Letter abstract
Nature Materials 6, 760 - 764 (2007)
Published online: 16 September 2007 | doi:10.1038/nmat1991
Subject Categories: Catalytic materials | Separation materials | Characterisation and analytical techniques
A microdiffraction set-up for nanoporous metal–organic-framework-type solids
Christophe Volkringer1, Dimitry Popov2, Thierry Loiseau1, Nathalie Guillou1, Gerard Ferey1, Mohamed Haouas1, Francis Taulelle1, Caroline Mellot-Draznieks1,3, Manfred Burghammer2 & Christian Riekel2
For the past decade, the emerging class of porous metal–organic frameworks1, 2, 3 has been becoming one of the most promising materials for the construction of extralarge pore networks in view of potential applications in catalysis, separation and gas storage. The knowledge of the atomic arrangements in these crystalline compounds is a key point for the understanding of the chemical and physical properties. Their crystal size limits the use of single-crystal diffraction analysis, and synchrotron radiation facilities4 may allow for the analysis of tiny crystals. We present here a microdiffraction set-up for the collection of Bragg intensities, which pushes down the limit to the micrometre scale by using a microfocused X-ray beam of 1 
m. We report the structure determination of a new porous metal–organic-framework-type aluminium trimesate (MIL-110) from a single crystal of a few micrometres length, showing very weak scattering factors owing to the composition of the framework (light elements) and very low density. Its structure is built up from a honeycomb-like network with hexagonal 16 Å channels, involving the connection of octahedrally coordinated aluminium octameric motifs with the trimesate ligands. Solid-state NMR (27Al,13C,1H) and molecular modelling are finally considered for the structural characterization.
- Institut Lavoisier—UMR CNRS 8180, Institut Universitaire de France, Université de Versailles Saint Quentin en Yvelines, 45, avenue des Etats-Unis,78035 Versailles, France
- ESRF, B.P. 220, 38043, Grenoble Cedex, France
- Royal Institution of Great Britain, 24 Albemarle Street, London, W1S 4BS, UK
Correspondence to: Thierry Loiseau1 e-mail: loiseau@chimie.uvsq.fr
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