Polyoxometalates (POMs) form a large and characteristic class of inorganic compounds with interesting properties [1, 2]. POMs chemistry has generated substantial interest especially in many fields such as medicine, theoretical studies and catalytic applications [3, 4]. Among the reported large POMs clusters, Preyssler anion possesses unusual doughnut–shaped structure and has recently shown its good properties in catalysis and material science [5]. To the best of our knowledge, this contribution report now, for the first time, synthesis and characterization of a novel hybrid built on Preyssler anion and mixed proline-leucine amino acids. The prepared crystals after purification have been characterized by IR and 1H-NMR approaches. The peaks at 1250-1725 cm-1 and 2950-2985 cm-1 are the characteristic bands of amino acids and prominent bands for the anion are located at1163, 1079, 1018, 932, 910, 780 cm-1. These results indicate that the polyanions in the title compound still retain the basic Preyssler structure, but we believed the compound is distorted due to the effects of hydrogen bonding interactions. The obtained results from 1H-NMR studies are consistent with IR analysis and confirm the presence of both amino acids in the crystal structure. Also further researches and characterization on this category of complexes

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