A conformationally adaptable tetrahedral cage with different guest encapsulation models
Tang, Hua; Lu, Yuyang; Qian, Yongwei; Ge, Chenqi; Liu, Jiyong; Chen, Hongliang; Li, Hao; Chemical Science 16 (2025) 10867–10873; doi:10.1039/D5SC01474C

data_1574594
_publ_section_title
;
 A conformationally adaptable tetrahedral cage with different guest
 encapsulation models
;
_journal_issue                   24
_journal_name_full               'Chemical Science'
_journal_page_first              10867
_journal_page_last               10873
_journal_paper_doi               10.1039/D5SC01474C
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety
'C132 H133 N28, 1[CCl3], 0.5[CHCl3], 0.5[CHCl3]'
_chemical_formula_sum            'C134 H134 Cl6 N28'
_chemical_formula_weight         2349.38
_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             2025-04-25
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7224)
;
_audit_update_record
;
2025-04-25 deposited with the CCDC.	2025-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                75.352(2)
_cell_angle_beta                 81.600(2)
_cell_angle_gamma                71.934(2)
_cell_formula_units_Z            2
_cell_length_a                   13.0765(8)
_cell_length_b                   17.2821(11)
_cell_length_c                   30.4781(19)
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    170.00
_cell_measurement_theta_max      44.186
_cell_measurement_theta_min      2.466
_cell_volume                     6318.2(7)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker Instrument Service vV6.2.14'
_computing_data_reduction        'SAINT V8.40B (?, 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 2018/2 (Sheldrick, 2018)'
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'ZJU Bruker D8 VENTURE Metaljet PHOTON III'
_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           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0975
_diffrn_reflns_av_unetI/netI     0.1379
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            69944
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        52.262
_diffrn_reflns_theta_max         52.262
_diffrn_reflns_theta_min         1.307
_diffrn_source                   'liquid Metal X-ray source'
_diffrn_source_current           3.57
_diffrn_source_power             0.24954300000000001
_diffrn_source_type              'Bruker Excillum Metaljet D2+'
_diffrn_source_voltage           69.9
_exptl_absorpt_coefficient_mu    1.145
_exptl_absorpt_correction_T_max  0.7503
_exptl_absorpt_correction_T_min  0.6164
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1532 before and 0.0776 after correction.
The Ratio of minimum to maximum transmission is 0.8215.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_description       needle
_exptl_crystal_F_000             2472
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1453
_refine_ls_number_reflns         21558
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1713
_refine_ls_R_factor_gt           0.0922
_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^)+(0.1870P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2715
_refine_ls_wR_factor_ref         0.3302
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9946
_reflns_number_total             21558
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc01474c2.cif
_cod_data_source_block           240909_th_1454
_cod_depositor_comments
'Adding full bibliography for 1574594--1574596.cif.'
_cod_database_code               1574594
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.803
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 N13, C98
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C79, C123
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N15, C35
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C9(H9A,H9B), C15(H15A,H15B), C27(H27A,H27B), C29(H29A,H29B),
 C31(H31A,H31B), C37(H37A,H37B), C39(H39A,H39B), C43(H43A,H43B), C53(H53A,H53B),
  C58(H58A,H58B), C59(H59A,H59B), C61(H61A,H61B), C63(H63A,H63B), C71(H71A,
 H71B), C77(H77A,H77B), C96(H96A,H96B), C101(H10A,H10B), C105(H10C,H10D),
 C113(H11A,H11B), C114(H11C,H11D), C116(H11E,H11F), C119(H11J,H11K), C129(H12J,
 H12K)
3.b Aromatic/amide H refined with riding coordinates:
 N15(H15), C3(H3), C4(H4), C5(H5), C6(H6), C12(H12), C13(H13), C14(H14),
 C20(H20), C23(H23), C24(H24), C26(H26), C34(H34), C38(H38), C40(H40), C41(H41),
  C45(H45), C47(H47), C49(H49), C51(H51), C52(H52), C55(H55), C57(H57),
 C60(H60), C62(H62), C74(H74), C78(H78), C84(H84), C85(H85), C89(H89), C91(H91),
  C93(H93), C94(H94), C95(H95), C97(H97), C99(H99), C100(H100), C104(H104),
 C106(H106), C107(H107), C110(H110), C112(H112), C115(H115), C117(H117),
 C120(H120), C124(H124), C126(H126), C128(H128), C130(H130)
3.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C17(H17A,H17B,H17C), C21(H21A,H21B,H21C), C33(H33A,H33B,
 H33C), C65(H65A,H65B,H65C), C90(H90A,H90B,H90C), C109(H10E,H10F,H10G),
 C118(H11G,H11H,H11I), C123(H12A,H12B,H12C), C125(H12D,H12E,H12F), C127(H12G,
 H12H,H12I), C131(H13A,H13B,H13C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 265 electrons were 
found in a volume of 960\%A^3^ in 4 voids per unit cell. 
This is consistent with the presence of 
1[CHCl3], 1[CCl3] per Asymmetric Unit 
which account for 232 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              4158
_shelx_fab_checksum              15068
_olex2_diffrn_ambient_temperature_device 'Oxford Cryostream 800'
_olex2_submission_special_instructions 'No special instructions were received'