Exfoliation of a metal-organic framework enabled by post-synthetic cleavage of a dipyridyl dianthracene ligand.
Logelin, Madison E.; Schreiber, Eric; Mercado, Brandon Q.; Burke, Michael J.; Davis, Caitlin M.; Bartholomew, Amymarie K.; Chemical science 15 (2024) 15198–15204; doi:10.1039/d4sc03524k

data_1572773
_publ_section_title
;
 Exfoliation of a metal-organic framework enabled by post-synthetic
 cleavage of a dipyridyl dianthracene ligand.
;
_journal_issue                   37
_journal_name_full               'Chemical science'
_journal_page_first              15198
_journal_page_last               15204
_journal_paper_doi               10.1039/d4sc03524k
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C66 H44 N4 O12 Zn3, 4(C3 H7 N O)'
_chemical_formula_sum            'C78 H72 N8 O16 Zn3'
_chemical_formula_weight         1573.54
_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
_audit_creation_date             2024-03-21
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-03-21 deposited with the CCDC.	2024-08-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.915(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   23.3813(11)
_cell_length_b                   8.8522(4)
_cell_length_c                   18.8122(9)
_cell_measurement_reflns_used    15369
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      63.9720
_cell_measurement_theta_min      2.0170
_cell_volume                     3612.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.112a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.92a 64-bit (release 05-10-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.112a (Rigaku OD, 2024)'
_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)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.976
_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    -48.00 132.00   2.00    4.00    --   42.00   0.00   0.00   90
  2  \w    -48.00 132.00   2.00    4.00    --   42.00   0.00 180.00   90
  3  \w    -48.00 132.00   2.00    4.00    --   42.00  54.00 220.00   90
  4  \w    -48.00 132.00   2.00    4.00    --   42.00  54.00  55.00   90
  5  \w    -48.00 132.00   2.00    4.00    --   42.00  54.00 320.00   90
  6  \w    -48.00 132.00   2.00    4.00    --   42.00  54.00 110.00   90
  7  \w    -48.00 132.00   2.00    4.00    --   42.00  54.00   0.00   90
  8  \w    -48.00 132.00   2.00    4.00    --   42.00  54.00 275.00   90
  9  \w    -48.00 132.00   2.00    4.00    --   42.00  54.00 200.00   90
 10  \w    -48.00 132.00   2.00    4.00    --   42.00  54.00 180.00   90
 11  \w    -48.00 132.00   2.00    4.00    --   42.00  54.00 165.00   90
 12  \w      0.00 180.00   2.00   35.00    --   90.00   0.00   0.00   90
 13  \w      0.00 180.00   2.00   35.00    --   90.00   0.00 180.00   90
 14  \w      0.00 180.00   2.00   35.00    --   90.00  54.00  50.00   90
 15  \w      0.00 180.00   2.00   35.00    --   90.00  54.00 125.00   90
 16  \w      0.00 180.00   2.00   35.00    --   90.00  54.00 225.00   90
 17  \w      0.00 180.00   2.00   35.00    --   90.00  54.00 300.00   90
 18  \w      0.00 180.00   2.00   35.00    --   90.00  54.00 250.00   90
 19  \w      0.00 180.00   2.00   35.00    --   90.00  54.00 150.00   90
 20  \w      0.00 180.00   2.00   35.00    --   90.00  54.00  75.00   90
 21  \w      0.00 180.00   2.00   35.00    --   90.00  54.00 350.00   90
 22  \w      0.00 166.00   2.00   35.00    --   90.00  54.00  25.00   83
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0056752000
_diffrn_orient_matrix_UB_12      0.1608775000
_diffrn_orient_matrix_UB_13      0.0332356000
_diffrn_orient_matrix_UB_21      0.0005583000
_diffrn_orient_matrix_UB_22      0.0652175000
_diffrn_orient_matrix_UB_23      -0.0757122000
_diffrn_orient_matrix_UB_31      -0.0707282000
_diffrn_orient_matrix_UB_32      0.0134874000
_diffrn_orient_matrix_UB_33      -0.0309589000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1685
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            97198
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.802
_diffrn_reflns_theta_min         2.037
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.782
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.112a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_description       plate
_exptl_crystal_F_000             1628
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.005
_refine_diff_density_max         1.240
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         6548
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1297
_refine_ls_R_factor_gt           0.0788
_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^)+(0.0901P)^2^+10.1953P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1936
_refine_ls_wR_factor_ref         0.2230
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3941
_reflns_number_total             6548
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03524k2.cif
_cod_data_source_block           Zn3BDC3diAnCNC-3Py
_cod_database_code               1572773
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C78H72N8O16Zn3
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.916
_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:
 C15(H15)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C7(H7), C10(H10), C11(H11), C12(H12),
 C13(H13), C17(H17), C18(H18), C19(H19), C20(H20), C24(H24), C25(H25), C28(H28),
  C29(H29), C32(H32), C33(H33), C34(H34), C37(H37)
2.d Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C39(H39A,H39B,
 H39C)
;
_shelx_res_checksum              23019
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.099
_oxdiff_exptl_absorpt_empirical_full_min 0.536