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_7250764
_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
'C52 H40 N12 O13 Zn4, 6.333[C1H3N1O2], 2.667[C1H3N1O2]'
_chemical_formula_sum            'C61 H67 N21 O31 Zn4'
_chemical_formula_weight         1851.917
_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
;
2025-07-04 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            3
_cell_length_a                   32.347(3)
_cell_length_b                   32.347(3)
_cell_length_c                   7.5375(10)
_cell_measurement_reflns_used    9582
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.355
_cell_measurement_theta_min      4.174
_cell_volume                     6830.1(13)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.9988
_diffrn_measured_fraction_theta_max 0.9989
_diffrn_measurement_device_type  'Bruker D8 4-circle goniometer'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_unetI/netI     0.0154
_diffrn_reflns_Laue_measured_fraction_full 0.9988
_diffrn_reflns_Laue_measured_fraction_max 0.9989
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            78568
_diffrn_reflns_point_group_measured_fraction_full 0.9993
_diffrn_reflns_point_group_measured_fraction_max 0.9994
_diffrn_reflns_theta_full        67.6786
_diffrn_reflns_theta_max         74.42
_diffrn_reflns_theta_min         4.18
_exptl_absorpt_coefficient_mu    1.923
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.6167
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            'light brown'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_description       needle
_exptl_crystal_F_000             2835.871
_exptl_crystal_recrystallization_method
'solvothermal synthesis, solvent exchange with nitromethane'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.008
_refine_diff_density_max         0.1778
_refine_diff_density_min         -0.2503
_refine_diff_density_rms         0.0297
_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   -0.040(7)
_refine_ls_d_res_high            0.8003
_refine_ls_d_res_low             10.5881
_refine_ls_goodness_of_fit_ref   1.0210
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    20
_refine_ls_number_parameters     186
_refine_ls_number_reflns         4692
_refine_ls_number_restraints     309
_refine_ls_restrained_S_all      0.9877
_refine_ls_R_factor_all          0.0220
_refine_ls_R_factor_gt           0.0214
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0347P)^2^+0.9190P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0589
_reflns_Friedel_coverage         1.000
_reflns_limit_h_max              35
_reflns_limit_h_min              -34
_reflns_limit_k_max              20
_reflns_limit_k_min              -19
_reflns_limit_l_max              9
_reflns_limit_l_min              -9
_reflns_number_gt                4580
_reflns_number_total             4692
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5ra02649k1.cif
_cod_data_source_block           2024S007_UA_3_EX_NM_a
_cod_original_cell_volume        6830.1(12)
_cod_original_sg_symbol_Hall     ' P 62 2 (0 0 4)'
_cod_database_code               7250764
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.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 834 electrons were 
found in a volume of 3455\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
6.333[C1H3N1O2], 2.667[C1H3N1O2] per Unit Cell 
which account for 864 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'