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High-resolution synchrotron powder X-ray data have been used to solve the structures of I2O4 and Al2Y4O9 by profile decomposition into individual structure amplitudes, followed by application of standard Patterson and direct methods. The data were obtained from a series of spectra recorded with a small linear position-sensitive detector, and some of the errors arising from this approach are discussed. The final structures were obtained by Rietveld refinement, and Rp values for the profile intensities are 10.9 and 9.2% for Al2Y4O9 and I2O4 respectively. For Al2Y4O9 good agreement was found with the known isomorphous compound Al2Eu4O9, while I2O4 data were compared with high-resolution neutron powder data. This analysis, together with other recently reported studies, shows that structure determination from powder data will be feasible even for rather complicated structures.

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