In the synthesis of catalytically active nanoparticles, combinations of oleic acid and oleylamine are commonly used. This allows the synthesis of tailor-made nanoparticles with core@ shell structures and distinct surface faceting in order to express a facet that is especially beneficial to the reaction in question. This report focuses on the synthesis of core@shell@shell Pt@NiPt@Pt nanoparticles with a rhombic dodecahedral shape and the {110} exposed facets. The synthesis was conducted with a 2:1 mixture of oleylamine and oleic acid as well as with a mixture of oleylamine and dioleamide that was formed from a 2:1 mixture of oleylamine and oleic acid. The use of preformed dioleamide allowed for superior reproducibility as the in situ water release during amide formation and the resulting superheating were avoided. The presence of dioleamide on the surface of the core@shell@shell Pt@ NiPt@Pt nanoparticles was ascertained. While dioleamide is not a particularly strong ligand for either Pt or NiPt surfaces, its formation has to be considered when using oleylamine and oleic acid. When large amounts of these ligands are used, dioleamide should be used instead. The core@shell@shell Pt@NiPt@Pt nanoparticles complete the list of low-index facet-terminated core@ shell NiPt nanoparticles synthesized so far. They showed good initial performance in the catalysis of the methanol oxidation reaction, but their stability needs to be improved.