Perylenediimide-based metal-organic frameworks: structural, electrochemical and spectroelectrochemical characterisation.
Ogar, Joseph O.; Davies, E. Stephen; Almuhana, Asia R. Y.; Griffin, Sarah L.; Addicoat, Matthew A.; Argent, Stephen P.; Champness, Neil R.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 16049–16055; doi:10.1039/d5dt02244d

data_7719537
_publ_section_title
;
 Perylenediimide-based metal-organic frameworks: structural,
 electrochemical and spectroelectrochemical characterisation.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16049
_journal_page_last               16055
_journal_paper_doi               10.1039/d5dt02244d
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C164 H120 Co4 N8 O24'
_chemical_formula_sum            'C186.5 H176.5 Co4 N15.5 O31.5'
_chemical_formula_weight         3374.64
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc2k0b86
_audit_creation_date             2022-05-23
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-05-07 deposited with the CCDC.	2025-10-02 downloaded from the CCDC.
;
_cell_angle_alpha                85.58(3)
_cell_angle_beta                 88.50(2)
_cell_angle_gamma                89.20(4)
_cell_formula_units_Z            1
_cell_length_a                   12.677(4)
_cell_length_b                   13.196(5)
_cell_length_c                   31.941(8)
_cell_measurement_reflns_used    1859
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      21.0576079155
_cell_measurement_theta_min      0.681147792963
_cell_volume                     5325(3)
_computing_cell_refinement
'DIALS 2theta refinement, DIALS 2.1.4-ga615ced2f-release'
_computing_data_collection       'GDA - generic data acquisition software'
_computing_data_reduction
;
DIALS 2.1.4-ga615ced2f-release (Winter, G. et al., 2018)
XIA2 0.6.380-g0f31cbd4-dials-2.1 (Winter, G., 2010)
;
_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    'XT  (Sheldrick, 2015)'
_diffrn_ambient_environment      'N2 gas'
_diffrn_ambient_temperature      100(1)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_type            'Dectris PILATUS 2M'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'Fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.1009
_diffrn_reflns_av_unetI/netI     0.0728
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            28141
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        18.247
_diffrn_reflns_theta_max         18.247
_diffrn_reflns_theta_min         0.620
_diffrn_source                   Synchrotron
_diffrn_source_details           'Allan et al. (2017)'
_diffrn_source_type              'Diamond Light Source Beamline I19-1'
_exptl_absorpt_coefficient_mu    0.341
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.9850311958473146
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
DIALS 2.1.4-ga615ced2f-release
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.052
_exptl_crystal_description       plate
_exptl_crystal_F_000             1764
_exptl_crystal_size_max          0.045
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.419
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.717
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     901
_refine_ls_number_reflns         8259
_refine_ls_number_restraints     1694
_refine_ls_restrained_S_all      1.600
_refine_ls_R_factor_all          0.1830
_refine_ls_R_factor_gt           0.1666
_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          0.4204
_refine_ls_wR_factor_ref         0.4394
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5608
_reflns_number_total             8259
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02244d2.cif
_cod_data_source_block           cojoql_a1
_cod_depositor_comments
'Adding full bibliography for 7719536--7719537.cif.'
_cod_original_cell_volume        5325(2)
_cod_original_formula_sum        'C186.50 H176.50 Co4 N15.50 O31.50'
_cod_database_code               7719537
_nottingham_internal_coll_name   COJOQL
_nottingham_internal_coll_number 18601
_nottingham_internal_coll_client JO/NRC
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'fine \w scans'
_nottingham_internal_coll_frame_time 0.2
_nottingham_internal_coll_frame_width 0.01
_nottingham_internal_coll_user   pczspa
_nottingham_internal_coll_date   05/03/2020
_nottingham_internal_coll_location DLS
_nottingham_internal_coll_instrument i19-EH1
_nottingham_internal_process_date 05/03/2020
_nottingham_internal_process_user pczspa/pcxjo3
_nottingham_internal_solution_date 05/03/2020
_nottingham_internal_solution_user pczspa/pcxjo3
_nottingham_internal_refinement_date 23/05/2022
_nottingham_internal_refinement_user pczspa/pcxjo3
_nottingham_internal_validation_date 23/05/2022
_nottingham_internal_validation_user pczspa
_nottingham_internal_archive_date 23/05/2022
_platon_squeeze_void_probe_radius 1.20
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.985
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C64C-C34C
 1.5 with sigma of 0.02
 C16B-C14B \\sim C26B-C24B \\sim C16A-C14A \\sim C26A-C24A
 with sigma of 0.02
 C15B-C14B \\sim C25B-C24B
 with sigma of 0.02
 C14A-C13A \\sim C24A-C23A \\sim C14B-C13B \\sim C24B-C23B
 with sigma of 0.02
 C17D-C11C \\sim C17C-C11D
 with sigma of 0.02
 C16D-C15D \\sim C16C-C15C
 with sigma of 0.02
 O27A-C26A \\sim O17A-C16A \\sim O27B-C26B \\sim O17B-C16B
 with sigma of 0.02
 O28B-C26B \\sim O18B-C16B \\sim O18A-C16A \\sim O28A-C26A
 with sigma of 0.02
 C19D-C18D \\sim C13D-C12D \\sim C19C-C18C \\sim C13C-C12C
 with sigma of 0.02
 C22A-C21A \\sim C12A-C11A \\sim C12B-C11B \\sim C22B-C21B
 with sigma of 0.02
 C51D-C32D \\sim C41D-C36D \\sim C51C-C32C \\sim C41C-C36C
 with sigma of 0.02
 C13B-C12B \\sim C23B-C22B \\sim C23A-C22A \\sim C13A-C12A
 with sigma of 0.02
 C43D-C41D \\sim C42D-C41D \\sim C52D-C51D \\sim C42C-C41C \\sim C43C-C41C
\\sim C52C-C51C \\sim C53C-
 C51C
 with sigma of 0.02
 C53D-C51D \\sim C52D-C51D \\sim C43D-C41D \\sim C42D-C41D \\sim C42C-C41C
\\sim C43C-C41C \\sim C53C-
 C51C \\sim C52C-C51C
 with sigma of 0.02
 C21B-C11B \\sim C21A-C11A
 with sigma of 0.02
 C21A-C15A \\sim C25A-C11A \\sim C25B-C11B \\sim C21B-C15B
 with sigma of 0.02
 Co1-O18A \\sim Co2-O17B
 with sigma of 0.02
 Co1-O18B \\sim Co2-O17A
 with sigma of 0.02
 C16B-O17B \\sim O18A-C16A
 with sigma of 0.02
 O18B-C16B \\sim O17A-C16A
 with sigma of 0.02
 C21D-C20D \\sim C24D-C14D \\sim C21C-C20C \\sim C24C-C14C
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(O28A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. 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
5. Same fragment restrains
{C17C, C18C, C19C, C20C, C15C, C16C, C11C, C12C, C13C, C14C, C24C, O25C, N23C,
C21C, O22C, C31C, C36C, C35C, C34C, C33C, C32C, C51C, C53C, C52C, C41C, C43C,
C42C, N61C, C66C, C65C, C64C, C63C, C62C} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C11C, C12C, C13C, C14C, C15C, C16C, C17C, C18C, C19C, C20C, C21C, O22C, N23C,
C24C, O25C, C31C, C32C, C33C, C34C, C35C, C36C, C41C, C42C, C43C, C51C, C52C,
C53C, N61C, C62C, C63C, C64C, C65C, C66C}
6.a Ternary CH refined with riding coordinates:
 C41C(H41C), C51C(H51C), C41D(H41D), C51D(H51D)
6.b Me refined with riding coordinates:
 C42C(H42A,H42B,H42C), C43C(H43A,H43B,H43C), C52C(H52A,H52B,H52C), C53C(H53A,
 H53B,H53C), C42D(H42D,H42E,H42F), C43D(H43D,H43E,H43F), C52D(H52D,H52E,H52F),
 C53D(H53D,H53E,H53F)
6.c Aromatic/amide H refined with riding coordinates:
 C12A(H12A), C13A(H13A), C15A(H15A), C22A(H22A), C23A(H23A), C25A(H25A),
 C12B(H12B), C13B(H13B), C15B(H15B), C22B(H22B), C23B(H23B), C25B(H25B),
 C12C(H12C), C13C(H13C), C18C(H18C), C19C(H19C), C33C(H33C), C35C(H35C),
 C62C(H62C), C63C(H63C), C65C(H65C), C66C(H66C), C12D(H12D), C13D(H13D),
 C18D(H18D), C19D(H19D), C33D(H33D), C35D(H35D), C62D(H62D), C63D(H63D),
 C65D(H65D), C66D(H66D)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              90991
_shelx_hkl_checksum              72037
_shelx_fab_checksum              42236
_olex2_submission_special_instructions 'No special instructions were received'