A dynamic pcu MOF(Zn) containing a ditopic T-shaped [2]rotaxane linker
Amarne, Hazem; Stirk, Alexander J.; O'Keefe, Christopher A.; Schurko, Robert W.; Loeb, Stephen J.; CrystEngComm 28 (2026) 631–634; doi:10.1039/D5CE01108F

data_7251545
_publ_section_title
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 A dynamic pcu MOF(Zn) containing a ditopic T-shaped [2]rotaxane linker
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_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              631
_journal_page_last               634
_journal_paper_doi               10.1039/D5CE01108F
_journal_volume                  28
_journal_year                    2026
_chemical_formula_moiety         'C29 H20.67 N2 O6.333 Zn, 0.167(O), C18 H36 O6'
_chemical_formula_sum            'C282 H342 N12 O75 Zn6'
_chemical_formula_weight         5491.88
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2025-10-31
_audit_creation_method
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Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
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_audit_update_record
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2025-11-05 deposited with the CCDC.	2025-12-23 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   25.8311(5)
_cell_length_b                   25.8311(5)
_cell_length_c                   44.9688(14)
_cell_measurement_reflns_used    9950
_cell_measurement_temperature    170.0
_cell_measurement_theta_max      51.945
_cell_measurement_theta_min      2.206
_cell_volume                     25985.3(11)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0631
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            91605
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        51.945
_diffrn_reflns_theta_max         51.945
_diffrn_reflns_theta_min         2.206
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.018
_exptl_absorpt_correction_T_max  0.7502
_exptl_absorpt_correction_T_min  0.5856
_exptl_absorpt_process_details
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SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1449 before and 0.0914 after correction.
The Ratio of minimum to maximum transmission is 0.7806.
The \l/2 correction factor is Not present.
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_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.053
_exptl_crystal_description       prism
_exptl_crystal_F_000             8694
_exptl_crystal_recrystallization_method 'Solvothermal synthesis from DMF'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.128
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.774
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         6419
_refine_ls_number_restraints     252
_refine_ls_restrained_S_all      1.819
_refine_ls_R_factor_all          0.1257
_refine_ls_R_factor_gt           0.1224
_refine_ls_shift/su_max          0.000
_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          0.3411
_refine_ls_wR_factor_ref         0.3494
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6124
_reflns_number_total             6419
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce01108f2.cif
_cod_data_source_block           test3
_cod_original_cell_volume        25985.3(13)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7251545
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
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1. Twinned data refinement
 Scales: 0.736(3)
 0.264(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H3 of O3, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H1B of O1B
3. Restrained distances
 C46-C47 = C30-C31 = C32-C33 = C34-C35 = C36-C37
 1.48 with sigma of 0.02
 C45-C44 = C45-C46 = O7-C47 = O7-C30 = O8-C31 = O8-C32
 1.42 with sigma of 0.02
 O9-C33 = O9-C34 = O10-C35 = O10-C36 = O11-C37 = O11-C38
 1.42 with sigma of 0.02
 C38-C39 = C39-O12 = O12-C40 = C40-C41 = C41-C42 = C42-C43 = C43-C44
 1.48 with sigma of 0.02
 C45-C47 = C45-C43 = O7-C46 = O7-C31 = O8-C30 = O8-C33 = O9-C32 = O9-C35
 2.4 with sigma of 0.04
 O10-C34 = O10-C37 = O11-C36 = O11-C39
 2.4 with sigma of 0.04
 C44-C46 = C47-C30 = C31-C32 = C33-C34 = C35-C36 = C37-C38
 2.44 with sigma of 0.04
 C38-O12 = C39-C40 = O12-C41 = C40-C42 = C41-C43 = C42-C44
 2.44 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim O5 \\sim C28 \\sim
O6 \\sim C29: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
O7 \\sim C30 \\sim C31 \\sim O8 \\sim C32 \\sim C33 \\sim O9 \\sim C34 \\sim
C35 \\sim O10 \\sim C36 \\sim C37 \\sim O11 \\sim C38 \\sim C39 \\sim O12:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
5. Others
 Fixed Sof: H3(0.67)
 Fixed X: H3(0.08558)
 Fixed Y: H3(0.039409)
 Fixed Z: H3(0.47394)
6.a Ternary CH refined with riding coordinates:
 O1B(H1B)
6.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,
 H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B),
 C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B),
  C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B)
6.c Me refined with riding coordinates:
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C)
6.d Aromatic/amide H refined with riding coordinates:
 N2(H2), C3(H3A), C4(H4), C6(H6), C7(H7), C12(H12), C13(H13), C15(H15),
 C16(H16), C18(H18), C19(H19), C23(H23), C25(H25), C27(H27)
6.e Fitted hexagon refined as free rotating group:
 C22(C23,C24,C25,C26,C27)
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_shelx_res_checksum              97429
_olex2_submission_special_instructions 'No special instructions were received'