Two one-dimensional chain-like cyanide-bridged compounds, [Fe(Phen)2(CN)2Ni- (Cyclam)](CIO4)2·DMF·2H2O 1 (Cyclam = 1,4,8,11-tetraaza-cyclotetradecane, Phen = 1,10-phenan- throline, and DMF = N,N-dimethylformamide) and [Fe(Phen)2(CN)2Zn(Cyclam)](PF6)2·CH3CN 2, were prepared by the reaction of [Fe(Phen)2(CN)2]·2H2O with M(Cyclam)2+ (M = Ni, Zn). In complexes 1 and 2, the metal atoms are connected alternatively with CN groups. X-ray structure and IR analyses for 1 and 2 were performed. Structure analysis revealed that both complexes are centrosymmetric and the geometry around each metal atom is an octahedron. The two complexes crystallize in triclinic with space group of Pi. For 1, a = 10.439(4), b = 14.976(7), c = 15.914(8) A, α= 83.168(15), β = 74.338(15), γ= 78.023(15)°, V= 2338.3(18) A3, Z = 2, Mr = 1035.37, Dc = 1.471 g/cm3, F(000) = 1076, # = 0.895 mm-1, the final R = 0.0616 and wR = 0.1414 for 5849 observed reflections (Ⅰ > 2σ(Ⅰ)). For 2, a = 9.656(6), b = 15.404(9), c = 15.822(10)A, α= 78.68(2), β= 78.917(19),γ = 77.15(2)°, V = 2223(2) A3, Z = 2, Mr = 1064.87, Dc = 1.587 g/cm3, F(000) = 1078, μ= 1.032 mm-1, the final R = 0.0672 and wR = 0.1595 for 6819 observed reflections (Ⅰ> 2σ(Ⅰ)).