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Anomalous small-angle X-ray scattering (ASAXS) experiments with synchrotron radiation were performed to study the three-dimensional nanostructures of metal/organic hybrids formed by crosslinking aluminium-organic-stabilized platinum nanoparticles with various bifunctional organic spacer molecules. The advantage of ASAXS is the possibility of separating the particle scattering from that of the organic components, thus providing unbiased information about particle size distributions and interparticle correlation. In order to obtain the structural information from the scattering data, a model function based on Vrij's analytical solution for a multicomponent system of hard spheres is proposed. The model is applied to three different samples and the results are compared with those obtained from the application of Fourier methods (characteristic function) and X-ray absorption measurements.

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