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Metal‐Directed Self‐Assembly of a Polyoxometalate‐Based Molecular Triangle: Using Powerful Analytical Tools to Probe the Chemical Structure of Complex Supramolecular Assemblies |
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| Authors: | Dr. Guillaume Izzet Dr. Andrew Macdonell Dr. Corentin Rinfray Madeleine Piot Séverine Renaudineau Dr. Etienne Derat Dr. Benjamin Abécassis Prof. Dr. Carlos Afonso Prof. Dr. Anna Proust |
| Affiliation: | 1. Institut Parisien de Chimie Moléculaire UMR CNRS 8232, Sorbonne Universités, UPMC‐Paris06, 4 Place Jussieu, 75005 Paris (France);2. WestCHEM, School of Chemistry, University of Glasgow, University Avenue, Glasgow, G12 8QQ (UK);3. Laboratoire de Physique des Solides, Univ. Paris‐Sud, CNRS, UMR 8502, 91405 Orsay Cedex (France);4. Normandie Université, COBRA, UMR6014 and FR3038;5. Université de Rouen, INSA de Rouen;6. CNRS, IRCOF, 1 rue Tesnière, 76821 Mont‐Saint‐Aignan Cedex (France) |
| Abstract: | A polyoxometalate‐based molecular triangle has been synthesized through the metal‐driven self‐assembly of covalent organic/inorganic hybrid oxo‐clusters with remote pyridyl binding sites. The new metallomacrocycle was unambiguously characterized by using a combination of 1H NMR spectroscopy, 2D diffusion NMR spectroscopy (DOSY), electrospray ionization travelling wave ion mobility mass spectrometry (ESI‐TWIM‐MS), small‐angle X‐ray scattering (SAXS) and molecular modelling. The collision cross‐sections obtained from TWIM‐MS and the hydrodynamic radii derived from DOSY are in good agreement with the geometry‐optimized structures obtained by using theoretical calculations. Furthermore, SAXS was successfully employed and proved to be a powerful technique for characterizing such large supramolecular assemblies. |
| Keywords: | mass spectrometry NMR spectroscopy polyoxometalates supramolecular chemistry X‐ray diffraction |