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_7244565
_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         '3(C28 H20 O16 S4), 2(C36 H36 N6), 57(H2 O)'
_chemical_formula_sum            'C156 H246 N12 O105 S12'
_chemical_formula_weight         4354.35
_chemical_name_common
'p-sulfonatocalix[4]arene/pillar[6]pyridinum host-guest complex'
_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   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                102.793(2)
_cell_angle_beta                 91.143(2)
_cell_angle_gamma                116.562(3)
_cell_formula_units_Z            2
_cell_length_a                   20.9250(7)
_cell_length_b                   21.5501(5)
_cell_length_c                   28.2109(6)
_cell_measurement_reflns_used    11679
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      69.707
_cell_measurement_theta_min      2.686
_cell_volume                     10992.4(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector_area_resol_mean 1.54184
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.998
_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  0.0643
_diffrn_reflns_av_unetI/netI     0.0895
_diffrn_reflns_Laue_measured_fraction_full 0.941
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            84106
_diffrn_reflns_point_group_measured_fraction_full 0.941
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         65.089
_diffrn_reflns_theta_min         5.582
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.962
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.58949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_description       block
_exptl_crystal_F_000             4596
_exptl_crystal_recrystallization_method
'crystallization by liquid-liquid diffusion'
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.967
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2973
_refine_ls_number_reflns         37424
_refine_ls_number_restraints     950
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.1794
_refine_ls_R_factor_gt           0.1154
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_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          0.3070
_refine_ls_wR_factor_ref         0.3759
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19777
_reflns_number_total             37424
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00232a2.cif
_cod_data_source_block           kk_58_fin
_cod_database_code               7244565
_shelxl_version_number           2013-3
_shelx_res_checksum              15674