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_1574595
_publ_section_title
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 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 H132 N28, C4 H12 N, 1.016(Cl), 3[CHCl3], 5[C6H14O]'
_chemical_formula_sum            'C169 H217 Cl10.02 N29 O5'
_chemical_formula_weight         3089.77
_space_group_crystal_system      cubic
_space_group_IT_number           203
_space_group_name_Hall           '-F 2uv 2vw 3'
_space_group_name_H-M_alt        'F d -3 :2'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.4774(7)
_cell_length_b                   32.4774(7)
_cell_length_c                   32.4774(7)
_cell_measurement_reflns_used    8609
_cell_measurement_temperature    170.00
_cell_measurement_theta_max      54.444
_cell_measurement_theta_min      3.349
_cell_volume                     34256.6(13)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  '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  0.0559
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            42739
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.379
_diffrn_reflns_theta_min         2.050
_diffrn_source                   'liquid Metal X-ray source'
_diffrn_source_current           3.57
_diffrn_source_power             0.24957869999999996
_diffrn_source_type              'Bruker Excillum Metaljet D2+'
_diffrn_source_voltage           69.91
_exptl_absorpt_coefficient_mu    1.327
_exptl_absorpt_correction_T_max  0.7518
_exptl_absorpt_correction_T_min  0.5861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1153 before and 0.0671 after correction.
The Ratio of minimum to maximum transmission is 0.7796.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_description       block
_exptl_crystal_F_000             13154
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.299
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         3283
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.295
_refine_ls_R_factor_all          0.1041
_refine_ls_R_factor_gt           0.0888
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2960
_refine_ls_wR_factor_ref         0.3190
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2427
_reflns_number_total             3283
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc01474c2.cif
_cod_data_source_block           250401_th_250325_tmacl
_cod_depositor_comments
'Adding full bibliography for 1574594--1574596.cif.'
_cod_original_cell_volume        34257(2)
_cod_original_sg_symbol_H-M      'F d -3'
_cod_database_code               1574595
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.750
_shelx_estimated_absorpt_t_min   0.626
_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. Uiso/Uaniso restraints and constraints
Uanis(Cl1) \\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(Cl3) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(Cl3) = Uanis(Cl1) = Uanis(Cl2)
3. Others
 1*[Sof(Cl1)]+1*[Sof(Cl3)]+1*[Sof(Cl2)]=0.083 with esd of 0.001
 Fixed Sof: H12A(0.333333) H12B(0.333333) H12C(0.333333)
 Fixed X: Cl1(0.225573) Cl3(0.230404) Cl2(0.25)
 Fixed Y: Cl1(0.024426) Cl3(-0.021935) Cl2(0)
 Fixed Z: Cl1(0.225573) Cl3(0.225583) Cl2(0.25)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C11(H11)
4.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C12(H12A,H12B,H12C)
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_smtbx_masks_special_details
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A solvent mask was calculated and 3726 electrons were 
found in a volume of 12958\%A^3^ in 3 voids per unit cell. 
This is consistent with the presence of 
24[CHCl3], 40[C6H14O] per Unit Cell 
which account for 3898 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              91158
_shelx_fab_checksum              8460
_olex2_diffrn_ambient_temperature_device 'Oxford Cryostream 800'
_olex2_submission_special_instructions 'No special instructions were received'