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To advance their use in green energy, it is crucial to understand what controls the formation of intermetallic NPs over alloy structures. By carefully selecting the additives used in NP synthesis, it is here shown that monodisperse, intermetallic PdCu NPs can be synthesized in a controllable manner. Introducing the additives iron(III) chloride and ascorbic acid, both morphological and structural control can be achieved. Combined, these additives provide a synergetic effect resulting in precursor reduction and defect\u2010free growth; ultimately leading to monodisperse, single\u2010crystalline, intermetallic PdCu NPs. Using in situ X\u2010ray total scattering, a hitherto unknown transformation pathway is reported that diverges from the commonly reported coreduction disorder\u2013order transformation. A Cu\u2010rich structure initially forms, which upon the incorporation of Pd(0) and atomic ordering forms intermetallic PdCu NPs. 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