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_1572774
_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'
_chemical_formula_sum            'C66 H44 N4 O12 Zn3'
_chemical_formula_weight         1281.26
_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             2024-05-08
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-05-17 deposited with the CCDC.	2024-08-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.7(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.9(5)
_cell_length_b                   9.5(2)
_cell_length_c                   18.2(3)
_cell_measurement_reflns_used    444
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      0.8230
_cell_measurement_theta_min      0.0800
_cell_volume                     2912(12)
_computing_cell_refinement       'CrysAlisPro 1.171.43.115a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.121a 64-bit (release 24-04-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.115a (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 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix-ED
_diffrn_measured_fraction_theta_full 0.874
_diffrn_measured_fraction_theta_max 0.874
_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    -60.00  55.00   0.20    0.20    --    0.00   0.00   0.00  575
  2  \w    -50.00  50.00   0.10    0.20    --    0.00   0.00   0.00 1000
  3  \w     -5.00  50.00   0.50    0.50    --    0.00   0.00   0.00  110
;
_diffrn_measurement_device       'electron diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy-ED, HyPix-ED, electron source at 200keV'
_diffrn_measurement_method       'continuous rotation electron diffraction'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0013442000
_diffrn_orient_matrix_UB_12      0.0001249000
_diffrn_orient_matrix_UB_13      0.0004974000
_diffrn_orient_matrix_UB_21      -0.0005443000
_diffrn_orient_matrix_UB_22      0.0012336000
_diffrn_orient_matrix_UB_23      -0.0011504000
_diffrn_orient_matrix_UB_31      -0.0003594000
_diffrn_orient_matrix_UB_32      -0.0023282000
_diffrn_orient_matrix_UB_33      -0.0005861000
_diffrn_radiation_monochromator  none
_diffrn_radiation_probe          electron
_diffrn_radiation_type           electron
_diffrn_radiation_wavelength     0.0251
_diffrn_reflns_av_R_equivalents  0.2226
_diffrn_reflns_av_unetI/netI     0.1803
_diffrn_reflns_Laue_measured_fraction_full 0.874
_diffrn_reflns_Laue_measured_fraction_max 0.874
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13047
_diffrn_reflns_point_group_measured_fraction_full 0.874
_diffrn_reflns_point_group_measured_fraction_max 0.874
_diffrn_reflns_theta_full        0.666
_diffrn_reflns_theta_max         0.666
_diffrn_reflns_theta_min         0.079
_diffrn_source                   'electron diffractometer'
_diffrn_source_type              'JEOL JSM-2300ED, LaB6'
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.13414
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.115a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_description       plate
_exptl_crystal_F_000             479
_exptl_crystal_size_max          0.0001
_exptl_crystal_size_mid          0.0001
_exptl_crystal_size_min          0.0001
_refine_diff_density_max         0.236
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       124(30)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         2112
_refine_ls_number_restraints     282
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.2839
_refine_ls_R_factor_gt           0.2263
_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^+20.4742P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5061
_refine_ls_wR_factor_ref         0.5386
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1389
_reflns_number_total             2112
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03524k2.cif
_cod_data_source_block           Zn3BDC3(AnCNC-3Py)2
_cod_original_cell_volume        2910(118)
_cod_database_code               1572774
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Zn O N C'
_diffrn_oxdiff_scatteringfactors_ed
'UCLA (2022) https://srv.mbi.ucla.edu/faes/data'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.002 and sigma
for terminal atoms of 0.004 within 2A
3.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C5(H5), C7(H7), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C20(H20), C19(H19), C18(H18), C17(H17), C24(H24), C25(H25),
  C27(H27), C28(H28), C32(H32), C33(H33)
3.c Fitted hexagon refined as free rotating group:
 C21(C20,C19,C18,C17,C16)
;
_shelx_res_checksum              20107
_olex2_exptl_crystal_mounting_method
;
Data collected from 3 crystals were used to refine the model associated with 
this CIF.
;
_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 3.604
_oxdiff_exptl_absorpt_empirical_full_min 0.279