In this study, the selective oximation of structurally diverse aromatic aldehydes (versus ketones) to the corresponding aldoxime derivatives was investigated using the combination system of NH₂OH.HCl and bisthiourea complexes of cobalt, nickel, copper and zinc chlorides, M^II(tu)₂Cl₂, in a mixture of CH₃CN‒H₂O (1:1 mL). All reactions were carried out successfully at room temperature within the immediate time up to 130 min giving the products in high yields. Investigation of the results exhibited that the applied bis-thiourea metal complexes show the catalytic activity in order of Co(tu)₂Cl₂₂Cl₂₂Cl₂₂Cl₂ in their oximation reactions.