Metal cations switch geometry of β-cyclodextrin complexes
Kolařík, Václav; Hromádková, Aneta; Knirsch, Adam; Prucková, Zdeňka; Janovský, Petr; Rouchal, Michal; Ward, Jas S.; Rissanen, Kari; Vícha, Robert; Chemical Communications 61 (2025) 7077–7080; doi:10.1039/D5CC00868A

data_7134394
_publ_section_title
;
 Metal cations switch geometry of \b-cyclodextrin complexes
;
_journal_issue                   39
_journal_name_full               'Chemical Communications'
_journal_page_first              7077
_journal_page_last               7080
_journal_paper_doi               10.1039/D5CC00868A
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C21 H24 N, Cl, H2 O'
_chemical_formula_sum            'C21 H26 Cl N O'
_chemical_formula_weight         343.88
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2025-02-06 deposited with the CCDC.	2025-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   42.2883(16)
_cell_length_b                   9.4126(2)
_cell_length_c                   9.1436(2)
_cell_measurement_reflns_used    4476
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      70.1130
_cell_measurement_theta_min      2.0930
_cell_volume                     3639.54(18)
_computing_cell_refinement       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -119.00 -27.00   0.50    3.00    --  -51.51 -77.00 150.00  184
  2  \w    -25.00  29.00   0.50    3.00    --   51.89 -19.00-180.00  108
  3  \w    -25.00  52.00   0.50    3.00    --   51.89 -38.00 120.00  154
  4  \w     19.00 104.00   0.50    3.00    --   51.89-125.00 120.00  170
  5  \w    -25.00  29.00   0.50    3.00    --   51.89 -19.00  60.00  108
  6  \w     38.00 130.00   0.50    3.00    --   62.00  76.00-142.76  184
  7  \w   -148.00 -58.00   0.50    3.00    --  -78.00 -69.00 -12.53  180
  8  \w   -112.00 -17.00   0.50   12.00    --  -87.58 125.00-120.00  190
  9  \w   -112.00 -20.00   0.50   12.00    --  -87.58  77.00 120.00  184
 10  \w   -171.00 -79.00   0.50   12.00    --  -95.50 -51.00-130.58  184
 11  \w     35.00 127.00   0.50   12.00    --  102.12 -77.00 150.00  184
 12  \w     88.00 176.00   0.50   12.00    --  102.12  38.00 150.00  176
 13  \w     25.00  52.00   0.50   12.00    --  102.12 -38.00 -30.00   54
 14  \w     63.00 176.00   0.50   12.00    --  102.12  19.00  30.00  226
 15  \w     32.00 111.00   0.50   12.00    --  102.12-125.00-120.00  158
 16  \w     35.00 106.00   0.50   12.00    --  102.12 -99.00 -60.00  142
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix-Arc 100'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0015594000
_diffrn_orient_matrix_UB_12      -0.0870603000
_diffrn_orient_matrix_UB_13      0.1424957000
_diffrn_orient_matrix_UB_21      0.0358531000
_diffrn_orient_matrix_UB_22      0.0278497000
_diffrn_orient_matrix_UB_23      0.0095939000
_diffrn_orient_matrix_UB_31      -0.0063453000
_diffrn_orient_matrix_UB_32      0.1357110000
_diffrn_orient_matrix_UB_33      0.0893604000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1118
_diffrn_reflns_av_unetI/netI     0.0533
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            33635
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.485
_diffrn_reflns_theta_min         4.182
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.895
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.912
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.89a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_description       plate
_exptl_crystal_F_000             1472
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol/benzene'
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.016
_exptl_crystal_size_min          0.006
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         3688
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0519
_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^)+(0.0583P)^2^+2.5377P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1161
_refine_ls_wR_factor_ref         0.1343
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2431
_reflns_number_total             3688
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc00868a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7134393--7134395.cif.'
_cod_original_sg_symbol_H-M      Pccn
_cod_database_code               7134394
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.871
_diffrn_oxdiff_digest_frames
;
01425afd63b0c0aba4868b9c88a6b7b25705272030d
;
_diffrn_oxdiff_digest_hkl
;
010abdc9aaec3a8757b954b9521b4887422ad7
;
_reflns_odcompleteness_completeness 98.48
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C17(H17), C19(H19), C21(H21)
2.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C18(H18A,H18B), C20(H20A,
 H20B), C22(H22A,H22B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12)
;
_shelx_res_checksum              80471
_shelx_hkl_checksum              47229
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.198
_oxdiff_exptl_absorpt_empirical_full_min 0.820