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A new reduced molybdenum(V) phosphate (H3dien)2(H2dien)2[NaMo12O24 (OH)6 (H2PO4)(HPO4)5(PO4)2]·nH2O (n = 10.92, dien = diethylenetriamine) has been synthesized under hydrothermal conditions and characterized by elemental analyses, IR and X-ray diffraction. C16H96.84Mo12N12NaO72.92P8 (Mr = 3046.73) crystallizes in the monoclinic system, space group P21/c with a = 13.3575(18), b = 21.907(3), c = 15.654(2) , β = 110.22(2)°, V = 4298.4(10) 3, Dc = 2.354 g/cm3, Z = 2, μ(MoKα) = 1.966 mm-1, F(000) = 2990.4, the final R = 0.0357 and wR = 0.1086 for 8739 observed reflections with I > 2σ(I). It consists of sandwich-shaped cluster anions [Na{Mo6P4}2]10- held together into a three-dimensional supramolecular framework through intermolecular hydrogen-bonding contacts. A probe reaction of the oxidation of acetaldehyde with H2O2 showed that this compound has high catalytic activity in the reaction.
A new reduced molybdenum (V) phosphate (H3dien) 2 (H2dien) 2 [NaMo12O24 (OH) 6 (H2PO4) (HPO4) 5 (PO4) 2] nH2O (n = 10.92, dien = diethylenetriamine) has been synthesized under hydrothermal conditions and characterized by elemental analyzes, IR and X-ray diffraction. C16H96.84Mo12N12NaO72.92P8 (Mr = 3046.73) crystallizes in the monoclinic system, space group P21 / c with a = 13.3575 (18), b = 21.907 (2), V = 4298.4 (10) 3, Dc = 2.354 g / cm3, Z = 2 and μ (MoKα) = 1.966 mm- = 2990.4, the final R = 0.0357 and wR = 0.1086 for 8739 observed reflections with I> 2σ (I). It consists of a sandwich-shaped cluster anions [Na {Mo6P4} 2] 10- held together into a three-dimensional supramolecular framework through intermolecular hydrogen-bonding contacts. A probe reaction of the oxidation of acetaldehyde with H2O2 showed that this compound has high catalytic activity in the reaction.