Solvent-controlled formation of alkali and alkali-earth-secured cucurbituril/guest trimers.
Lončarić, Doroteja; Movahedifar, Fahimeh; Štoček, Jakub Radek; Dračínský, Martin; Cvačka, Josef; Guan, Shanshan; Bythell, Benjamin J.; Císařová, Ivana; Masson, Eric; Kaleta, Jiří; Chemical science 14 (2023) 9258–9266; doi:10.1039/d3sc02032k

data_1569686
_publ_section_title
;
 Solvent-controlled formation of alkali and alkali-earth-secured
 cucurbituril/guest trimers.
;
_journal_issue                   35
_journal_name_full               'Chemical science'
_journal_page_first              9258
_journal_page_last               9266
_journal_paper_doi               10.1039/d3sc02032k
_journal_volume                  14
_journal_year                    2023
_chemical_compound_source        'synthesized by the authors'
_chemical_formula_moiety         'C22 H26 N, Cl, 0.5(H2 O)'
_chemical_formula_sum            'C22 H27 Cl N O0.5'
_chemical_formula_weight         348.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-11-23 deposited with the CCDC.	2023-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.9010(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.5283(4)
_cell_length_b                   9.7746(2)
_cell_length_c                   20.5000(4)
_cell_measurement_reflns_used    9805
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      72.0951
_cell_measurement_theta_min      2.9931
_cell_volume                     3667.98(13)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_collection       'Bruker Instrument Service vV6.2.15'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON III'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Helios Cu  multilayer optic'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            40378
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.094
_diffrn_reflns_theta_min         2.993
_diffrn_source                   'I\mS  micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.867
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_description       prism
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.211
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.199
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         7203
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0373P)^2^+1.6142P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0797
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6887
_reflns_number_total             7203
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02032k2.cif
_cod_data_source_block           cu_dl074_kaleta
_cod_depositor_comments
;
Adding full bibliography for 1569684--1569687.cif.

2025-06-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C44 H54 Cl2 N2 O'
_cod_original_formula_weight         697.79
_cod_original_formula_moiety         '2(C22 H26 N), 2(Cl), H2 O'
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1569686
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.694
_shelx_estimated_absorpt_t_max   0.871
_shelx_res_checksum              69523