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Controlled partial interpenetration in metal–organic frameworks

Nature Chemistry volume 8, pages 250–257 (2016)Cite this article

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Abstract

Interpenetration, the entwining of multiple lattices, is a common phenomenon in metal–organic frameworks (MOFs). Typically, in interpenetrated MOFs the sub-lattices are fully occupied. Here we report a family of MOFs in which one sub-lattice is fully occupied and the occupancy level of the other can be controlled during synthesis to produce frameworks with variable levels of partial interpenetration. We also report an ‘autocatenation’ process, a transformation of non-interpenetrated lattices into doubly interpenetrated frameworks via progressively higher degrees of interpenetration that involves no external reagents. Autocatenation maintains crystallinity and can be triggered either thermally or by shear forces. The ligand used to construct these MOFs is chiral, and both racemic and enantiopure partially interpenetrated frameworks can be accessed. X-ray diffraction, nonlinear optical microscopy and theoretical calculations offer insights into the structures and dynamic behaviour of these materials and the growth mechanisms of interpenetrated MOFs.

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Figure 1: MOFs with controlled degrees of interpenetration derived from the ligand rac-1.
Figure 2: MOFs with controlled degrees of interpenetration derived from ligand R-1 or S-1.
Figure 3: Ligand functionalization.
Figure 4: Autocatenation in MUF-9.
Figure 5: Characteristics of frameworks with various levels of interpenetration produced by different methods.

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Acknowledgements

We are grateful to the RSNZ Marsden Fund and the MacDiarmid Institute for financial support, to D. Lun for technical assistance, to S. Narayanaswamy and C. Lepper for assistance with the high-pressure experiments and to the staff of the Manawatu Microscopy and Imaging Centre at Massey University. F.X.C. acknowledges computing time on HPC platforms provided by a GENCI grant (x2015087069), and M.A.v.d.V., S.V.C. and T.V. acknowledge financial support from the Hercules Foundation and FWO-Flanders (research project G.0927.13).

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Authors and Affiliations

  1. MacDiarmid Institute for Advanced Materials and Nanotechnology, Institute of Fundamental Sciences, Massey University, Palmerston North, New Zealand

    Alan Ferguson, Lujia Liu, Stefanus J. Tapperwijn, David Perl & Shane G. Telfer

  2. PSL Research University, Chimie ParisTech – CNRS, Institut de Recherche de Chimie Paris, Paris, 75005, France

    François-Xavier Coudert

  3. Molecular Visualisation and Photonics, University of Leuven, Celestijnenlaan 200D, Heverlee, Belgium

    Stijn Van Cleuvenbergen & Thierry Verbiest

  4. Department of Chemical Engineering, Catalysis Engineering, Delft University of Technology, Julianalaan 136, Delft, 2628 BL, The Netherlands

    Monique A. van der Veen

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Contributions

A.F., L.L., D.P., S.J.T., S.V.C., M.A.v.d.V., T.V. and S.G.T. designed the experiments, carried out the experimental work and interpreted the experimental data. F.X.C. performed the theoretical calculations and analysed the results. S.G.T. coordinated the writing of the manuscript with input from all authors.

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Correspondence to Shane G. Telfer.

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Supplementary information

Supplementary information

Supplementary information (PDF 26227 kb)

Supplementary movie

Supplementary movie 1 (MP4 1623 kb)

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Crystallographic data for non-interpenetrated MUF-9. (CIF 405 kb)

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Crystallographic data for doubly interpenetrated MUF-9. (CIF 621 kb)

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Crystallographic data for non-interpenetrated MUF-10. (CIF 194 kb)

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Crystallographic data for doubly interpenetrated MUF-10. (CIF 422 kb)

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Crystallographic data for the gamma phase of MUF-9. (CIF 730 kb)

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Crystallographic data for the gamma phase of MUF-10. (CIF 1689 kb)

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rystallographic data for the partially interpenetrated MUF-9 formed after 16 h reaction in DBF. (CIF 159 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed after 40 h reaction in DBF. (CIF 160 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed after 65 h reaction in DBF. (CIF 162 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed after 134 h reaction in DBF. (CIF 129 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed after 8 h reaction in DMF. (CIF 168 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed after 2 h reaction in DEF. (CIF 139 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by desolvation of DMF-occluded alpha-MUF-9 over 100 mins MOF PIP-77-MUF-9. (CIF 173 kb)

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Crystallographic data for doubly interpenetrated MUF-9 formed by the further desolvation of DRY-1-MUF-9 over another 100 mins MOF beta-MUF-9. (CIF 167 kb)

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Crystallographic data for non-interpenetrated MUF-9 formed by reaction in 0% DMF in DBF. (CIF 166 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by reaction in 1% DMF in DBF, dataset a. (CIF 162 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by reaction in 1% DMF in DBF, dataset b. (CIF 161 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by reaction in 1% DMF in DBF, dataset c. (CIF 162 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by reaction in 2% DMF in DBF, dataset a. (CIF 161 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by reaction in 2% DMF in DBF, dataset b. (CIF 163 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by reaction in 2% DMF in DBF, dataset c. (CIF 162 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by reaction in 3% DMF in DBF, dataset a. (CIF 155 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by reaction in 3% DMF in DBF, dataset b. (CIF 162 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by reaction in 3% DMF in DBF, dataset c. (CIF 163 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by reaction in 4% DMF in DBF, dataset a. (CIF 162 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by reaction in 4% DMF in DBF, dataset b. (CIF 152 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by reaction in 4% DMF in DBF, dataset c. (CIF 163 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by reaction in 5% DMF in DBF, dataset a. (CIF 162 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by reaction in 5% DMF in DBF, dataset b. (CIF 162 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by reaction in 5% DMF in DBF, dataset c. (CIF 163 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by reaction in 6% DMF in DBF, dataset a. (CIF 161 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by reaction in 6% DMF in DBF, dataset b. (CIF 162 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by reaction in 6% DMF in DBF, dataset c. (CIF 161 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by reaction in 7% DMF in DBF, dataset a. (CIF 153 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by reaction in 7% DMF in DBF, dataset b. (CIF 153 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by reaction in 7% DMF in DBF, dataset c. (CIF 162 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by reaction in 8% DMF in DBF, dataset a. (CIF 161 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by reaction in 8% DMF in DBF, dataset b. (CIF 161 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by reaction in 8% DMF in DBF, dataset c. (CIF 162 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by reaction in 10% DMF in DBF, dataset a. (CIF 162 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by reaction in 10% DMF in DBF, dataset b. (CIF 163 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by reaction in 10% DMF in DBF, dataset c. (CIF 163 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by reaction in 12% DMF in DBF, dataset a. (CIF 162 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by reaction in 12% DMF in DBF, dataset b. (CIF 162 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by reaction in 12% DMF in DBF, dataset c. (CIF 151 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by reaction in 15% DMF in DBF over 6 hours, dataset a. (CIF 160 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by reaction in 15% DMF in DBF over 6 hours, dataset b. (CIF 162 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by reaction in 15% DMF in DBF over 7 hours. (CIF 170 kb)

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Crystallographic data for doubly interpenetrated MUF-9 formed by reaction in 15% DMF in DBF over 8 hours. (CIF 156 kb)

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Crystallographic data for non-interpenetrated MUF-9 before heating in DMF. (CIF 248 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by heating alpha-MUF-9 in DMF for 6 h. (CIF 196 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by heating alpha-MUF-9 in DMF for 10 h. (CIF 440 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by heating alpha-MUF-9 in DMF for 12 h. (CIF 258 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by heating alpha-MUF-9 in DMF for 18 h, dataset a. (CIF 246 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by heating alpha-MUF-9 in DMF for 18 h, dataset b. (CIF 253 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by heating alpha-MUF-9 in DMF for 21 h. (CIF 260 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by heating alpha-MUF-9 in DMF for 23 h. (CIF 278 kb)

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Crystallographic data for the Partially interpenetrated MUF-9 formed by heating alpha-MUF-9 in DMF for 24 h, dataset a. (CIF 259 kb)

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Crystallographic data for the Partially interpenetrated MUF-9 formed by heating alpha-MUF-9 in DMF for 24 h, dataset b. (CIF 244 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by heating alpha-MUF-9 in DMF for 27 h. (CIF 256 kb)

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Crystallographic data for doubly interpenetrated MUF-9 formed by heating alpha-MUF-9 in DMF for 30 h. (CIF 256 kb)

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Crystallographic data for the partially interpenetrated MUF-9 formed by heating alpha-MUF-9 in DMF for 36 h. (CIF 239 kb)

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Crystallographic data for doubly interpenetrated MUF-9 formed by heating alpha-MUF-9 in DMF for 45 h. (CIF 248 kb)

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Crystallographic data for doubly interpenetrated MUF-9 formed by heating alpha-MUF-9 in DMF for 60 h. (CIF 235 kb)

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Crystallographic data for non-interpenetrated MUF-9 after heating alpha-MUF-9 in DMF/DBF (20/80) for 40 h. (CIF 250 kb)

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Crystallographic data for doubly interpenetrated MUF-11 grown in DMF. (CIF 172 kb)

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Crystallographic data for doubly interpenetrated MUF-12 grown in DMF. (CIF 181 kb)

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Crystallographic data for non-interpenetrated MUF-14 grown in DEF. (CIF 170 kb)

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Calculated crystallographic parameters for MOF alpha-MUF-10. (CIF 3 kb)

Supplementary information

Calculated crystallographic parameters for MOF beta-MUF-10. (CIF 6 kb)

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Calculated crystallographic parameters for MOF gamma-MUF-10. (CIF 8 kb)

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Calculated crystallographic parameters for MOF IRMOF-9. (CIF 3 kb)

Supplementary information

Calculated crystallographic parameters for MOF IRMOF-10. (CIF 4 kb)

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Ferguson, A., Liu, L., Tapperwijn, S. et al. Controlled partial interpenetration in metal–organic frameworks. Nature Chem 8, 250–257 (2016). https://doi.org/10.1038/nchem.2430

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