Interplay between Solid‐State NMR and Single‐Crystal X‐Ray Diffraction

The complementary relationship between solid‐state nuclear magnetic resonance (NMR) spectroscopy and diffraction techniques, specifically single‐crystal X‐ray diffraction (XRD), is explained and illustrated. It is demonstrated how solid‐state NMR and single‐crystal XRD can be combined advantageously, allowing structural chemists to investigate the detailed structures of materials in a way that could not be achieved by using a single technique alone. By using few examples involving zeolites and organic host‐guest complexes, the importance of a combined approach with solid‐state NMR and single‐crystal XRD for detailed structural characterization is illustrated.