Structural adaptation in a cadmium–porphyrin MOF through solvent-driven change of interpenetration
Ernst, Michelle; Poręba, Tomasz; CrystEngComm 27 (2025) 7032–7037; doi:10.1039/D5CE00815H

data_7250937
_publ_section_title
;
 Structural adaptation in a cadmium--porphyrin MOF through solvent-driven
 change of interpenetration
;
_journal_issue                   43
_journal_name_full               CrystEngComm
_journal_page_first              7032
_journal_page_last               7037
_journal_paper_doi               10.1039/D5CE00815H
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C40 H26 Cd Cl2 N8'
_chemical_formula_sum            'C40 H26 Cd Cl2 N8'
_chemical_formula_weight         801.99
_chemical_name_common            ESRF-1
_chemical_name_systematic
catena-[(m4-5,10,15,20-tetrakis(4-Pyridyl)porphyrin-N,N',N'',N''')-bis(chloro)-cadmium(ii)]
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-03-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-08-12 deposited with the CCDC.	2025-10-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8121(2)
_cell_length_b                   15.6630(2)
_cell_length_c                   20.3134(4)
_cell_measurement_reflns_used    4398
_cell_measurement_temperature    298(1)
_cell_measurement_theta_max      21.3600
_cell_measurement_theta_min      1.8450
_cell_volume                     4076.41(11)
_computing_cell_refinement       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.974
_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    -24.50  80.00   0.50    0.50    --    0.00   0.00   0.00  209
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0086777000
_diffrn_orient_matrix_UB_12      0.0098008000
_diffrn_orient_matrix_UB_13      0.0178860000
_diffrn_orient_matrix_UB_21      0.0196099000
_diffrn_orient_matrix_UB_22      -0.0203471000
_diffrn_orient_matrix_UB_23      0.0028355000
_diffrn_orient_matrix_UB_31      0.0237376000
_diffrn_orient_matrix_UB_32      0.0132239000
_diffrn_orient_matrix_UB_33      -0.0088977000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.40988
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_unetI/netI     0.0680
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15493
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        14.237
_diffrn_reflns_theta_max         14.843
_diffrn_reflns_theta_min         1.655
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.729
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.04419
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.116a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_recrystallization_method
'thermal desolvation of AGISUI at 393 K for 1.5h'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.307
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         4070
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0675
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1204P)^2^+7.0131P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2276
_refine_ls_wR_factor_ref         0.2327
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3415
_reflns_number_total             4070
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00815h2.cif
_cod_data_source_block           mof_amb_0023
_cod_depositor_comments          'Adding full bibliography for 7250937.cif.'
_cod_database_code               7250937
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.931
_reflns_odcompleteness_completeness 75.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     21.61
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Others
 Fixed Sof: H1(0.5) H2(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C4(H4), C19(H19), C22(H22), C3(H3), C21(H21), C9(H9),
 C18(H18), C8(H8), C17(H17), C16(H16), C13(H13), C14(H14)
;
_shelx_res_checksum              25213
_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 18.488
_oxdiff_exptl_absorpt_empirical_full_min 0.298