The reaction of 1,1-diethyl-3-(4-fluorobenzoyl)-thiourea (HL) with CuCl2 · 2H2O and NiCl2 · 6H2O give two complexes, Cu(HL)3Cl (1) and NiL2 (2). The crystal structures of these products were determined by single crystal X-ray diffraction. In 1, three HL molecules are unidentate, coordinating through the sulfur, and the copper is tetrahedral with three S and one Cl. In 2, two HL molecules are O and S donor bidentate and coordinate as anionic species with loss of the proton from the acyl-substituted nitrogen; the nickel is square-planar.