Synthesis and characterization of a reduced molybdenum(v) phosphate, (H3dien)2(H2dien)2 H[NaMo12O24(

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  A new reduced molybdenum(V) phosphate (H3dien)2(H2dien)2H[NaMo12O24(OH)6(HPO4)6 (PO4)2]·nH2O (n =10.93, dien =diethylenetriamine) has been synthesized under hydrothermal conditions and characterized by elemental analyses, IR and X-ray diffraction.C16H96.86Mo12N12NaO72.93P8 (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) (A), β=110.22(2)°, V=4298.4(10) (A)3, Dc=2.354 g/cm3, Z =2, μ(Mo Kα) =1.966 mm-1, F(000) =2990.6, the final R =0.0356 and wR =0.1083 for 8739 observed reflections with Ⅰ > 2σ(Ⅰ).It consists of the sandwich-shaped cluster anions [Na{Mo6O12(OH)3(HPO4)3(PO4)}2] 11-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.
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