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A heterometallic assembly, [Mn(salen)] 2 [Ni(CN) 4 ]·1/2H 2 O (where salen=N, N′-ethylene-bis(salicylideneiminato)-dianion), has been prepared from the reaction of [Mn(salen)H 2 O]ClO 4 ·H 2 O with K 2 [Ni(CN) 4 ]·H 2 O in methanol/water. The compound crystallizes in the tetragonal space group P 4/ncc with the cell dimensions of a =14.604(2) Å, c =16.949(3) Å, and Z=4. The compound assumes a two-dimensional distorted square network structure, formed from ${\rm Ni}{{\hskip -1pt -\!\!\!- \hskip-.5pt}}{\rm CN}{{\hskip -1pt -\!\!\!- \hskip-.5pt}}{\rm Mn(salen)}{{\hskip -1pt -\!\!\!- \hskip-.5pt}}{\rm NC}{{\hskip -1pt -\!\!\!- \hskip-.5pt}}{\rm Ni}$ [ABSTRACT FROM AUTHOR]