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A family of solution‐stable polyanions [Na⊂{Ln III (H 2 O)}{W VI O(H 2 O)}P V  4 W VI  26 O 98 ] 12−  (Ln=Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu and Y) represent the first examples of polyoxometalates comprising a single lanthanide(III) or yttrium(III) ion in a rare trigonal prismatic O 6  environment. Their synthesis exploits the reactivity of the organophosphonate‐functionalized precursor [P 4 W 24 O 92 (C 6 H 5 P V O) 2 ] 16−  with heterometal ions and yields hydrated potassium or mixed lithium/potassium salts of composition K  x  Ln  y  H 12– x – y  [Na⊂{Ln(H 2 O)}{WO(H 2 O)}P 4 W 26 O 98 ]⋅ n H 2 O⋅ m LiCl ( x =8.5–11;  y =0–2;  n =24–34;  m =0–1.5). The Dy, Ho, Er and Yb derivatives are characterized by slow magnetization relaxation.

Trigonal Prismatic Coordination of Discrete Rare Earth Ions, Enforced by the Polyoxotungstate [P 4 W 27 O 99 (H 2 O)] 16–