The title compound (H₂teta)₂{[Ni(teta)][Fe(CN)₆]₂}•17H₂O was obtained by slow diffusion of an aqueous solution of K₃[Fe(CN)₆] and a DMF solu-tion of [Ni(teta)](ClO₄)₂ through a U-tube containing agar at room temperature. The compound crystallizes in the triclinic space group P1 with a＝0.9998(2) nm, b＝1.5514(3) nm, c＝1.6647(4) nm, α＝114.15(2)°, β＝100.91(2)°, γ＝93.42(2)°, V＝2.2863(10) nm³, z＝1, D_c＝1.196 g•cm^－3, F(000)＝890, μ＝5.84 cm^－1, GOF＝0.894, R₁＝0.0582, wR₂＝0.1446 [I＞2σ(I)]. Its structure con-sists of two cations of [H₂teta]^2＋, one trinuclear anion of {[Ni(teta)][Fe(CN)₆]₂}^4－ and seventeen water molecules, which are held together by the N—H…N hydrogen bonds to form a two-dimensional supramolecule. The variable temperature magnetic susceptibility, measured in the 1.8～300 K range, indicates the presence of a strong ferromagnetic interaction through the cyanide bridge in trinuclear system Fe (s＝1/2)-Ni (s＝1)-Fe (s＝1/2) with magnetic parameters J＝4.33 cm^－1, g＝2.6, θ＝60 K. The thermal stability of the complex was studied by TG-DTG.

Key words: [Ni(teta)]^2＋, cyano-bridged, supramolecule, crystal structure, magnetic property