APPLICATIONS OF SYNCHROTRON/IMAGING PLATE SYSTEM TO ELUCIDATE THE STRUCTURE AND SYNTHETIC PATHWAYS TO OPEN FRAMEWORK ANTIMONY SULFIDES. Kemin Tan, John B. Parise and Younghee Ko, Department of Earth and Space Sciences State University of New York at Stony Brook Stony Brook, New York 11794, Alex Darovsky SUNY X3A Beamline, National Synchrotron Lingh Source Brookhaven National Laboratory, Upton, New York 11973, Poul Norby and Jonathan C. Hanson, X7B Beamline, National Synchrotron Lingh Source Brookhaven National Laboratory, Upton, New York 11973.

Open framework antimony sufides are potential useful optical and catalytic materials. Recrystallization of antimony sulfide in the presence of organic templates under hydrothermal condition has generated a number of novel open framework phases. The single crystal of these materials are usually small and unsuitable for conventional x-ray diffractometry. Further, multiple-phases can crystallize from one batch of a hydrotheraml experiment and this can makes it difficult to obtain one pure phase for further studies and applications. In order to determine the systematics of structure for these novel materials, single crystal diffraction data have been collected using the imaging plate (IP) system at the NSLS beamline X-3A. From these data, several structures have been solved and their structural relationships have been analysized. A Sb4S7(2-) single chain has been found to be a major building block in these materials. It is also important to follow the possible crystallization pathways of these phases, and their dependence on such syntheic parameters as pH, sulfur content, temperature and aging, the transformations from starting materials. We have done this under real-time hydrothermal conditions using powder diffraction and an IP at beamline X7B. From these results, information on the kinetics of formation, useful to optimize future syntheses, has been obtained.