Discovery and Structure Determination of an Unusual Sulfide Telluride through an Effective Combination of TEM and Synchrotron Microdiffraction.

The structure elucidation of the novel sulfide telluride Pb8Sb8S15Te5 demonstrates a new versatile procedure that exploits the synergism of electron microscopy and synchrotron diffraction methods for accurate structure analyses of side-phases in heterogeneous microcrystalline samples. Suitable crystallites of unknown compounds can be identified by transmission electron microscopy and relocated and centered in a microfocused synchrotron beam by means of X-ray fluorescence scans. The refined structure model is then confirmed by simulating HRTEM images of the same crystallite. Pb8Sb8S15Te5 consists of chains of heterocubane-like units. Cation coordination polyhedra form unusually entwined chains of edge- and face-sharing bicapped trigonal prisms. The structure data are precise enough for bond-valence calculations, which confirm the disordered atom distribution. On this basis, optimization of physical properties becomes feasible.