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Zirconolites based on the replacement of Ti 4+  with equimolar amounts of Nb 5+ and Fe 3+ , CaZrTi 2-2x  NbxFexO 7 , have been jointly refined using high-resolution neutron powder diffraction and resonant X-ray powder diffraction data, with extra information provided from  57 Fe Mössbauer spectroscopy, to determine cation disorder. The results indicate that the CaZrTi 2-2x NbxFexO 7  series adopts the zirconolite-2M polytype across the range, with the replacement of Ti 4+  by Fe 3+  and Nb 5+  located within the hexagonal tungsten bronze (HTB) layers. Mössbauer spectroscopy shows that Fe 3+  preferentially fills the Ti split (C2) site, with secondary filling of the C1 site and no observable occupancy of the C3 site. This has been confirmed by neutron and resonant X-ray diffraction. Niobium has been found to occupy both the C1 and C3 sites with no evidence for occupancy of the C2 site.

Combined neutron and X-ray diffraction determination of disorder in doped zirconolite-2M