Unlocking porosity: structural tuning of urea-based MOFs via reaction parameter control
Esrafili, Leili; Cheung, Ocean; Adriaensens, Peter; Derveaux, Elien; Glasby, Lawson T.; Moghadam, Peyman Z.; Vande Velde, Christophe M. L.; RSC Advances 15 (2025) 27531–27543; doi:10.1039/D5RA02649K

data_7250763
_publ_section_title
;
 Unlocking porosity: structural tuning of urea-based MOFs via reaction
 parameter control
;
_journal_issue                   34
_journal_name_full               'RSC Advances'
_journal_page_first              27531
_journal_page_last               27543
_journal_paper_doi               10.1039/D5RA02649K
_journal_volume                  15
_journal_year                    2025
_chemical_absolute_configuration unk
_chemical_formula_moiety
'C13 H10 N3 O3.25 Zn, 1[C5H11N1O1], 0.333[C5H11N1O1]'
_chemical_formula_sum            'C19.67 H24.67 N4.33 O4.58 Zn'
_chemical_formula_weight         460.447
_chemical_name_systematic
di-Zinc-4,4'-(carbonylbis(azanediyl))dibenzoate;1,3-di(pyridin-4-yl)urea;hemioxide
_space_group_crystal_system      hexagonal
_space_group_IT_number           180
_space_group_name_Hall           'P 62 2 (0 0 4)'
_space_group_name_H-M_alt        'P 62 2 2'
_symmetry_Int_Tables_number      180
_audit_creation_date             2025-05-28
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7224)
;
_audit_update_record
;
2025-06-18 deposited with the CCDC.	2025-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   32.2989(8)
_cell_length_b                   32.2989(8)
_cell_length_c                   7.56433(19)
_cell_measurement_reflns_used    8918
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      73.3840
_cell_measurement_theta_min      4.1420
_cell_volume                     6834.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.76a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.76a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.76a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-alpha (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.9951
_diffrn_measured_fraction_theta_max 0.9672
_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     29.00  63.00   0.50    7.00    --   72.72-140.00   2.00   68
  2  \w     30.00  63.00   0.50    7.00    --   72.72-108.00 147.00   66
  3  \w     81.00 107.00   0.50    7.00    --   72.72-140.00   2.00   52
  4  \w     40.00  75.00   0.50    7.00    --   83.44-112.00   2.00   70
  5  \w     20.00  46.00   0.50    7.00    --   58.76 -95.00 -30.00   52
  6  \w     18.00  52.00   0.50    7.00    --   58.76 -95.00-150.00   68
  7  \w     37.00  66.00   0.50    7.00    --   72.72 -95.00 -30.00   58
  8  \w   -116.00 -57.00   0.50    7.00    --  -74.45 -15.00  90.00  118
  9  \w    -65.00 -39.00   0.50    7.00    --  -74.77 108.00-114.00   52
 10  \w     88.00 129.00   0.50    7.00    --   83.44  15.00 120.00   82
 11  \w     57.00 130.00   0.50    7.00    --   83.44  15.00   0.00  146
 12  \w     50.00  77.00   0.50    7.00    --   83.44 -95.00  90.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0512347000
_diffrn_orient_matrix_UB_12      0.0211309000
_diffrn_orient_matrix_UB_13      -0.0721957000
_diffrn_orient_matrix_UB_21      0.0153925000
_diffrn_orient_matrix_UB_22      0.0462095000
_diffrn_orient_matrix_UB_23      0.1056104000
_diffrn_orient_matrix_UB_31      0.0130910000
_diffrn_orient_matrix_UB_32      -0.0211458000
_diffrn_orient_matrix_UB_33      0.1584469000
_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  0.0431
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.9951
_diffrn_reflns_Laue_measured_fraction_max 0.9672
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            25516
_diffrn_reflns_point_group_measured_fraction_full 0.9966
_diffrn_reflns_point_group_measured_fraction_max 0.9604
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         75.70
_diffrn_reflns_theta_min         4.18
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.795
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52182
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.76a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_description       needle
_exptl_crystal_F_000             2866.216
_exptl_crystal_recrystallization_method 'solvothermal synthesis in DEF'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.4217
_refine_diff_density_min         -0.8246
_refine_diff_density_rms         0.0512
_refine_ls_abs_structure_details
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   -0.023(15)
_refine_ls_d_res_high            0.7956
_refine_ls_d_res_low             10.5723
_refine_ls_goodness_of_fit_ref   0.9881
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    20
_refine_ls_number_parameters     186
_refine_ls_number_reflns         4580
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.9881
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+1.5648P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.0903
_reflns_Friedel_coverage         0.951
_reflns_limit_h_max              34
_reflns_limit_h_min              -34
_reflns_limit_k_max              19
_reflns_limit_k_min              -19
_reflns_limit_l_max              8
_reflns_limit_l_min              -8
_reflns_number_gt                3990
_reflns_number_total             4580
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5ra02649k1.cif
_cod_data_source_block           UA3_TMU31_dDEF_RigSynR
_cod_original_sg_symbol_Hall     ' P 62 2 (0 0 4)'
_cod_original_formula_sum        'C19.67 H24.67 N4.33 O4.58 Zn1'
_cod_database_code               7250763
_diffrn_oxdiff_digest_hkl
;
01f745a0b51d1d154fc7898d29b776def66321
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C3(H3), C4(H4), C6(H6), C7(H7), N52(H52), C52(H52a), C53(H53),
 C55(H55), C56(H56)
;
_platon_squeeze_special_details
;
A solvent mask was calculated and 854 electrons were 
found in a volume of 3436\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
1[C5H11N1O1], 0.333[C5H11N1O1] per Unit Cell 
which account for 896 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_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 1.651
_oxdiff_exptl_absorpt_empirical_full_min 0.558