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_1575926
_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(C H Cl3), C86 H18 O8'
_chemical_formula_sum            'C88 H20 Cl6 O8'
_chemical_formula_weight         1417.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                 104.348(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8371(6)
_cell_length_b                   27.752(3)
_cell_length_c                   16.345(2)
_cell_measurement_reflns_used    2345
_cell_measurement_temperature    150.00(14)
_cell_measurement_theta_max      72.6060
_cell_measurement_theta_min      3.5240
_cell_volume                     5641.4(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      150.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3385
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.984
_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   -110.00 -17.00   1.00    8.00    --  -42.81 -57.00 120.00   93
  2  \w   -113.00 -18.00   1.00    8.00    --  -42.81 -38.00-150.00   95
  3  \w    -66.00  16.00   1.00    8.00    --  -42.81  38.00  30.00   82
  4  \w    -84.00  -9.00   1.00    8.00    --  -42.81 125.00   0.00   75
  5  \w     36.00  97.00   1.00    8.00    --   42.81-125.00-120.00   61
  6  \w    115.00 140.00   1.00   32.00    --  112.00 -30.00 -90.00   25
  7  \w    103.00 129.00   1.00   32.00    --  112.00 -61.00 150.00   26
  8  \w     36.00  87.00   1.00   32.00    --  112.00 -77.00 -60.00   51
  9  \w     64.00 109.00   1.00   32.00    --  112.00-111.00  30.00   45
 10  \w     40.00  86.00   1.00   32.00    --  112.00-111.00 150.00   46
 11  \w     59.00  99.00   1.00   32.00    --  112.00-111.00 -60.00   40
 12  \w     40.00  84.00   1.00   32.00    --  112.00 -30.00 -90.00   44
 13  \w     83.00 124.00   1.00   32.00    --  112.00  61.00   0.00   41
 14  \w    104.00 133.00   1.00   32.00    --  112.00  77.00 -90.00   29
 15  \w     48.00  74.00   1.00   32.00    --  112.00 -61.00 150.00   26
 16  \w     30.00  70.00   1.00   32.00    --  112.00 -95.00 -60.00   40
 17  \w     52.00 102.00   1.00   32.00    --  112.00-111.00 120.00   50
 18  \w     36.00  99.00   1.00   32.00    --  112.00 -30.00 120.00   63
 19  \w     77.00 106.00   1.00   32.00    --  112.00 -95.00 -60.00   29
 20  \w    107.00 164.00   1.00   32.00    --  112.00 111.00 150.00   57
 21  \w     60.00 109.00   1.00   32.00    --  112.00-111.00-120.00   49
 22  \w     81.00 106.00   1.00   32.00    --  112.00 -95.00  60.00   25
 23  \w    150.00 175.00   1.00   32.00    --  112.00  77.00 -90.00   25
 24  \w     75.00 128.00   1.00   32.00    --  112.00 -45.00 -30.00   53
 25  \w     74.00 109.00   1.00   32.00    --  112.00-111.00-150.00   35
 26  \w     49.00  89.00   1.00   32.00    --  112.00-111.00 -90.00   40
 27  \w    108.00 167.00   1.00   32.00    --  112.00  77.00-150.00   59
 28  \w    136.00 161.00   1.00   32.00    --  112.00  61.00   0.00   25
 29  \w    103.00 129.00   1.00   32.00    --  112.00  77.00-120.00   26
 30  \w    146.00 171.00   1.00   32.00    --  112.00  77.00-120.00   25
 31  \w    110.00 144.00   1.00   32.00    --  112.00 -77.00 -60.00   34
 32  \w    109.00 157.00   1.00   32.00    --  112.00 111.00   0.00   48
 33  \w     24.00 135.00   1.00   32.00    --  112.00   0.00-150.00  111
 34  \w     41.00 109.00   1.00   32.00    --  112.00-111.00-180.00   68
;
_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      0.0287079000
_diffrn_orient_matrix_UB_12      0.0366314000
_diffrn_orient_matrix_UB_13      0.0729768000
_diffrn_orient_matrix_UB_21      -0.0221690000
_diffrn_orient_matrix_UB_22      0.0416750000
_diffrn_orient_matrix_UB_23      -0.0642739000
_diffrn_orient_matrix_UB_31      -0.1184323000
_diffrn_orient_matrix_UB_32      0.0010974000
_diffrn_orient_matrix_UB_33      0.0043894000
_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  0.3837
_diffrn_reflns_av_unetI/netI     0.3052
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            54962
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.650
_diffrn_reflns_theta_min         3.554
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.389
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.712
_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
;
_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    1.669
_exptl_crystal_description       needle
_exptl_crystal_F_000             2856
_exptl_crystal_recrystallization_method
'Crystallized by slow evaporation from chloroform'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.027
_refine_diff_density_min         -0.021
_refine_diff_density_rms         0.003
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     923
_refine_ls_number_reflns         11695
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.937
_refine_ls_R_factor_all          0.2319
_refine_ls_R_factor_gt           0.1031
_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^)+(0.0724P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2272
_refine_ls_wR_factor_ref         0.3138
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4165
_reflns_number_total             11695
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc05734e3.cif
_cod_data_source_block           fst25042_auto
_cod_depositor_comments
'Adding full bibliography for 1575925--1575927.cif.'
_cod_original_cell_volume        5641.3(9)
_cod_database_code               1575926
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C86 H18 O8'
_chemical_oxdiff_usercomment     FSt-B1-246_F1F1F2
_cell_oxdiff_angle_alpha         90.004(8)
_cell_oxdiff_angle_beta          104.406(7)
_cell_oxdiff_angle_gamma         89.980(6)
_cell_oxdiff_length_a            12.8417(7)
_cell_oxdiff_length_b            27.759(3)
_cell_oxdiff_length_c            16.3391(17)
_cell_oxdiff_measurement_reflns_used 2345
_cell_oxdiff_volume              5641.2(8)
_shelx_estimated_absorpt_t_max   0.823
_shelx_estimated_absorpt_t_min   0.551
_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.a Ternary CH refined with riding coordinates:
 C02T(H02T), C02U(H02U)
2.b Secondary CH2 refined with riding coordinates:
 C01F(H01A,H01B), C027(H02A,H02B)
2.c Aromatic/amide H refined with riding coordinates:
 C01R(H01R), C01W(H01W), C021(H021), C022(H022), C02C(H02C), C02D(H02D),
 C02J(H02K), C02Q(H02Q)
2.d Idealised Me refined as rotating group:
 C02G(H02E,H02F,H02G), C02I(H02H,H02I,H02J)
;
_shelx_res_checksum              41204
_olex2_date_sample_data_collection 2025-04-24
_olex2_date_sample_submission    2025-04-01
_olex2_submission_original_sample_id FSt-B1-246_F1F2F2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.877
_oxdiff_exptl_absorpt_empirical_full_min 0.398