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Reaction of copper sulfate with two ligands, pyridoxal [3-hydroxy-5-(hydroxymethyl)-2-methylpyridine-4-carbaldehyde] (H2L) and methylpyruvate thiosemicarbazones (Hmpt) leads to the formation of two new complexes [Cu(H2L)(OH2)2]SO4·H2O (1) and [Cu(Hpt)(OH2)2SO4] (2) (H2pt = pyruvic acid thiosemicarbazone) which have been characterized using single-crystal X-ray diffraction and IR spectroscopy. Crystals of complex 1are triclinic, space group Pl¯, with a= 10.885(4), b= 10.022(4), c= 8.721(4)Å, α = 87.38(2), β = 72.14(3), γ = 64.99(1)° and Z= 2. Compound 2crystallizes monoclinic, space group C2/c, with a= 15.478(2), b= 17.733(2), c= 6.891(1)Å, β = 106.10(2)° and Z= 4. The structure of 1consists of discrete [Cu(H2L)(OH2)2]2cations, SO42anions and uncoordinated water molecules; in complex 2the sulfate group acts as bridging bidentate giving rise to dimers produced by a two-fold axis. In both compounds the copper atom is coordinated in a rather distorted square pyramid. The main vibrational bands are also discussed.