The synthesis and characterization of the dicarbonyl mixed ligand cis-[Re-(CO)(2)(quin)(cisc)(PPh3)] complex, 4, where quin is the deprotonated quinaldic acid, cisc is cyclohexyl isocyanide, and PPh3 is triphenylphosphine, is presented. The synthesis of 4 proceeds in three steps. In the first, the intermediate fac-[Re(CO)(3)(quin)(H2O)] aqua complex 2 is generated from the fac-[NEt4](2)[Re(CO)(3)Br-3] precursor, together with the brominated products fac-[Re(CO)(3)(quinH)(Br)] la and fac-[NEt4][Re(CO)(3)(quin)(Br)] 1b, in low yield. In the following step, replacement of the aqua ligand of complex 2 by the monodentate isocyanide ligand leads to the formation of fac-[Re(CO)(3)(quin)(cisc)], 3. In the third step replacement of the species trans to the isocyanide carbonyl group of 3 by a phosphine generates complex 4. The Re complexes 2-4 were prepared in high yield and fully characterized by elemental analysis, spectroscopic methods, and X-ray crystallography. At the technetium-99m (Tc-99m) tracer level, the analogous complexes 3' and 4' were produced in high radiochemical purity, characterized by comparative reverse phase high-performance liquid chromatography and showed high resistance to transchelation by histidine or cysteine. This new [N,O] [C] [P] donor atom combination with the cis-[M(CO)(2)](+) core (M = Re, Tc-99m) is a promising scaffold for the development of novel diagnostic and therapeutic targeted radiopharmaceuticals.