Surface inclusion and dynamics of cucurbit[7]uril-based supramolecular complexes.
Santos Hurtado, Carina; Bastien, Guillaume; Lončarić, Doroteja; Dračínský, Martin; Císařová, Ivana; Masson, Eric; Kaleta, Jiří; Chemical science 16 (2025) 14081–14087; doi:10.1039/d5sc03152d

data_1574859
_publ_section_title
;
 Surface inclusion and dynamics of cucurbit[7]uril-based supramolecular
 complexes.
;
_journal_issue                   31
_journal_name_full               'Chemical science'
_journal_page_first              14081
_journal_page_last               14087
_journal_paper_doi               10.1039/d5sc03152d
_journal_volume                  16
_journal_year                    2025
_chemical_compound_source        'synthesized by the authors'
_chemical_formula_moiety         'C17 H11 Br N3 O4, Cl, 1.236(H2 O)'
_chemical_formula_sum            'C17 H13.47 Br Cl N3 O5.24'
_chemical_formula_weight         458.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2025-01-12 deposited with the CCDC.	2025-06-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.1050(10)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   14.3576(5)
_cell_length_b                   42.1432(15)
_cell_length_c                   9.9596(4)
_cell_measurement_reflns_used    9002
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.4944
_cell_measurement_theta_min      2.44
_cell_volume                     5500.8(4)
_computing_cell_refinement       'SAINT V8.41 (Bruker AXS LLC)'
_computing_data_collection       'Bruker Instrument Service vV6.2.15'
_computing_data_reduction        'SAINT V8.41 (Bruker AXS LLC)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 7.391
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;<Phi   scan: start= 360.0; len= 180.0; end= 540.0 at [Counterclockwise Eulerian
angles: dx= 46.00 mm theta=   0.000 deg omega=   0.000 deg chi=  54.740 deg]
measure for 3.0 seconds; frame angle 0.40 degrees, wavelength=0.71073>
<Phi   scan: start=   0.0; len= 360.0; end= 360.0 at [Counterclockwise Eulerian
angles: dx= 45.00 mm theta=   4.096 deg omega= 267.341 deg chi=  24.000 deg]
measure for 15.0 seconds; frame angle 0.40 degrees, wavelength=0.71073>
<Omega scan: start=  29.8; len= -64.8; end= -35.0 at [Counterclockwise Eulerian
angles: dx= 45.00 mm theta=   9.421 deg phi= 108.000 deg chi=  68.500 deg]
measure for 15.0 seconds; frame angle 0.40 degrees, wavelength=0.71073>
<Omega scan: start=  29.8; len= -64.8; end= -35.0 at [Counterclockwise Eulerian
angles: dx= 45.00 mm theta=   9.421 deg phi= 324.000 deg chi=  68.500 deg]
measure for 15.0 seconds; frame angle 0.40 degrees, wavelength=0.71073>
<Omega scan: start= 325.0; len=  64.8; end= 389.8 at [Counterclockwise Eulerian
angles: dx= 45.00 mm theta=   9.421 deg phi= 180.000 deg chi=  68.500 deg]
measure for 15.0 seconds; frame angle 0.40 degrees, wavelength=0.71073>
<Omega scan: start=   3.0; len= 116.0; end= 119.0 at [Counterclockwise Eulerian
angles: dx= 45.00 mm theta=   4.096 deg phi=  72.000 deg chi= -44.500 deg]
measure for 15.0 seconds; frame angle 0.40 degrees, wavelength=0.71073>
<Phi   scan: start= 360.0; len=   0.4; end= 360.4 at [Counterclockwise Eulerian
angles: dx= 45.00 mm theta=   4.096 deg omega=   2.886 deg chi= -44.500 deg]
measure for 15.0 seconds; frame angle 0.40 degrees, wavelength=0.71073>
<Omega scan: start= 325.0; len=  64.8; end= 389.8 at [Counterclockwise Eulerian
angles: dx= 45.00 mm theta=   9.421 deg phi= 252.000 deg chi=  68.500 deg]
measure for 15.0 seconds; frame angle 0.40 degrees, wavelength=0.71073>
<Omega scan: start= 325.0; len=  64.8; end= 389.8 at [Counterclockwise Eulerian
angles: dx= 45.00 mm theta=   9.421 deg phi=  36.000 deg chi=  68.500 deg]
measure for 15.0 seconds; frame angle 0.40 degrees, wavelength=0.71073>
<Omega scan: start=   3.0; len= 116.0; end= 119.0 at [Counterclockwise Eulerian
angles: dx= 45.00 mm theta=   4.096 deg phi= 288.000 deg chi= -44.500 deg]
measure for 15.0 seconds; frame angle 0.40 degrees, wavelength=0.71073>
<Omega scan: start=   3.0; len= 116.0; end= 119.0 at [Counterclockwise Eulerian
angles: dx= 45.00 mm theta=   4.096 deg phi= 144.000 deg chi= -44.500 deg]
measure for 15.0 seconds; frame angle 0.40 degrees, wavelength=0.71073>
;
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTONIII CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Quazar Mo multilayer optic'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       54
_diffrn_reflns_limit_k_min       -54
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            130821
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.196
_diffrn_source                   'I\mS  micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.424
_exptl_absorpt_correction_T_max  0.797
_exptl_absorpt_correction_T_min  0.664
_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            yellow
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_description       prism
_exptl_crystal_F_000             2764
_exptl_crystal_size_max          0.184
_exptl_crystal_size_mid          0.158
_exptl_crystal_size_min          0.098
_refine_diff_density_max         2.215
_refine_diff_density_min         -0.844
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details
;
 Flack x determined using 5936 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0014(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     759
_refine_ls_number_reflns         12596
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0302
_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^)+(0.0551P)^2^+6.5692P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0837
_reflns_Friedel_coverage         0.994
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                12292
_reflns_number_total             12596
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc03152d3.cif
_cod_data_source_block           mo_dl006_kaleta
_cod_depositor_comments
'Adding full bibliography for 1574857--1574859.cif.'
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               1574859
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.664
_shelx_estimated_absorpt_t_max   0.797
_exptl_bruker_absorpt_correction_t_ratio 0.9413
_diffrn_measurement_bruker_total_exposure_time 53550.0
_shelx_res_checksum              53276