A metallosupramolecular-based ring-in-ring complex showing reversible host-guest dynamics and switchable electrochemical properties.
Martínez-Visiedo, Joel; Ibáñez, Susana; Dawe, Louise N.; Peris, Eduardo; Nanoscale 17 (2025) 20089–20095; doi:10.1039/d5nr02758f

data_1575231
_publ_section_title
;
 A metallosupramolecular-based ring-in-ring complex showing reversible
 host-guest dynamics and switchable electrochemical properties.
;
_journal_issue                   35
_journal_name_full               Nanoscale
_journal_page_first              20089
_journal_page_last               20095
_journal_paper_doi               10.1039/d5nr02758f
_journal_volume                  17
_journal_year                    2025
_chemical_formula_moiety         'C38 H28 N2 O8'
_chemical_formula_sum            'C38 H28 N2 O8'
_chemical_formula_weight         640.62
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-02-28
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.10.31 svn.r3677 for OlexSys, GUI svn.r5972)
;
_audit_update_record
;
2025-06-16 deposited with the CCDC.	2025-07-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.197(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.82660(10)
_cell_length_b                   15.0675(3)
_cell_length_c                   24.1674(4)
_cell_measurement_reflns_used    10210
_cell_measurement_temperature    200.0(3)
_cell_measurement_theta_max      71.7510
_cell_measurement_theta_min      4.6610
_cell_volume                     2827.54(8)
_computing_cell_refinement       'CrysAlisPro 1.171.43.117a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.117a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.117a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4051
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     -5.00  39.00   0.25    3.00    --  -41.25  19.00-150.00  176
  2  \w     -5.00  39.00   0.25    3.00    --  -41.25  19.00 -90.00  176
  3  \w    -20.00  33.00   0.25    3.00    --  -41.25  37.00 120.00  212
  4  \w     -5.00  39.00   0.25    3.00    --  -41.25  19.00-180.00  176
  5  \w     -5.00  39.00   0.25    3.00    --  -41.25  19.00-120.00  176
  6  \w     61.00 130.00   0.25    3.00    --   41.25 178.00 -90.00  276
  7  \w     26.00  57.00   0.25    7.50    --  102.61 -30.00   0.00  124
  8  \w     50.00 178.00   0.25    7.50    --  102.61  15.00 -60.00  512
  9  \w     26.00  57.00   0.25    7.50    --  102.61 -30.00  30.00  124
 10  \w     26.00  57.00   0.25    7.50    --  102.61 -30.00 -60.00  124
 11  \w     26.00  57.00   0.25    7.50    --  102.61 -30.00 120.00  124
 12  \w     30.00  93.00   0.25    7.50    --  102.61 -61.00-150.00  252
 13  \w     26.00  57.00   0.25    7.50    --  102.61 -30.00  60.00  124
 14  \w     30.00  72.00   0.25    7.50    --  102.61 -45.00 -30.00  168
 15  \w     26.00  57.00   0.25    7.50    --  102.61 -30.00 150.00  124
 16  \w     30.00  93.00   0.25    7.50    --  102.61 -61.00 -90.00  252
 17  \w   -113.00 -13.00   0.25    3.00    --  -41.25 -57.00 150.00  400
 18  \w   -113.00 -13.00   0.25    3.00    --  -41.25 -57.00-120.00  400
 19  \w   -113.00 -13.00   0.25    3.00    --  -41.25 -57.00   0.00  400
 20  \w     -5.00  39.00   0.25    3.00    --  -41.25  19.00 -60.00  176
 21  \w     50.00 178.00   0.25    7.50    --  102.61  15.00 120.00  512
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0450230000
_diffrn_orient_matrix_UB_12      0.0196081000
_diffrn_orient_matrix_UB_13      0.0627030000
_diffrn_orient_matrix_UB_21      -0.1746783000
_diffrn_orient_matrix_UB_22      0.0469535000
_diffrn_orient_matrix_UB_23      0.0003561000
_diffrn_orient_matrix_UB_31      -0.0826435000
_diffrn_orient_matrix_UB_32      -0.0886745000
_diffrn_orient_matrix_UB_33      0.0140266000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            20111
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.592
_diffrn_reflns_theta_max         66.592
_diffrn_reflns_theta_min         3.687
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.879
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.786
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.117a (Rigaku Oxford Diffraction, 2024)
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            'clear dark orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_description       needle
_exptl_crystal_F_000             1336
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CHCl3, Methanol'
_exptl_crystal_size_max          0.231
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.041
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.205
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         4988
_refine_ls_number_restraints     420
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0412
_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^)+(0.0687P)^2^+0.8780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1160
_refine_ls_wR_factor_ref         0.1227
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4258
_reflns_number_total             4988
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nr02758f2.cif
_cod_data_source_block           str2306_auto
_cod_depositor_comments
'Adding full bibliography for 1575231--1575232.cif.'
_cod_database_code               1575231
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O'
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C35(H35A,H35B), C17(H17A,H17B), C38(H38A,H38B), C15(H15A,
 H15B), C18(H18A,H18B), C36(H36A,H36B), C16(H16A,H16B)
3.b Aromatic/amide H refined with riding coordinates:
 C27(H27), C32(H32), C21(H21), C26(H26), C8(H8), C33(H33), C20(H20), C7(H7),
 C6(H6), C30(H30), C9(H9), C25(H25)
;
_shelx_res_checksum              71685
_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 1.450
_oxdiff_exptl_absorpt_empirical_full_min 0.753