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_1574596
_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 H140 Cs2 N28 O4, 1.5(C2 F6 N O4 S2), C F3 N0.273 O1.09 S0.545, 0.227(N O4 S2), 1[CHCl3], 2[C6H14O], 1[C6H14O]'
_chemical_formula_sum            'C155 H183 Cl3 Cs2 F12 N30 O15 S4'
_chemical_formula_weight         3434.71
_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     dual
_audit_creation_date             2025-05-06
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7224)
;
_audit_update_record
;
2025-05-06 deposited with the CCDC.	2025-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                81.578(2)
_cell_angle_beta                 82.615(2)
_cell_angle_gamma                84.009(2)
_cell_formula_units_Z            2
_cell_length_a                   15.9658(10)
_cell_length_b                   16.1176(10)
_cell_length_c                   33.451(2)
_cell_measurement_reflns_used    9558
_cell_measurement_temperature    170.00
_cell_measurement_theta_max      57.102
_cell_measurement_theta_min      2.579
_cell_volume                     8412.3(9)
_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  (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  '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  0.0626
_diffrn_reflns_av_unetI/netI     0.0683
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            137619
_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         57.201
_diffrn_reflns_theta_min         2.339
_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    3.315
_exptl_absorpt_correction_T_max  0.7512
_exptl_absorpt_correction_T_min  0.5627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0927 before and 0.0747 after correction.
The Ratio of minimum to maximum transmission is 0.7491.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_description       block
_exptl_crystal_F_000             3552
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.841
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1989
_refine_ls_number_reflns         34407
_refine_ls_number_restraints     514
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0682
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1369P)^2^+6.2945P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2117
_refine_ls_wR_factor_ref         0.2207
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26735
_reflns_number_total             34407
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc01474c2.cif
_cod_data_source_block           241008_th_1489_2cs
_cod_depositor_comments
'Adding full bibliography for 1574594--1574596.cif.'
_cod_original_cell_volume        8412.2(9)
_cod_database_code               1574596
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.777
_shelx_estimated_absorpt_t_min   0.619
_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, All O(H,H) groups, All O(H,H,H,H) groups
2. Restrained distances
 S3-C135
 1.8 with sigma of 0.02
 S5-N31 = S5A-N31
 1.56 with sigma of 0.01
 S5-O12A = S5-O11A = S5A-O12 = S5A-O11
 1.42 with sigma of 0.01
 S5-C137 = S5A-C145
 1.83 with sigma of 0.01
 F14-C137 = F15-C137 = F13-C137 = F14A-C145 = F15A-C145 = F13A-C145
 1.33 with sigma of 0.01
 S3-O8
 1.4 with sigma of 0.02
 S4-C136
 1.8 with sigma of 0.02
 O8-S3
 1.4 with sigma of 0.01
 C135-S3
 1.7 with sigma of 0.01
 C135-F7 = C135-F8 = C135-F9
 1.5 with sigma of 0.02
 O8A-S3A
 1.4 with sigma of 0.01
 O7A-S3A
 1.4 with sigma of 0.01
 O9A-S4A
 1.4 with sigma of 0.01
 O10A-S4A
 1.4 with sigma of 0.01
 O7-S3
 1.4 with sigma of 0.01
 O9-S4
 1.4 with sigma of 0.01
 O10-S4
 1.4 with sigma of 0.01
 S3A-N30A
 1.7 with sigma of 0.02
 S4A-N30A
 1.7 with sigma of 0.02
 O7-O8
 2.4 with sigma of 0.04
 F15A-F14A
 2.12 with sigma of 0.03
 F13A-F14A
 2.12 with sigma of 0.03
 F13A-F15A
 2.12 with sigma of 0.03
 F13-F14
 2.12 with sigma of 0.03
 F15-F13
 2.12 with sigma of 0.03
 F14-F15
 2.12 with sigma of 0.03
 S5-S5A
 2.807 with sigma of 0.03
 S3-O8 \\sim S3A-O8A
 with sigma of 0.02
 O7-O8 \\sim O7A-O8A
 with sigma of 0.04
 O8-N30 \\sim O8A-N30A
 with sigma of 0.04
 C135-F7 \\sim C135-F8 \\sim C135-F9
 with sigma of 0.02
 O8-C135 \\sim O8A-C135
 with sigma of 0.04
 F7-F8 \\sim F7-F9 \\sim F8-F9
 with sigma of 0.02
 S3-O7 \\sim S3A-O7A
 with sigma of 0.02
 S3-N30 \\sim S3A-N30A
 with sigma of 0.02
 S3-C135 \\sim S3A-C135
 with sigma of 0.02
 S4-O9 \\sim S4A-O9A
 with sigma of 0.02
 S4-O10 \\sim S4A-O10A
 with sigma of 0.02
 S4-N30 \\sim S4A-N30A
 with sigma of 0.02
 S4-C136 \\sim S4A-C136
 with sigma of 0.02
 S3-S4 \\sim S3A-S4A
 with sigma of 0.04
 O7-N30 \\sim O7A-N30A
 with sigma of 0.04
 O7-C135 \\sim O7A-C135
 with sigma of 0.04
 O9-O10 \\sim O9A-O10A
 with sigma of 0.04
 O9-N30 \\sim O9A-N30A
 with sigma of 0.04
 O9-C136 \\sim O9A-C136
 with sigma of 0.04
 O10-N30 \\sim O10A-N30A
 with sigma of 0.04
 O10-C136 \\sim O10A-C136
 with sigma of 0.04
 N30-C135 \\sim N30A-C135
 with sigma of 0.04
 N30-C136 \\sim N30A-C136
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
S3 \\sim S4 \\sim F7 \\sim F8 \\sim F9 \\sim F10 \\sim F11 \\sim F12 \\sim O7
\\sim O8 \\sim O9 \\sim O10 \\sim N30 \\sim C135 \\sim C136: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A
S1 \\sim S2 \\sim F1 \\sim F2 \\sim F3 \\sim F4 \\sim F5 \\sim F6 \\sim O3
\\sim O4 \\sim O5 \\sim O6 \\sim N29 \\sim C133 \\sim C134: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A
C136 \\sim S3 \\sim O7 \\sim O8 \\sim N30 \\sim C135 \\sim S4 \\sim F7 \\sim F8
\\sim F9 \\sim O9 \\sim O10 \\sim F10 \\sim F11 \\sim F12 \\sim N30A \\sim S3A
\\sim S4A \\sim O7A \\sim O8A \\sim O9A \\sim O10A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(O9) \\sim Ueq, Uanis(O8) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(S5) \\sim Ueq, Uanis(F13A) \\sim Ueq, Uanis(F14A) \\sim Ueq, Uanis(F15A)
\\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(N31) \\sim Ueq,
Uanis(C145) \\sim Ueq, Uanis(S5A) \\sim Ueq, Uanis(O11A) \\sim Ueq, Uanis(F13)
\\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F15) \\sim Ueq, Uanis(C137) \\sim Ueq,
Uanis(O12A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O9A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O8A) = Uanis(O8)
Uanis(S5) = Uanis(S5A)
Uanis(O12A) = Uanis(O12)
Uanis(O11A) = Uanis(O11)
4. Others
 Sof(Cs1)=Sof(Cs1A)=Sof(H1BC)=Sof(H1BD)=Sof(H2BC)=Sof(H2BD)=Sof(O13)=Sof(H13A)=
 Sof(H13B)=Sof(O14)=Sof(H14A)=Sof(H14B)=1-FVAR(1)
 Sof(Cs2)=Sof(Cs2A)=Sof(H1AA)=Sof(H1AB)=Sof(H2AA)=Sof(H2AB)=Sof(O15)=Sof(H15A)=
 Sof(H15B)=Sof(O16)=Sof(H16A)=Sof(H16B)=FVAR(1)
 Sof(N30A)=Sof(S3A)=Sof(O7A)=Sof(O8A)=Sof(O9A)=Sof(S4A)=Sof(O10A)=0.5*(1-
 FVAR(3))
 Sof(S3)=Sof(S4)=Sof(O7)=Sof(O8)=Sof(O9)=Sof(O10)=Sof(N30)=0.5*FVAR(3)
 Fixed Sof: F7(0.5) F8(0.5) F9(0.5) F10(0.5) F11(0.5) F12(0.5) C135(0.5)
 C136(0.5) S5(0.5) F13(0.5) F13A(0.5) F14(0.5) F14A(0.5) F15(0.5) F15A(0.5)
 O11(0.5) O12(0.5) N31(0.5) C137(0.5) C145(0.5) S5A(0.5) O12A(0.5) O11A(0.5)
5.a Riding coordinates:
 O1(H1AA,H1AB), O1(H1BC,H1BD), O2(H2AA,H2AB), O2(H2BC,H2BD), O13(H13A,H13B),
 O15(H15A,H15B), O16(H16A,H16B), O14(H14A,H14B)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C10(H10A,H10B), C11(H11A,H11B), C19(H19A,H19B),
 C20(H20A,H20B), C28(H28A,H28B), C29(H29A,H29B), C37(H37A,H37B), C38(H38A,H38B),
  C46(H46A,H46B), C47(H47A,H47B), C67(H67A,H67B), C68(H68A,H68B), C76(H76A,
 H76B), C77(H77A,H77B), C85(H85A,H85B), C86(H86A,H86B), C94(H94A,H94B),
 C95(H95A,H95B), C103(H10F,H10G), C104(H10H,H10I), C112(H11F,H11G), C113(H11H,
 H11I)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C12(H12), C14(H14), C17(H17), C21(H21), C23(H23),
 C26(H26), C30(H30), C32(H32), C35(H35), C39(H39), C41(H41), C44(H44), C48(H48),
  C50(H50), C53(H53), C56(H56), C58(H58), C60(H60), C62(H62), C64(H64),
 C66(H66), C69(H69), C71(H71), C74(H74), C78(H78), C80(H80), C83(H83), C87(H87),
  C89(H89), C92(H92), C96(H96), C98(H98), C101(H101), C105(H105), C107(H107),
 C110(H110), C114(H114), C116(H116), C119(H119), C122(H122), C124(H124),
 C126(H126), C128(H128), C130(H130), C132(H132)
5.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C18(H18A,H18B,H18C), C27(H27A,H27B,H27C), C36(H36A,H36B,
 H36C), C45(H45A,H45B,H45C), C54(H54A,H54B,H54C), C75(H75A,H75B,H75C), C84(H84A,
 H84B,H84C), C93(H93A,H93B,H93C), C102(H10C,H10D,H10E), C111(H11C,H11D,H11E),
 C120(H12A,H12B,H12C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 485 electrons were 
found in a volume of 1730\%A^3^ in 3 voids per unit cell. 
This is consistent with the presence of 
1[CHCl3], 3[C6H14O]per Asymmetric Unit 
which account for 464 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              47459
_shelx_fab_checksum              50168
_olex2_diffrn_ambient_temperature_device 'Oxford Cryostream 800'
_olex2_submission_special_instructions 'No special instructions were received'