The synthesis and characterization of the novel systems [Zn-2(H2N(CH2)(2)NH2)(5)][{Zn(H2N(CH2)(2)NH2)(2)}(2)V18O42(H2O).9H(2)O (1), [Cd-2(H2N(CH2)(2)NH2)(5)][{Cd(H2N(CH2)(2)NH2)(2)}(2)V18O42(Br)].9H(2)O (2), and [Zn-2(H2N(CH2)(2)NH2)(5)][{Zn(H2N(CH2)(2)NH2)(2)}(2)V18O42(CI).9H(2)O (3) have been described. These materials represent a new class of solids that have been prepared by combining conventional coordination compounds with spherical polyoxovanadate clusters. The isomorphous structures of these hybrid solids consist of two-dimensional arrays of container cluster molecules {V18O42(X)} (X = H2O, Br-, Cl-) interlinked by the transition metal complex moieties {M(H2N(CH2)(2)NH2)(2)} (M = Zn, Cd). These compounds contain an unprecedented complex cation, {M-2(H2N(CH2)(2)NH2)(5)](4+). Crystal data for 1: C9H46N9O26V9Zn2, monoclinic space group P2(1/m) (No. 11), a = 12.3723(7) Angstrom , b = 20.9837(11) Angstrom, c = 15.8379(8) Angstrom, beta = 97.3320(10)degrees, Z = 4.
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