Synthesis and crystal structure of a [2+4]-type organic cage based on calix[4]arene
Kishimoto, Yuto; Katagiri, Hiroshi; Yamada, Manabu; New Journal of Chemistry 50 (2026) 3450–3456; doi:10.1039/D5NJ03563E

data_7064296
_publ_section_title
;
 Synthesis and crystal structure of a [2+4]-type organic cage based on
 calix[4]arene
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3450
_journal_page_last               3456
_journal_paper_doi               10.1039/D5NJ03563E
_journal_volume                  50
_journal_year                    2026
_chemical_formula_moiety         'C76 H72 N8 O8 [+ solvent]'
_chemical_formula_sum            'C76 H72 N8 O8'
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_space_group_crystal_system      triclinic
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_space_group_name_Hall           '-P 1'
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_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
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_audit_update_record
;
2025-09-04 deposited with the CCDC.	2026-01-07 downloaded from the CCDC.
;
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_cell_length_b                   15.7908(5)
_cell_length_c                   16.3627(7)
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_cell_measurement_theta_max      27.0240
_cell_measurement_theta_min      2.1040
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_computing_data_collection       'CrysAlisPro 1.171.43.115a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.115a (Rigaku OD, 2024)'
_computing_molecular_graphics    'PLATON (Spek, 2020)'
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_diffrn_ambient_temperature      150
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_av_unetI/netI     0.0574
_diffrn_reflns_Laue_measured_fraction_full 0.999
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_diffrn_reflns_limit_h_min       -12
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_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            36599
_diffrn_reflns_point_group_measured_fraction_full 0.999
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_min         2.099
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
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_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93903
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.115a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.868
_exptl_crystal_description       plate
_exptl_crystal_F_000             648
_exptl_crystal_recrystallization_method 'Vapor diffusion method'
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.482
_refine_diff_density_min         -0.300
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_refine_ls_extinction_method     none
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_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.1539
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_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^)+(0.0977P)^2^+7.1665P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2890
_refine_ls_wR_factor_ref         0.3154
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5011
_reflns_number_total             8489
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj03563e2.cif
_cod_data_source_block           20240525_yamada_cpoc-pda_150k_auto_sq
_cod_original_cell_volume        2345.00(16)
_cod_database_code               7064296
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.996
_shelx_estimated_absorpt_t_max   0.999
_oxdiff_exptl_absorpt_empirical_full_min 0.831
_oxdiff_exptl_absorpt_empirical_full_max 1.292
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              49192
_shelx_fab_checksum              24757