Solvent-etching-induced in situ crystal structure transformation in hydrogen-bonded organic frameworks
Wang, Xiaokang; Liu, Hongyan; Sun, Meng; Gao, Fei; Feng, Xueying; Xu, Mingming; Wang, Yutong; Fan, Weidong; Sun, Daofeng; Chemical Communications 61 (2025) 6166–6169; doi:10.1039/D5CC00829H

data_7134344
_publ_section_title
;
 Solvent-etching-induced in situ crystal structure transformation in
 hydrogen-bonded organic frameworks
;
_journal_issue                   33
_journal_name_full               'Chemical Communications'
_journal_page_first              6166
_journal_page_last               6169
_journal_paper_doi               10.1039/D5CC00829H
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C37 H25 Co O8, 2(C3 H7 N O)'
_chemical_formula_sum            'C43 H39 Co N2 O10'
_chemical_formula_weight         802.69
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-03-04
_audit_creation_method
;
Olex2 1.5
(compiled 2025.02.27 svn.r83f5de26 for OlexSys, GUI svn.r7172)
;
_audit_update_record
;
2025-03-05 deposited with the CCDC.	2025-03-21 downloaded from the CCDC.
;
_cell_angle_alpha                74.105(4)
_cell_angle_beta                 88.003(3)
_cell_angle_gamma                71.393(4)
_cell_formula_units_Z            2
_cell_length_a                   11.4687(5)
_cell_length_b                   13.0070(6)
_cell_length_c                   14.1101(5)
_cell_measurement_reflns_used    6162
_cell_measurement_temperature    294.2(3)
_cell_measurement_theta_max      70.4780
_cell_measurement_theta_min      3.7220
_cell_volume                     1915.37(15)
_computing_cell_refinement       'CrysAlisPro 1.171.43.137a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.137a 64-bit (release 10-09-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.137a (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)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      294.2(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.981
_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    -72.00  -9.00   1.00    1.09    --    0.00 -43.00 148.00   63
  2  \w    -22.00   5.00   1.00    1.09    --    0.00 -43.00 148.00   27
  3  \w    -16.00  59.00   1.00    4.37    --   53.63 -43.00 148.00   75
  4  \w     30.00 101.00   1.00    4.37    --   53.63  43.00 -60.00   71
  5  \w     45.00  93.00   1.00    4.37    --  107.26 -43.00 148.00   48
  6  \w     91.00 178.00   1.00    4.37    --  107.26  43.00 -60.00   87
  7  \w    -16.00  25.00   1.00    1.09    --    0.00  43.00 -60.00   41
  8  \w    -16.00  11.00   1.00    1.09    --    0.00 -77.00  60.00   27
  9  \w    -21.00  30.00   1.00    1.09    --    0.00 -77.00 -90.00   51
 10  \w     24.00  74.00   1.00    4.37    --   53.63 -38.00  30.00   50
 11  \w    -14.00  70.00   1.00    4.37    --   53.63 -57.00   0.00   84
 12  \w     32.00  89.00   1.00    4.37    --   53.63-125.00   0.00   57
 13  \w     53.00  80.00   1.00    4.37    --   53.63-125.00-120.00   27
 14  \w     39.00 102.00   1.00    4.37    --   53.63-125.00-180.00   63
 15  \w     58.00 122.00   1.00    4.37    --   53.63  70.00 -49.92   64
 16  \w     73.00 116.00   1.00    4.37    --   53.63  57.00-150.00   43
 17  \w     -6.00  20.00   1.00    4.37    --   53.63 -38.00  30.00   26
 18  \w    108.00 163.00   1.00    4.37    --  107.26 111.00-150.00   55
 19  \w     83.00 174.00   1.00    4.37    --  107.26  38.00-150.00   91
 20  \w     39.00 105.00   1.00    4.37    --  107.26-111.00-180.00   66
 21  \w    111.00 175.00   1.00    4.37    --  107.26  77.00 150.00   64
 22  \w     35.00  81.00   1.00    4.37    --  107.26 -91.00-180.00   46
 23  \w     80.00 129.00   1.00    4.37    --  107.26-178.00  90.00   49
 24  \w    153.00 178.00   1.00    4.37    --  107.26  50.00 -90.00   25
 25  \w     84.00 124.00   1.00    4.37    --  107.26  50.00 -90.00   40
 26  \w     53.00 101.00   1.00    4.37    --  107.26 -91.00  30.00   48
 27  \w     80.00 106.00   1.00    4.37    --  107.26-111.00 120.00   26
 28  \w    121.00 151.00   1.00    4.37    --  107.26-178.00  60.00   30
 29  \w     60.00 101.00   1.00    4.37    --  107.26-178.00  60.00   41
 30  \w     76.00 102.00   1.00    4.37    --  107.26-178.00 -30.00   26
 31  \w    116.00 150.00   1.00    4.37    --  107.26-178.00 -30.00   34
 32  \w     82.00 108.00   1.00    4.37    --  107.26-111.00   0.00   26
 33  \w     41.00 130.00   1.00    4.37    --  107.26 -63.00-150.00   89
 34  \w    104.00 175.00   1.00    4.37    --  107.26 111.00-120.00   71
 35  \w    120.00 166.00   1.00    4.37    --  107.26 111.00-180.00   46
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0614610000
_diffrn_orient_matrix_UB_12      0.0907200000
_diffrn_orient_matrix_UB_13      -0.0439529000
_diffrn_orient_matrix_UB_21      0.0987809000
_diffrn_orient_matrix_UB_22      -0.0848560000
_diffrn_orient_matrix_UB_23      -0.0422856000
_diffrn_orient_matrix_UB_31      -0.0813689000
_diffrn_orient_matrix_UB_32      0.0385975000
_diffrn_orient_matrix_UB_33      -0.0959702000
_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  0.0276
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14237
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.576
_diffrn_reflns_theta_min         3.732
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.039
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79695
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.137a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'yellowish brown'
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         7199
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0464P)^2^+0.7873P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1160
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6031
_reflns_number_total             7199
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc00829h2.cif
_cod_data_source_block           UPC-HOF-13
_cod_depositor_comments
'Adding full bibliography for 7134343--7134344.cif.'
_cod_database_code               7134344
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Co'
_shelx_estimated_absorpt_t_max   0.688
_shelx_estimated_absorpt_t_min   0.688
_diffrn_oxdiff_ac3_digest_hkl    410090820b25769637a838b51d520628707e1f
_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, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C22(H22), C14(H14), C28(H28), C20(H20), C27(H27), C15(H15), C6(H6A), C23(H23),
  C11(H11), C3(H3), C12(H12), C4(H4A), C19(H19), C31(H31), C7(H7), C30(H30),
 C34(H34), C38(H38), C35(H35), C33(H33), C37(H37), C36(H36), C41(H41)
2.b Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C39(H39A,H39B,H39C), C43(H43A,H43B,H43C), C42(H42A,H42B,
 H42C)
2.c Idealised tetrahedral OH refined as rotating group:
 O6(H6), O8(H8), O2(H2)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              2177
_shelx_hkl_checksum              42721
_shelx_fab_checksum              61038
_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 1.526
_oxdiff_exptl_absorpt_empirical_full_min 0.681