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_7134343
_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      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     iterative
_audit_creation_date             2025-03-04
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-03-05 deposited with the CCDC.	2025-03-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.130(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.7931(4)
_cell_length_b                   14.9960(3)
_cell_length_c                   16.0649(3)
_cell_measurement_reflns_used    5583
_cell_measurement_temperature    296.12(10)
_cell_measurement_theta_max      70.2830
_cell_measurement_theta_min      4.1900
_cell_volume                     3941.95(17)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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
;
Superflip  (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      296.12(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.977
_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     20.00  60.00   1.00    2.50    --    0.00  57.00-120.00   40
  2  \w    -20.00  14.00   1.00    2.50    --    0.00  57.00-120.00   34
  3  \w    -51.00  -5.00   1.00    2.50    --    0.00 127.00-164.00   46
  4  \w     31.00  56.00   1.00    2.50    --    0.00  57.00-180.00   25
  5  \w      1.00  96.00   1.00    5.00    --   53.63 -99.00-150.00   95
  6  \w     22.00 119.00   1.00    5.00    --   53.63  77.00 -30.00   97
  7  \w      3.00  47.00   1.00    5.00    --   53.63 -57.00-150.00   44
  8  \w     69.00 123.00   1.00    5.00    --   53.63  57.00  30.00   54
  9  \w     35.00 112.00   1.00    5.00    --  107.26-111.00  30.00   77
 10  \w     35.00 112.00   1.00    5.00    --  107.26-111.00-180.00   77
 11  \w     49.00 101.00   1.00    5.00    --  107.26-111.00-120.00   52
 12  \w     73.00 176.00   1.00    5.00    --  107.26  25.00 -60.00  103
 13  \w     71.00  97.00   1.00    5.00    --  107.26-111.00 -60.00   26
 14  \w    104.00 142.00   1.00    5.00    --  107.26 111.00  60.00   38
 15  \w     35.00 117.00   1.00    5.00    --  107.26 -38.00 120.00   82
 16  \w    107.00 135.00   1.00    5.00    --  107.26 111.00 120.00   28
 17  \w     47.00 114.00   1.00    5.00    --  107.26 -50.00 -30.00   67
;
_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      0.0872420000
_diffrn_orient_matrix_UB_12      0.0381982000
_diffrn_orient_matrix_UB_13      0.0331799000
_diffrn_orient_matrix_UB_21      -0.0348531000
_diffrn_orient_matrix_UB_22      0.0953497000
_diffrn_orient_matrix_UB_23      -0.0107327000
_diffrn_orient_matrix_UB_31      0.0059837000
_diffrn_orient_matrix_UB_32      -0.0025098000
_diffrn_orient_matrix_UB_33      0.0982775000
_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  0.0345
_diffrn_reflns_av_unetI/netI     0.0596
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15488
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.744
_diffrn_reflns_theta_min         3.999
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.925
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62262
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       block
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.085
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         7411
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0662
_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^)+(0.0904P)^2^+3.1930P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1754
_refine_ls_wR_factor_ref         0.1995
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5498
_reflns_number_total             7411
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc00829h2.cif
_cod_data_source_block           UPC-HOF-12
_cod_depositor_comments
'Adding full bibliography for 7134343--7134344.cif.'
_cod_original_cell_volume        3941.94(16)
_cod_database_code               7134343
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O Co'
_shelx_estimated_absorpt_t_max   0.695
_shelx_estimated_absorpt_t_min   0.695
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Uiso/Uaniso restraints and constraints
Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36)
\\sim Ueq, Uanis(C37) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.01
3.a Ternary CH refined with riding coordinates:
 C36(H36), C35(H35)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4A), C19(H19), C22(H22), C23(H23), C3(H3), C11(H11), C15(H15), C31(H31),
 C20(H20), C6(H6), C30(H30), C12(H12), C14(H14), C7(H7), C28(H28), C27(H27),
 C41(H41), C33(H33), C37(H37), C34(H34), C40(H40)
3.c Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C38(H38A,H38B,H38C), C39(H39A,H39B,
 H39C)
3.d Idealised tetrahedral OH refined as rotating group:
 O8(H8), O5(H5), O4(H4), O2(H2)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              62202
_shelx_hkl_checksum              43508
_shelx_fab_checksum              28322
_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 2.245
_oxdiff_exptl_absorpt_empirical_full_min 0.773