An Electron Diffraction and XRPD Study of Superlattice Ordering in the Elpasolite-Related Oxyfluoride K3MoO3F3

A detailed electron diffraction and XRPD study has been made of the room-temperature α polymorph of K3MoO3F3. It is shown that the true symmetry of this polymorph is neither tetragonal, trigonal, nor triclinic as previously reported but rather monoclinic I1a1, a=2ap−cp, b=4bp, c=ap+2cp when expressed in terms of the underlying elpasolite (ordered perovskite) parent structure type. A highly structured, three-dimensional, continuous diffuse intensity distribution (presumably arising from local O/F ordering and associated structural relaxation) is shown to coexist with the sharp satellite reflections characteristic of the monoclinic supercell.