The compound of diphosphopentamolybdate {[Cu(en) (Hen)]2[P2Mo5O23]}·3H2O [en=ethylenediamine] had been obtained from the hydrothermal method and characterized by single crystal X-ray diffraction, elemental analysis, FT-IR, and thermogravimetric analysis. The structure consist of [P2Mo5O23]6- clusters anions, complex [Cu(en) (Hen)]3+ cations and crystallization water molecules, which are held together to a two-dimensional framework. The most interesting feature of the compound is that two nitrogen atoms are both coordinated with Cu (Ⅱ) in one ethylenediamine molecule, for the other ethylenediamine molecule, only one nitrogen atom is towards Cu (Ⅱ) and the other nitrogen atom is protonated and formed Hen+.
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