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The intermetallic ytterbium compound Yb 2 Pd 2 Cd shows a structural phase transition at ∼150 K. The structures of the room-temperature (Mo 2 B 2 Fe type,  P 4/ mbm ,  a  = 757.07(7),  c  = 371.99(4) pm,  wR 2 = 0.0620, 272  F   2  values, 12 variables) and low-temperature (new type,  P 4/ mbm ,  a  = 747.26(4),  c  = 741.46(4) pm,  wR 2 = 0.0384, 511  F   2  values, 19 variables) modifications were refined from single crystal X-ray diffractometer data. The superstructure formation corresponds to an  isomorphic  transition of index 2. The driving force for the structural phase transition is an ytterbium charge ordering (the superstructure exhibits two crystallographically independent ytterbium sites) with a much higher degree of divalent ytterbium in the low-temperature modification. The striking structural feature concerns the ytterbium–palladium coordination with different Yb–Pd distances: longer ones for predominantly divalent Yb1 (2 × 284.7 and 4 × 296.1 pm, ∅ = 292.3 pm) and shorter ones for trivalent Yb2 (2 × 277.5 and 4 × 288.4 pm, ∅ = 284.8 pm).

Ytterbium valence ordering in the low-temperature superstructure of Yb 2 Pd 2 Cd