Neutron powder diffraction studies on PdD0.65 demonstrate that the 50
K anomaly is due to an order-disorder transition of deuterium within o
ctahedral interstitial sites. The slow transition to the ordered phase
involves diffusion of deuterium from the nearest-neighbour deuterium
positions to the second-nearest-neighbour positions. The ordered cryst
al structure remains cubic, and is accurately described in space group
Pm (3) over bar n by doubling the cell constant relative to the disor
dered structure (space group Fm3m).