anion-detecting organic cages based on anion-&#x3c0;
 interactions.
;
_journal_issue                   12
_journal_name_full               'Chemical science'
_journal_page_first              5993
_journal_page_last               6004
_journal_paper_doi               10.1039/d5sc08157b
_journal_volume                  17
_journal_year                    2026
_chemical_formula_moiety
'B F4, 0.9(C H Cl3), C120 H96 Cl12 N28, C16 H36 N, 5[CHCl3]'
_chemical_formula_sum            'C141.9 H137.9 B Cl29.7 F4 N29'
_chemical_formula_weight         3389.18
_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
_audit_creation_date             2025-12-26
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2026-01-09 deposited with the CCDC.	2026-01-12 downloaded from the CCDC.
;
_cell_angle_alpha                102.3817(19)
_cell_angle_beta                 93.1489(18)
_cell_angle_gamma                94.7641(16)
_cell_formula_units_Z            2
_cell_length_a                   17.5969(6)
_cell_length_b                   21.9736(7)
_cell_length_c                   22.7357(9)
_cell_measurement_reflns_used    9142
_cell_measurement_temperature    170.00
_cell_measurement_theta_max      54.73
_cell_measurement_theta_min      2.76
_cell_volume                     8533.1(5)
_computing_cell_refinement       'SAINT V8.41 (?, 2016)'
_computing_data_collection       'Bruker Instrument Service vV6.2.14'
_computing_data_reduction        'SAINT V8.41 (?, 2016)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.00
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III M28'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0856
_diffrn_reflns_av_unetI/netI     0.0719
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            136792
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.111
_diffrn_reflns_theta_min         2.901
_diffrn_source                   'liquid Metal X-ray source'
_diffrn_source_current           3.57
_diffrn_source_power             0.2491146
_diffrn_source_type              'Bruker Excillum Metaljet D2+'
_diffrn_source_voltage           69.78
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.249
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.5759
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1406 before and 0.0948 after correction.
The Ratio of minimum to maximum transmission is 0.7670.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_description       block
_exptl_crystal_F_000             3476
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1716
_refine_ls_number_reflns         32440
_refine_ls_number_restraints     169
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.1168
_refine_ls_R_factor_gt           0.0760
_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^)+(0.1141P)^2^+3.9297P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2079
_refine_ls_wR_factor_ref         0.2342
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19531
_reflns_number_total             32440
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc08157b2.cif
_cod_data_source_block           250716lyy_2
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C141.90 H137.90 B Cl29.70 F4 N29'
_cod_database_code               1576947
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.854
_shelx_estimated_absorpt_t_min   0.608
_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
2. Restrained distances
 F4A-F2A = F4-F1
 2.3 with sigma of 0.01
 B1-F1 = B1-F2 = B1-F3 = B1-F4 = B1-F1A = B1-F2A = B1-F3A = B1-F4A
 1.42 with sigma of 0.01
 C138-C137 = C137-C136 = C136-C135 = N28-C135 = N28-C123 = C124-C123 = C125-
 C124 = C126-C125 = C132-C131 = C133-C132 = C134-C133 = N28-C131 = N28-C127 =
 C128-C127 = C129-C128 = C130-C129
 1.53 with sigma of 0.01
 B1-F1 \\sim B1-F1A
 with sigma of 0.02
 B1-F2 \\sim B1-F2A
 with sigma of 0.02
 B1-F3 \\sim B1-F3A
 with sigma of 0.02
 B1-F4 \\sim B1-F4A
 with sigma of 0.02
3. Rigid bond restraints
 C133, C134
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
B1 \\sim F4A \\sim F4 \\sim F2 \\sim F3 \\sim F2A \\sim F1 \\sim F3A \\sim F1A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C131 \\sim C132 \\sim C133 \\sim C134: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
C135 \\sim C136 \\sim C137: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01 within 2A
5. Others
 Sof(F3A)=Sof(F4A)=Sof(F2A)=Sof(F1A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=FVAR(1)
 Fixed Sof: Cl2(0.9) Cl3(0.9) Cl4(0.9) C1(0.9) H1(0.9)
6.a Ternary CH refined with riding coordinates:
 C1(H1)
6.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C29(H29A,
 H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C46(H46A,H46B),
 C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B), C57(H57A,H57B), C58(H58A,H58B),
  C75(H75A,H75B), C76(H76A,H76B), C82(H82A,H82B), C83(H83A,H83B), C95(H95A,
 H95B), C96(H96A,H96B), C97(H97A,H97B), C98(H98A,H98B), C104(H10A,H10B),
 C105(H10C,H10D), C123(H12C,H12D), C124(H12E,H12F), C125(H12G,H12H), C127(H12L,
 H12M), C128(H12N,H12O), C129(H12P,H12Q), C131(H13F,H13G), C132(H13H,H13I),
 C133(H13J,H13K), C135(H13O,H13P), C136(H13Q,H13R), C137(H13S,H13T)
6.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C11(H11), C16(H16), C18(H18), C26(H26), C28(H28), C33(H33), C35(H35),
 C43(H43), C45(H45), C50(H50), C52(H52), C55(H55), C56(H56), C59(H59), C61(H61),
  C69(H69), C71(H71), C72(H72), C73(H73), C79(H79), C81(H81), C84(H84),
 C85(H85), C86(H86), C87(H87), C88(H88), C89(H89), C92(H92), C94(H94), C99(H99),
  C101(H101), C102(H102), C103(H103), C106(H106), C108(H108), C111(H111),
 C112(H112), C113(H113), C114(H114), C115(H115), C116(H116), C117(H117),
 C118(H118), C119(H119), C120(H120), C121(H121), C122(H122)
6.d Idealised Me refined as rotating group:
 C126(H12I,H12J,H12K), C130(H13C,H13D,H13E), C134(H13L,H13M,H13N), C138(H13U,
 H13V,H13W)
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_smtbx_masks_special_details
;
A solvent mask was calculated and 586 electrons were 
found in a volume of 2280\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
5[CHCl3] per Asymmetric Unit 
which account for 580 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              19335
_shelx_fab_checksum              67711
_olex2_diffrn_ambient_temperature_device 'Oxford Cryostream 800'
_olex2_submission_special_instructions 'No special instructions were received'