Electrostatic co-assembly of pillar[n]pyridiniums and calix[4]arene in aqueous media
Kravets, Kateryna; Kravets, Mykola; Butkiewicz, Helena; Kosiorek, Sandra; Sashuk, Volodymyr; Danylyuk, Oksana; CrystEngComm  (2022) –; doi:10.1039/D2CE00232A

data_7244564
_publ_section_title
;
 Electrostatic co-assembly of pillar[n]pyridiniums and calix[4]arene in
 aqueous media
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00232A
_journal_year                    2022
_chemical_formula_moiety         '(C28 H20 O16 S4), (C24 H24 N4), 14(H2 O)'
_chemical_formula_sum            'C52 H72 N4 O30 S4'
_chemical_formula_weight         1361.37
_chemical_name_common
'p-sulfonatocalix[4]arene/pillar[4]pyridinum host-guest complex'
_space_group_crystal_system      tetragonal
_space_group_IT_number           84
_space_group_name_Hall           '-P 4c'
_space_group_name_H-M_alt        'P 42/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2021-12-08 deposited with the CCDC.	2022-03-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.3974(1)
_cell_length_b                   18.3974(1)
_cell_length_c                   20.6604(2)
_cell_measurement_reflns_used    16410
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      69.694
_cell_measurement_theta_min      4.011
_cell_volume                     6992.81(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector_area_resol_mean 16.2974
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.992
_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  0.0271
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            41529
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.242
_diffrn_reflns_theta_min         5.788
_exptl_absorpt_coefficient_mu    1.969
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78178
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_description       prism
_exptl_crystal_F_000             2864
_exptl_crystal_recrystallization_method 'crystallization in agarose gel'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     557
_refine_ls_number_reflns         6549
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0993
_refine_ls_R_factor_gt           0.0893
_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^)+(0.1894P)^2^+5.7390P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2615
_refine_ls_wR_factor_ref         0.2781
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5516
_reflns_number_total             6549
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00232a2.cif
_cod_data_source_block           kk_54
_cod_original_cell_volume        6992.81(10)
_cod_database_code               7244564
_shelxl_version_number           2013-3
_shelx_res_checksum              36343