Observation of shuttling on the one-second timescale in a [10]cycloparaphenylene/C<sub>60</sub> [2]catenane.
Steudel, Fabian M.; Sabrià, Clara; Piane, Massimo Delle; Feixas, Ferran; Ribas, Xavi; Pavan, Giovanni M.; von Delius, Max; Chemical science 16 (2025) 21908–21916; doi:10.1039/d5sc05734e

data_1575925
_publ_section_title
;
 Observation of shuttling on the one-second timescale in a
 [10]cycloparaphenylene/C<sub>60</sub> [2]catenane.
;
_journal_issue                   46
_journal_name_full               'Chemical science'
_journal_page_first              21908
_journal_page_last               21916
_journal_paper_doi               10.1039/d5sc05734e
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         '2(C43 H9 O4), 2.362[CHCl3]'
_chemical_formula_sum            'C88.36 H20.36 Cl7.09 O8'
_chemical_formula_weight         1461.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-05-02
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7224)
;
_audit_update_record
;
2025-05-02 deposited with the CCDC.	2025-10-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.120(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8349(16)
_cell_length_b                   24.4206(16)
_cell_length_c                   18.1092(18)
_cell_measurement_reflns_used    3199
_cell_measurement_temperature    149.9(2)
_cell_measurement_theta_max      74.5520
_cell_measurement_theta_min      3.8090
_cell_volume                     5780.8(10)
_computing_cell_refinement       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.9(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3385
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.917
_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    -37.00  -7.00   1.00   12.50    --  -42.93 125.00-180.00   30
  2  \w    -74.00 -40.00   1.00   12.50    --  -42.93 125.00  90.00   34
  3  \w    -12.00  28.00   1.00   12.50    --  -42.93  38.00-180.00   40
  4  \w     43.00  97.00   1.00   12.50    --   42.93-125.00 150.00   54
  5  \w     20.00 109.00   1.00   12.50    --   42.93  38.00 120.00   89
  6  \w     14.00  58.00   1.00   12.50    --   42.93 -99.00 -90.00   44
  7  \w    125.00 178.00   1.00   50.00    --  112.00  45.00-120.00   53
  8  \w     47.00  83.00   1.00   50.00    --  112.00-111.00 120.00   36
  9  \w     88.00 120.00   1.00   50.00    --  112.00  45.00-120.00   32
 10  \w     48.00  82.00   1.00   50.00    --  112.00 -95.00-150.00   34
 11  \w    146.00 177.00   1.00   50.00    --  112.00  61.00-180.00   31
 12  \w     91.00 125.00   1.00   50.00    --  112.00  61.00-180.00   34
 13  \w     94.00 130.00   1.00   50.00    --  112.00  30.00  30.00   36
 14  \w    147.00 174.00   1.00   50.00    --  112.00  30.00  30.00   27
 15  \w     51.00 112.00   1.00   50.00    --  112.00 -45.00 -90.00   61
 16  \w     47.00  84.00   1.00   50.00    --  112.00-111.00  60.00   37
 17  \w    129.00 158.00   1.00   50.00    --  112.00  77.00 -60.00   29
 18  \w     89.00 178.00   1.00   50.00    --  112.00  45.00 -90.00   89
 19  \w     39.00 102.00   1.00   50.00    --  112.00-111.00  90.00   63
 20  \w     97.00 175.00   1.00   50.00    --  112.00  30.00   0.00   78
 21  \w    117.00 144.00   1.00   50.00    --  112.00 178.00  30.00   27
;
_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      0.0665231000
_diffrn_orient_matrix_UB_12      -0.0252933000
_diffrn_orient_matrix_UB_13      -0.0447538000
_diffrn_orient_matrix_UB_21      0.0806149000
_diffrn_orient_matrix_UB_22      -0.0163351000
_diffrn_orient_matrix_UB_23      0.0781484000
_diffrn_orient_matrix_UB_31      -0.0544618000
_diffrn_orient_matrix_UB_32      -0.0553613000
_diffrn_orient_matrix_UB_33      -0.0026971000
_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  0.1524
_diffrn_reflns_av_unetI/netI     0.1693
_diffrn_reflns_Laue_measured_fraction_full 0.942
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29565
_diffrn_reflns_point_group_measured_fraction_full 0.942
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.857
_diffrn_reflns_theta_min         3.620
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.780
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.699
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.102a (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            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_description       prism
_exptl_crystal_F_000             2940
_exptl_crystal_preparation
'The sample was dissolved in CDCl3 with added 1,2,4,5-tetramethylbenzene as internal standard.'
_exptl_crystal_recrystallization_method 'Slow evaporation from NMR tube'
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.271
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     863
_refine_ls_number_reflns         11454
_refine_ls_number_restraints     942
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1922
_refine_ls_R_factor_gt           0.1296
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3363
_refine_ls_wR_factor_ref         0.4202
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5143
_reflns_number_total             11454
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc05734e3.cif
_cod_data_source_block           fst25044_auto
_cod_depositor_comments
'Adding full bibliography for 1575925--1575927.cif.'
_cod_database_code               1575925
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C86 H18 O8'
_chemical_oxdiff_usercomment     FSt-B1-247_tlcF1hplcF1_qNMR
_cell_oxdiff_angle_alpha         90.013(5)
_cell_oxdiff_angle_beta          109.073(7)
_cell_oxdiff_angle_gamma         90.106(6)
_cell_oxdiff_length_a            13.8314(13)
_cell_oxdiff_length_b            24.4420(13)
_cell_oxdiff_length_c            18.0928(12)
_cell_oxdiff_measurement_reflns_used 3198
_cell_oxdiff_volume              5780.8(7)
_shelx_estimated_absorpt_t_max   0.863
_shelx_estimated_absorpt_t_min   0.343
_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 C(H,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
 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:
 C02Q(H02A,H02B), C02Z(H02F,H02G)
3.b Aromatic/amide H refined with riding coordinates:
 C00Y(H00Y), C01E(H01E), C01N(H01N), C01Z(H01Z), C02I(H02I), C02T(H02T),
 C02W(H02W), C02X(H02X)
3.c Idealised Me refined as rotating group:
 C01O(H01A,H01B,H01C), C02U(H02C,H02D,H02E)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              39190
_shelx_fab_checksum              91014
_olex2_date_sample_data_collection 2025-04-29
_olex2_date_sample_submission    2025-04-14
_olex2_submission_original_sample_id FSt-B1-247_tlcF1hplcF1_qNMR
_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 2.516
_oxdiff_exptl_absorpt_empirical_full_min 0.384