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The propensity of the new, phenylphosphonate‐stabilized polyoxotungstate [(C 6 H 5 P V O) 2 P 4 W 24 O 92 ] 16−  to act as a precursor for new 3d metal‐functionalized polyanions has been investigated. Reactions with Mn II  and Cu II  induce the formation of the previously unknown polyoxotungstate archetype {P 4 W 27 }, isolated as salts of the polyanions [Na⊂{Mn II (H 2 O)}{WO(H 2 O)}P 4 W 26 O 98 ] 13−  ( 1 ) and [K⊂{Cu II (H 2 O)}{W(OH)(H 2 O)}P 4 W 27 O 99 ] 14−  ( 2 ), which were characterized in the solid state (single‐crystal X‐ray diffraction, elemental and TG analyses, IR spectroscopy, SQUID magnetometry) and in aqueous solution (UV/Vis spectroscopy, cyclic voltammetry).

Polyoxotungstate Archetype {P 4 W 27 } and its 3d Derivatives