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In this study, the usage of ClCH2CCCH2Cl alkyne as a reagent for the oxidative addition reaction with organoplatinum‌(II) complex [PtMe2(bipy)] (1), in which bipy = 2,2′‐bipyridine to give a mixture including of trans‐[PtClMe2(CH2CCCH2Cl)(bipy)] (2a) and a cis‐[PtClMe2(CH2CCCH2Cl)(bipy)] (2b) complexes is reported. Kinetic study was investigated by monitoring the disappearance of the metal‐to‐ligand charge transfer (MLCT) band in the UV–Vis spectra. 1H NMR experimental results confirmed that trans isomer (2a) is more stable than its corresponding cis isomer. A liquid–liquid planar interface has been employed as a template for self‐assembly of platinum nanoparticles. The as prepared complex was applied for the synthesis of platinum thin film that characterized by transmission electron microscopy (TEM), X‐ray diffraction (XRD), energy dispersive analysis of X‐rays (EDAX), field emission‐scanning electron micrographs (FE‐SEM) and elemental mapping. The electrocatalytical activity of Pt thin film was investigated in methanol oxidation reaction.