The charge transfer complex N,N-dimethylbenzylamine which is between the molybdosilicic acid and organic substrate has been prepared. Yellow crystals of the title compound ([(CH3)2NH(CH2)C6H5]4SiMo12O402CH3CNH2O) were synthesized from the mixture of water and acetonitrile. The single-crystal X-ray analysis reveals that the crystal crystallizes in triclinic system, space group P1 with a = 13.313(2), b = 14.673(2), c = 19.736(3) ? a = 86.22(1), b = 88.76(1), g = 66.97(1), V = 3540.2(9) 3 and Z = 2. The anion has the Keggin structure. The MoO bond distances range from 1.675(3) to 1.691(3) ?for the terminal oxygen atoms, 1.798(3) to 2.045(3) ?for the bridging ones, and 2.328(3) to 2.361(3) ?for those in the SiO4 tetrahedron. The SiO bond distances fall in the range of 1.623(3)～1.630(3) ?
The salt, [Y（H2O）8]2[V10O28]·9H2O, contains two discrete water-groups coordinated Y（Ⅲ） cations, an isopoly complex ion, decavanadate （V10O28^6-） and nine additional water molecules, which are combined together by static electric forces and hydrogen bonds. The y^3＋ is eight-coordinated with a square antiprism geometry. The single-crystal X-ray analysis reveals that the crystal crystallizes in triclinic, space group P1^- with a = 9.1454 （18）, b = 10.007（2）, c = 12.772（3） A°, α= 68.86（3）, β = 77.50（3）, γ= 89.23（3）°, V= 1061.7（4）A°^3 and Z= 1.
