The polycrystalline and nanocrystalline states play an increasingly important role in exploiting the properties of materials, encompassing applications as diverse as pharmaceuticals, catalysts, solar cells and energy storage. A knowledge of the three-dimensional atomic and molecular structure of materials is essential for understanding and controlling their properties, yet traditional single-crystal X-ray diffraction methods lose their power when only polycrystalline and nanocrystalline samples are available. It is here that powder diffraction and single-crystal electron diffraction techniques take over, substantially extending the range of applicability of the crystallographic principles of structure determination. This volume, a collection of teaching contributions presented at the Crystallographic Course in Erice in 2011, clearly describes the fundamentals and the state-of-the-art of powder diffraction and electron diffraction methods in materials characterisation, encompassing a diverse range of disciplines and materials stretching from archeometry to zeolites. As such, it is a comprehensive and valuable resource for those wishing to gain an understanding of the broad applicability of these two rapidly developing fields.