Linker desymmetrisation unlocks new topologies, defective clusters, and catalytic activity in zirconium- and rare-earth metal-organic frameworks.
Ortín-Rubio, Borja; Yang, Yunhui; Borrego-Marin, Emilio; Rostoll-Berenguer, Jaume; Vila, Carlos; Juanhuix, Judith; Imaz, Inhar; Navarro, Jorge A. R.; Maspoch, Daniel; Chemical science 16 (2025) 21600–21613; doi:10.1039/d5sc05365j

data_1576034
_publ_section_title
;
 Linker desymmetrisation unlocks new topologies, defective clusters, and
 catalytic activity in zirconium- and rare-earth metal-organic frameworks.
;
_journal_issue                   45
_journal_name_full               'Chemical science'
_journal_page_first              21600
_journal_page_last               21613
_journal_paper_doi               10.1039/d5sc05365j
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C52 H22 O16 Zr3'
_chemical_formula_sum            'C52 H22 O16 Zr3'
_chemical_formula_weight         1176.396
_space_group_crystal_system      orthorhombic
_space_group_IT_number           65
_space_group_name_Hall           '-C 2 2'
_space_group_name_H-M_alt        'C m m m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-07-15
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_audit_update_record
;
2025-07-15 deposited with the CCDC.	2025-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.1486(10)
_cell_length_b                   34.1491(10)
_cell_length_c                   24.7133(5)
_cell_measurement_reflns_used    99212
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.360
_cell_measurement_theta_min      1.401
_cell_volume                     17848.1(11)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'pilatus DECTRIS 6M'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.82653
_diffrn_reflns_av_R_equivalents  0.0758
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_Laue_measured_fraction_full 0.951
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            99212
_diffrn_reflns_point_group_measured_fraction_full 0.951
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.360
_diffrn_reflns_theta_min         1.401
_exptl_absorpt_coefficient_mu    0.283
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    0.438
_exptl_crystal_description       prism
_exptl_crystal_F_000             2296
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.877
_refine_diff_density_min         -1.457
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         8350
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.1280
_refine_ls_R_factor_gt           0.0937
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2772
_refine_ls_wR_factor_ref         0.3110
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5380
_reflns_number_total             8350
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc05365j3.cif
_cod_data_source_block           shelx_sqd
_cod_depositor_comments
'Adding full bibliography for 1576030--1576035.cif.'
_cod_database_code               1576034
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C6-C5
 1.35 with sigma of 0.02
 C6-C45
 2.2 with sigma of 0.02
 C3-C6
 2.2 with sigma of 0.02
 C6-C3
 2.4 with sigma of 0.02
 C3-C5
 1.45 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uiso(C45) = Uiso(C5)
Uiso(C5) = Uiso(C45)
Uiso(C1) = Uiso(C45) = Uiso(C6) = Uiso(C5)
Uiso(C1) = Uiso(C5) = Uiso(C6) = Uiso(C45)
Uiso(C3) = Uiso(C1) = Uiso(C6) = Uiso(C45) = Uiso(C2)
4. Others
 Fixed Sof: C45(0.5) C5(0.5) C6(0.5)
 Fixed X: C45(0.2406)
 Fixed Y: C45(0.7593)
5.a Aromatic/amide H refined with riding coordinates:
 C00E(H00E), C00G(H00G), C00J(H00J), C00L(H00L), C8(H8), C13(H13)
;
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              77596
_olex2_submission_special_instructions 'No special instructions were received'