title: Metal-Directed Self-Assembly of a Polyoxometalate-Based Molecular Triangle: Using Powerful Analytical Tools to Probe the Chemical Structure of Complex Supramolecular Assemblies.
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 (1)H 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.
authors.affiliation: Institut Parisien de Chimie Moléculaire UMR CNRS 8232, Sorbonne Universités, UPMC-Paris06, 4 Place Jussieu, 75005 Paris (France). guillaume.izzet@upmc.fr.
authors.forename: Guillaume
authors.initials: G
authors.lastname: Izzet
authors.affiliation: WestCHEM, School of Chemistry, University of Glasgow, University Avenue, Glasgow, G12 8QQ (UK).
authors.forename: Andrew
authors.initials: A
authors.lastname: Macdonell
authors.affiliation: Institut Parisien de Chimie Moléculaire UMR CNRS 8232, Sorbonne Universités, UPMC-Paris06, 4 Place Jussieu, 75005 Paris (France).
authors.forename: Corentin
authors.initials: C
authors.lastname: Rinfray
authors.affiliation: Institut Parisien de Chimie Moléculaire UMR CNRS 8232, Sorbonne Universités, UPMC-Paris06, 4 Place Jussieu, 75005 Paris (France).
authors.forename: Madeleine
authors.initials: M
authors.lastname: Piot
authors.affiliation: Institut Parisien de Chimie Moléculaire UMR CNRS 8232, Sorbonne Universités, UPMC-Paris06, 4 Place Jussieu, 75005 Paris (France).
authors.forename: Séverine
authors.initials: S
authors.lastname: Renaudineau
authors.affiliation: Institut Parisien de Chimie Moléculaire UMR CNRS 8232, Sorbonne Universités, UPMC-Paris06, 4 Place Jussieu, 75005 Paris (France).
authors.forename: Etienne
authors.initials: E
authors.lastname: Derat
authors.affiliation: Laboratoire de Physique des Solides, Univ. Paris-Sud, CNRS, UMR 8502, 91405 Orsay Cedex (France).
authors.forename: Benjamin
authors.initials: B
authors.lastname: Abécassis
authors.affiliation: Normandie Université, COBRA, UMR6014 and FR3038; Université de Rouen, INSA de Rouen; CNRS, IRCOF, 1 rue Tesnière, 76821 Mont-Saint-Aignan Cedex (France).
authors.forename: Carlos
authors.initials: C
authors.lastname: Afonso
authors.affiliation: Institut Parisien de Chimie Moléculaire UMR CNRS 8232, Sorbonne Universités, UPMC-Paris06, 4 Place Jussieu, 75005 Paris (France).
authors.forename: Anna
authors.initials: A
authors.lastname: Proust
keywords: NMR spectroscopy; X-ray diffraction; mass spectrometry; polyoxometalates; supramolecular chemistry