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A novel inorganic-organic hybrid polyoxomolybdate (C 4 H 16 N 3 ) 2 [NiMo 12 O 40 ]Cl 2 ⋅ 9H 2 O has been synthesized under hydrothermal conditions and structurally caracterised by elemental analysis, TG, IR and single crystal X ray diffraction. The crystals are orthorhombic, a = 10.138(3) Å, b = 19.508(2) Å, c = 26.790(4) Å, Z = 4, sp. gr. Pcnb. Keggin polyoxomolybdate anion [NiMo 12 O 40 ] 4-, protonated diethylen etriamine molecules, chloride anions and water molecules are linked via a large number of hydrogen bonds.

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The crystal structure, Hirshfeld surface analysis and spectroscopic analysis of a new polyoxometalate (POM) compound, namely, nonakis(2-methoxyaniline) bis(diphosphopentamolybdate) trihydrate, (C 7 H 9 NO) 9 [P 2 Mo 5 O 23 ] 2 Á3H 2 O, is reported. The title compound was synthesized using the solution method and was structurally characterized by single-crystal X-ray diffraction, which revealed P1 symmetry. A study of the intermolecular interactions using Hirshfeld surface analysis confirmed that the hydrogen-bonding interactions play the dominant role in the stability of the crystal structure. The refinement was complicated by extensive disorder affecting 11 of the 16 ions and molecules in the asymmetric unit. IR and UV-Vis spectroscopic techniques were used to identify the vibrational modes and to classify this compound as an insulator.

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