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KSbTeO6 defect pyrochlore has been prepared from K2C2O4, Sb2O3, and 15% excess TeO2 by solid-state reaction at 850 °C. Direct methods implemented in the software EXPO2013 allowed establishing the basic structural framework. This was followed by a combined Rietveld refinement from X-ray powder diffraction (XRD) and neutron powder diffraction (NPD) data, which unveiled additional structural features. KSbTeO6 is cubic, a = 10.1226(7) Å, space group <inline-formula> <math display="inline"> <semantics> <mrow> <mi>F</mi> <mi>d</mi> <mover accent="true"> <mn>3</mn> <mo stretchy="true">¯</mo> </mover> <mi>m</mi> </mrow> </semantics> </math> </inline-formula>, Z = 8 and it is made of a mainly covalent framework of corner-sharing (Sb,Te)O6 octahedra, with weakly bonded K+ ions located within large cages. The large K-O distances, 3.05(3)–3.07(3) Å, and quite large anisotropic atomic displacement parameters account for the easiness of K+ exchange for other cations of technological importance.We thank the financial support of the Spanish MINECO tot he proyect MAT2013-41099-R\udWe are grateful to the Institut Laue-Langevin (ILL) in Grenoble for making all the facilities availablWe acknowledge support by the CSIC Open Access Publication Initiative through its Unit of Information Resources for Research (URICI)

Potassium Disorder in the Defect Pyrochlore KSbTeO6: A Neutron Diffraction Study