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A microdiffraction set-up for nanoporous metal-organic-framework-type solids.

Christophe Volkringer¹, Dimitry Popov, Thierry Loiseau

¹Institut Lavoisier-UMR CNRS 8180, Institut Universitaire de France, Université de Versailles Saint Quentin en Yvelines, 45, avenue des Etats-Unis,78035 Versailles, France.

Nature Materials

|September 18, 2007

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Researchers developed a microdiffraction technique to determine the atomic structure of tiny porous metal-organic frameworks (MOFs). This breakthrough enabled the characterization of a new aluminum trimesate (MIL-110) MOF with large channels.

Area of Science:

Materials Science
Crystallography
Chemistry

Background:

Porous metal-organic frameworks (MOFs) are promising for catalysis, separation, and gas storage due to their large pore networks.
Understanding MOF atomic arrangements is crucial for predicting chemical and physical properties.
Small crystal sizes often limit traditional single-crystal diffraction analysis.

Purpose of the Study:

To present a microdiffraction setup capable of analyzing crystals down to the micrometer scale.
To determine the crystal structure of a new porous metal-organic framework, aluminum trimesate (MIL-110).

Main Methods:

Development of a microdiffraction setup using a microfocused X-ray beam (1 µm).
Collection of Bragg intensities from a single crystal of MIL-110 measuring a few micrometers.

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Structure determination aided by solid-state NMR (27Al, 13C, 1H) and molecular modeling.

Main Results:

Successful structure determination of MIL-110 from a sub-micrometer single crystal.
MIL-110 exhibits a honeycomb-like network with hexagonal 16 Å channels.
The structure comprises octahedrally coordinated aluminum octameric motifs linked by trimesate ligands.
The framework consists of light elements, resulting in very low density and weak scattering factors.

Conclusions:

The microdiffraction technique enables the structural analysis of extremely small MOF crystals.
The newly determined structure of MIL-110 provides insights into its potential applications in catalysis, separation, and gas storage.
Combined methods confirm the structural characteristics of this novel, low-density MOF.