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• W3115694015 abstract "Controlling the internal molecular dynamics in reticular materials is a major challenge for the development of nanotechnological applications. In this issue of Chem, Schurko, Loeb, and co-workers show how the ring motion of the [2]rotaxane-based linker and that of the surrounding triphenylene-based struts influence each other within a series of robust zirconium(IV) organic frameworks. Controlling the internal molecular dynamics in reticular materials is a major challenge for the development of nanotechnological applications. In this issue of Chem, Schurko, Loeb, and co-workers show how the ring motion of the [2]rotaxane-based linker and that of the surrounding triphenylene-based struts influence each other within a series of robust zirconium(IV) organic frameworks. Rotaxanes, entangled compounds composed of a ring threaded by a stoppered axle, are probably the most reputed mechanically interlocked molecular architectures.1Sluysmans D. Stoddart J.F. The burgeoning of mechanically interlocked molecules in chemistry.Trends Chem. 2019; 1: 185-197Abstract Full Text Full Text PDF Scopus (47) Google Scholar The mechanical bond of their structures has been and still is a source of inspiration for the discovery of a number of useful molecular systems, including sensors, catalysts, ion transporters, synthesizers, pumps, and responsive materials, among others.1Sluysmans D. Stoddart J.F. The burgeoning of mechanically interlocked molecules in chemistry.Trends Chem. 2019; 1: 185-197Abstract Full Text Full Text PDF Scopus (47) Google Scholar,2Erbas-Cakmak S. Leigh D.A. McTernan C.T. Nussbaumer A.L. Artificial molecular machines.Chem. Rev. 2015; 115: 10081-10206Crossref PubMed Scopus (1041) Google Scholar Controlling the internal rotational and translational motions in these multicomponent compounds as a response to external stimuli gave birth to a novel generation of functional switching systems. Among them, shuttles, in which the ring of the rotaxane travels between two docking places embedded in the thread, occupy a privileged position because they are considered one of the most promising scaffolds for the building of artificial molecular machines.2Erbas-Cakmak S. Leigh D.A. McTernan C.T. Nussbaumer A.L. Artificial molecular machines.Chem. Rev. 2015; 115: 10081-10206Crossref PubMed Scopus (1041) Google Scholar The fabrication of mechanical devices operated by molecular machines is among the most important objectives in nanoscience. For this purpose, scientists must discover how to incorporate switchable molecules into hierarchical assemblies enabled for exporting the effects of their motion to their surroundings.3Coskun A. Banaszak M. Astumian R.D. Stoddart J.F. Grzybowski B.A. Great expectations: can artificial molecular machines deliver on their promise?.Chem. Soc. Rev. 2012; 41: 19-30Crossref PubMed Scopus (650) Google Scholar The organization of molecular machines into the backbone of solid three-dimensional ordered scaffolds has been considered an important strategy for rendering a suitable empty volume that permits the molecular motion of their building blocks.4Wilson B.H. Loeb S.J. Integrating the mechanical bond into metal-organic frameworks.Chem. 2020; 6: 1604-1612Abstract Full Text Full Text PDF Scopus (20) Google Scholar Over the last decades, metal-organic frameworks (MOFs), crystal lattices with metallic nodes linked by organic ligands, have been postulated as porous materials with promising applications in various fields such as catalysis, biomedicine, and even water harvesting.5Yaghi O.M. Kalmutzki M.J. Diercks C.S. Introduction to Reticular Chemistry: Metal-Organic Frameworks and Covalent Organic Frameworks. Wiley-VCH, 2019Crossref Scopus (192) Google Scholar Wilson and Loeb devised that the incorporation of mechanically interlocked molecules as organic linkers in these well-ordered materials would allow the mechanical motion inside these materials in the solid state.4Wilson B.H. Loeb S.J. Integrating the mechanical bond into metal-organic frameworks.Chem. 2020; 6: 1604-1612Abstract Full Text Full Text PDF Scopus (20) Google Scholar A couple of key milestones showed the potential of metal organic rotaxane frameworks in the development of molecular machinery. In 2012, the first example of rotational dynamics of a rotaxane-based MOF was reported.6Vukotic V.N. Harris K.J. Zhu K. Schurko R.W. Loeb S.J. Metal-organic frameworks with dynamic interlocked components.Nat. Chem. 2012; 4: 456-460Crossref PubMed Scopus (194) Google Scholar This example consists of a crown ether ring and a benzylaniline axle linked to copper ions. The thermal desolvation of this material creates a regular network of cavities in the framework to allow the fast rotation of the macrocycle. In 2015, the back-and-forth motion of the same ring along an axis was demonstrated inside a MOF.7Zhu K. O’Keefe C.A. Vukotic V.N. Schurko R.W. Loeb S.J. A molecular shuttle that operates inside a metal-organic framework.Nat. Chem. 2015; 7: 514-519Crossref PubMed Scopus (189) Google Scholar Although the number of reported cases of dynamics inside mechanized frameworks is still very limited,4Wilson B.H. Loeb S.J. Integrating the mechanical bond into metal-organic frameworks.Chem. 2020; 6: 1604-1612Abstract Full Text Full Text PDF Scopus (20) Google Scholar,8Saura-Sanmartin A. Martinez-Cuezva A. Bautista D. Marzari M.R.B. Martins M.A.P. Alajarin M. Berna J. Copper-linked rotaxanes for the building of photoresponsive metal organic frameworks with controlled cargo delivery.J. Am. Chem. Soc. 2020; 142: 13442-13449Crossref PubMed Scopus (12) Google Scholar those examples paved the way to transferring the internal motion of the rotaxanes in solution to more ordered assemblies, a crucial step toward the next generation of solid-state porous devices.3Coskun A. Banaszak M. Astumian R.D. Stoddart J.F. Grzybowski B.A. Great expectations: can artificial molecular machines deliver on their promise?.Chem. Soc. Rev. 2012; 41: 19-30Crossref PubMed Scopus (650) Google Scholar In the development of collectively working molecular assemblies,9Krause S. Feringa B.L. Towards artificial molecular factories from framework embedded molecular machines.Natl. Rev. 2020; 4: 550-562Google Scholar the incorporation of rotaxanes (and other tools in the molecular machinery toolbox) into framework materials is an ideal scenario. The coupling and disengaging of the motion of individual molecular machines at the solid state could be engineered to program coordinated operations with different missions, including multistep synthesis, the development of unusual catalytic environments, and the finding of enhanced energy transductors. The work presented by Loeb and colleagues in this issue of Chem10Wilson B.H. Vojvodin C.S. Gholami G. Abdulla L.M. O’Keefe C.A. Schurko R.W. Loeb S.J. Precise spatial arrangement and interaction between two different mobile components in a metal-organic framework.Chem. 2021; 7: 202-211Abstract Full Text Full Text PDF Scopus (8) Google Scholar discloses the integration of an interlocked H-shaped tetracarboxylate with a bis(benzimidazole) thread and a crown ether ring (Figure 1A) into the tetrahedral cavity of a set of three Zr-based MOFs. The authors designed the molecular neighborhood of this rotaxane-based strut by including a variety of terphenylene-type dicarboxylate linkers in the central para-disubstituted ring: perdeuterated phenyl, tetramethylphenyl, and tetrazine units (Figure 1). These central units with different steric demands could interfere to varying degrees with the translational ring motion of the interlocked strut and, at same time, with their rotational motion. To conduct this study, the authors judiciously selected chemically and thermally stable Zr-based MOFs as their starting reticular materials; these included terphenylene-type linkers connecting metal nodes, thus providing a well-ordered network of tetrahedral and octahedral cavities. They used either the direct solvothermal method or the solvent-assisted linker exchange protocol to integrate the interlocked linker into the tetrahedral cavities.10Wilson B.H. Vojvodin C.S. Gholami G. Abdulla L.M. O’Keefe C.A. Schurko R.W. Loeb S.J. Precise spatial arrangement and interaction between two different mobile components in a metal-organic framework.Chem. 2021; 7: 202-211Abstract Full Text Full Text PDF Scopus (8) Google Scholar To explore the dynamics of the non-interlocked and interlocked linkers, the authors performed varying-temperature solid-state nuclear magnetic resonance (VT SS-NMR). For this purpose, the interlocked linkers were previously labeled with 13C, and the MOF with non-interlocked struts bearing deuterium isotopes was particularly scrutinized. These experiments revealed that orthogonal positioning of the sterically hindered tetramethyl linker at the edges of the tetrahedral void in which the crossbar [2]rotaxane was situated prevented any possibility of motion of the ring (Figure 1B). In stark contrast, a flattering disposition of the tetrazine-based linker let the ring move to the center region of the thread to get rid of the steric pressure of its immediate surrounding (Figure 1C). Moreover, the authors report a captivating state for the third Zr mechanized material with deuterated triphenylene struts (Figure 1D) whereby a molecular cross-talk between the motions of both mobile linkers was established. In this particular dynamic material, the rotational motion of the deuterated central phenylene unit proved to be coupled with that of the translational positioning of the ring of the interlocked linker via transient through-space interactions. Last but not the least, a delicate analysis of the VT SS-NMR data from the non-mechanized materials and their mechanized surrogates, comprising a number of theoretical simulations for the rotating models, demonstrates how the dynamics of the non- and interlocked linkers interplay with each other. This work nicely illustrates an elegant roadmap for designing dynamic mechanized materials in which two different motions can be coupled on a spatial and temporal domain. This report must be considered one of the first characterized examples en route toward cooperative working molecular assemblies. The authors gratefully acknowledge financial support from the Ministerio de Economia y Competitividad ( CTQ2017-87231-P ) with joint financing by the European Regional Development Fund and Fundacion Seneca-Comunidad Autonoma de la Region de Murcia (project 20811/PI/18). A.M.-C. thanks the Ministerio de Ciencia e Innovacion for a Ramon y Cajal contract ( RYC-2017-22700 ). A.S.-S. also thanks the Fundacion Seneca-CARM for his PhD fellowship. Precise Spatial Arrangement and Interaction between Two Different Mobile Components in a Metal-Organic FrameworkWilson et al.ChemDecember 1, 2020In BriefControlling the interactions of multiple dynamic components is key to unlocking the potential of molecular machines. Herein, an H-shaped [2]rotaxane molecular shuttle is imbedded in a series of zirconium-based MOFs in conjunction with a variety of other co-ligands. The bulk of the co-ligand dictates the translational position of the rotaxane macrocycle, determined via 13C solid-state NMR (SSNMR). 2H SSNMR revealed that for a co-ligand capable of exhibiting motion, the dynamics are influenced by the translational position of the [2]rotaxane macrocycle. Full-Text PDF" @default.
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• W3115694015 title "Coupling the Individual Motions of the Machine-like Components of Zirconium(IV) Organic Frameworks" @default.
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