Host–guest conformational adaptation in the crystal complexes of pentamidine and p-sulfonato-calix[n]arenes
Kravets, Kateryna; Kravets, Mykola; Danylyuk, Oksana; CrystEngComm 27 (2025) 6611–6622; doi:10.1039/D5CE00666J

data_1575748
_publ_section_title
;
 Host--guest conformational adaptation in the crystal complexes of
 pentamidine and p-sulfonato-calix[n]arenes
;
_journal_issue                   40
_journal_name_full               CrystEngComm
_journal_page_first              6611
_journal_page_last               6622
_journal_paper_doi               10.1039/D5CE00666J
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety
'2(C56 H40 O32 S8), 8(C19 H26 N4 O2), 2(C2 H6 O), 48.3(H2 O)'
_chemical_formula_sum            'C268 H396.58 N32 O130.29 S16'
_chemical_formula_weight         6664.32
_chemical_name_common
'p-sulfonato-calix[8]arene/ pentamidine / ethanol host-guest complex'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2025-08-22 deposited with the CCDC.	2025-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.332(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   33.9061(5)
_cell_length_b                   41.7359(5)
_cell_length_c                   46.4819(7)
_cell_measurement_reflns_used    70991
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      68.977
_cell_measurement_theta_min      2.139
_cell_volume                     65588.7(16)
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector_area_resol_mean 16.2974
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1667
_diffrn_reflns_av_unetI/netI     0.0673
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            637017
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.601
_diffrn_reflns_theta_max         66.601
_diffrn_reflns_theta_min         4.939
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.818
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.47537
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_description       prism
_exptl_crystal_F_000             28215
_refine_diff_density_max         0.661
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     4340
_refine_ls_number_reflns         57878
_refine_ls_number_restraints     2852
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.1742
_refine_ls_R_factor_gt           0.1141
_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^)+(0.1851P)^2^+82.6691P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3092
_refine_ls_wR_factor_ref         0.3796
_reflns_Friedel_coverage         0.000
_reflns_number_gt                30121
_reflns_number_total             57878
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00666j1.cif
_cod_data_source_block           shelx_CCDC4
_cod_depositor_comments
'Adding full bibliography for 1575742--1575748.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1575748
_shelx_shelxl_version_number     2019/3
_shelx_res_checksum              56596
_shelx_fab_checksum              93302