A cyano-bridged coordination polymer, j [ Fe (salen)]_2 [Ni ( CN)_4] }_n ( salen = N, N'-ethylenebis-(salicylideneimi-nato)-dianion), prepared by slow diffusion of an aqueous solution of K2[Ni(CN)4]· H_2O and a MeOH solution of [Fe(salen)-NO3] in an H tube, has been characterized by X-ray structure analysis, IR spectra and magnetic measurements. The complex crystallizes in the tetragonal space group PA/ncc with a = b = 1.4216(2) nm, c= 1.7471(5) nm, V = 3.5308(12) nm~3, Z = 4. The product assumes a two-dimensional network structure consisting of pillow-like octanuclear [-Ni-CN-Fe(salen)-NC-_]4 units with dimensions: Ni-C = 0.1876(3) nm, Fe-N = 0.2170(3) nm, Fe-N- C= 164.9(3)°, Ni-C-N= 178.9(4)°. The two metal atoms Ni( II )and Fe( HI) have square and slightly distorted octahedral arrangements, respectively. The variable temperature magnetic susceptibility, measured in the 5 ～ 300 K range, indicates the presence of a weak intralayer antiferromagnetic interaction and gives an Fe( III) …Fe (III) exchange integral of - 0.041 cm"

Key words: NICKEL COMPLEX, IRON COMPLEX, CRYSTAL STRUCTURE, MAGNETISM, CYANO GROUP, SCHIFF BASE