A Novel 3D Polyoxotungstate Constructed from Dawson Polyanions and Alkaline Earth Cations

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A novel 3D polyoxotungstate[Ca(H2O)2][Ca(H2O)3]H2[P2W18O62]·9H2O(1)has been synthesized by the conventional aqueous solution method and characterized by IR spectrum,elemental analyses,single-crystal X-ray diffraction and electrochemistry.1 crystallizes in triclinic,space group (P1)with a = 12.9077(14),b = 14.8593(16),c = 20.023(2)(A),α = 70.1620(10),β =80.8110(10),γ = 64.3770(10)°,V= 3256.9(6)(A)3,Z= 2,Dc = 4.790 g/cm3,μ = 31.975 mm-1,F(000)= 4080,R = 0.0412,and wR = 0.1039.X-ray single-crystal structural analysis indicates that the molecular structural unit of 1 consists of one saturated Dawson[α-P2W18O62]6-polyanion,one seven-coordinate[Ca(H2O)2]2+cation,one eight-coordinate[Ca(H2O)3]2+cation,two protons and nine lattice water molecules.Interestingly,adjacent Dawson[α-P2W18O62]6-polyanions are connected by[Ca(H2O)2]2+and[Ca(H2O)3]2+cations and hydrogen bonding interactions to form a3D infinite framework.The electrochemistry property of 1 has been studied.
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