Two new cantilever-type polyoxometalates Na5(NH4){VIV[(Mo2O6)CH3C(O)(PO3)2]2}·13H2O (1) and (NH4)4{VIV[(Mo2O6)NH3CH2CH2CH2C(O)(PO3)2]2}·6H2O (2) have been synthesized and characterized by IR spectroscopy, UV-visible spectroscopy, elemental analysis, TG analysis, XPS, 31P NMR and single-crystal X-ray diffraction. The structure analysis reveals that the diphosphonate, hydroxyethylidene diphosphonic acid and alendronic acid as the scaffolds, have been grafted on the “S”-shaped polyoxoanions 1 and 2 respectively. The alkyl groups of the diphosphonates like arms hanged on the polyoxoanions form the cantilever-type polyoxometalates.
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