Mechanically interlocked porphyrinoids: self-assembly of metal-stabilised catenaphyrins.
Sarwa, Aleksandra; Matviyishyn, Maksym; Perdek, Jędrzej P; Trzaskowski, Bartosz; Kulesza, Dagmara; Zych, Eugeniusz; Szyszko, Bartosz; Chemical communications (Cambridge, England) 62 (2026) 148–151; doi:10.1039/d5cc05702g

data_7135154
_publ_section_title
;
 Mechanically interlocked porphyrinoids: self-assembly of metal-stabilised
 catenaphyrins.
;
_journal_issue                   1
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              148
_journal_page_last               151
_journal_paper_doi               10.1039/d5cc05702g
_journal_volume                  62
_journal_year                    2026
_chemical_formula_moiety         'C76 H64 N12 O8 Zn2'
_chemical_formula_sum            'C76 H64 N12 O8 Zn2'
_chemical_formula_weight         1404.13
_space_group_crystal_system      trigonal
_space_group_IT_number           152
_space_group_name_Hall           'P 31 2"'
_space_group_name_H-M_alt        'P 31 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     difmap
_audit_creation_date             2025-08-28
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7205)
;
_audit_update_record
;
2025-08-28 deposited with the CCDC.	2025-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   23.123(4)
_cell_length_b                   23.123(4)
_cell_length_c                   16.184(3)
_cell_measurement_reflns_used    37828
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      74.7410
_cell_measurement_theta_min      2.1840
_cell_volume                     7494(2)
_computing_cell_refinement       'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 42.102a 64-bit (release 15-09-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.104a (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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_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     93.00 118.00   0.50    1.00    --   80.75  64.00 170.11   50
  2  \w     91.00 127.00   0.50    1.00    --   80.75  36.00  75.83   72
  3  \w     66.00 125.00   0.50    1.00    --   80.75  20.00  74.96  118
  4  \w     52.00  89.00   0.50    1.00    --   80.75  10.00  70.14   74
  5  \w     78.00 125.00   0.50    1.00    --   80.75  12.00 131.18   94
  6  \w     93.00 125.00   0.50    1.00    --   80.75  13.00 -45.90   64
  7  \w     65.00  91.00   0.50    1.00    --   80.75  22.00-153.02   52
  8  \w     52.00  77.00   0.50    1.00    --   80.75  13.00 -45.90   50
  9  \w     45.00  70.00   0.50    1.00    --   80.75 -66.00  58.81   50
 10  \w     42.00  95.00   0.50    1.00    --   80.75-124.00   1.92  106
 11  \w     24.00  60.00   0.50    1.00    --   62.21-125.00 -90.00   72
 12  \w     46.00  71.00   0.50    1.00    --   80.75-122.00-107.95   50
 13  \w     37.00  62.00   0.50    1.00    --   75.70 -99.00 -47.00   50
 14  \w     38.00  63.00   0.50    1.00    --   76.74 -99.00 -47.00   50
 15  \w     33.00  71.00   0.50    1.00    --   62.21 -99.00 -47.00   76
 16  \w     28.00  54.00   0.50    1.00    --   62.21 -95.00  30.00   52
 17  \w     63.00  92.00   0.50    1.00    --   80.75-100.00  -5.81   58
 18  \w     89.00 118.00   0.50    1.00    --   80.75 105.00 155.65   58
 19  \w     41.00  68.00   0.50    1.00    --   75.70 -95.00 150.00   54
 20  \w   -118.00 -93.00   0.50    1.00    --  -79.25 -67.00 -84.23   50
 21  \w   -124.00 -95.00   0.50    1.00    --  -79.25 -50.00-138.34   58
 22  \w    -65.00 -40.00   0.50    1.00    --  -79.25  58.00-178.36   50
 23  \w    -62.00 -37.00   0.50    1.00    --  -79.25  56.00  15.92   50
 24  \w    -93.00 -42.00   0.50    1.00    --  -74.80   0.00 120.00  102
 25  \w    -60.00 -34.00   0.50    1.00    --  -63.24  99.00  59.00   52
 26  \w    -84.00 -56.00   0.50    1.00    --  -74.80  99.00  59.00   56
 27  \w    -87.00 -62.00   0.50    1.00    --  -76.67  99.00  59.00   50
 28  \w    -77.00 -51.00   0.50    1.00    --  -79.25  98.00 -15.98   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0137323000
_diffrn_orient_matrix_UB_12      0.0585416000
_diffrn_orient_matrix_UB_13      0.0066688000
_diffrn_orient_matrix_UB_21      -0.0346499000
_diffrn_orient_matrix_UB_22      -0.0269599000
_diffrn_orient_matrix_UB_23      0.0838661000
_diffrn_orient_matrix_UB_31      0.0672726000
_diffrn_orient_matrix_UB_32      0.0419793000
_diffrn_orient_matrix_UB_33      0.0445594000
_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  0.0203
_diffrn_reflns_av_unetI/netI     0.0106
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            56592
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.780
_diffrn_reflns_theta_min         2.206
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.959
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.443
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.104a (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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.933
_exptl_crystal_description       block
_exptl_crystal_F_000             2184
_exptl_crystal_recrystallization_method 'slow evaporation from MeOH'
_exptl_crystal_size_max          0.342
_exptl_crystal_size_mid          0.228
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.226
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Flack x determined using 4248 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.019(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         10160
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0436
_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^)+(0.1055P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1270
_refine_ls_wR_factor_ref         0.1281
_reflns_Friedel_coverage         0.829
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.957
_reflns_number_gt                9704
_reflns_number_total             10160
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc05702g4.cif
_cod_data_source_block           catenaphyrin
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_primary' value 'diffmap' was changed
to 'difmap'.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7135153--7135154.cif.
;
_cod_original_cell_volume        7494(3)
_cod_database_code               7135154
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C17(H17A,H17B), C35(H35A,H35B), C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C24(H24), C26(H26), C22(H22), C27(H27), C3(H3), C6(H6), C36(H36),
 C12(H12), C15(H15), C9(H9), C16(H16), C19(H19), C20(H20), C7(H7), C30(H30),
 C34(H34), C31(H31), C33(H33), C13(H13), C2(H2)
2.c Idealised Me refined with riding coordinates:
 C38(H38A,H38B,H38C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              35224
_shelx_hkl_checksum              91924
_shelx_fab_checksum              12378
_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 1.174
_oxdiff_exptl_absorpt_empirical_full_min 0.852