Novel polyoxometalate-based organic-inorganic hybrid [NH3-CH(CH3)COOH][H3O]8[PMo12O40]3.4NH3CH(CH3)COO was synthesized and characterized by 31P, 1H, 13C NMR and IR spectroscopies, elemental analysis and single crystal X-ray determination. Two of the PMo12O40 3- anions in the title hybrid are symmetrically equivalent. They are crystallographically independent from the third PMo12O40 3- polyoxoanion, in the case of various interactions with neighboring components in the crystal network (i.e. +NH3-CH(CH3)-COOH and H3O+ cations, +NH3CH(CH3)COO- zwitterions and polyoxoanions). The compound crystallizes in an orthorhombic C222 space group with a = 16.0392(16) Å, b = 34.480(4) Å, c = 12.8968(13) Å and Z = 2.

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