Synthesis and characterization of materials containing arrays of decavanadate clusters

The synthesis and characterization by single crystal x-ray structure analysis, manganometric titration, valence sum calculations, thermogravimetric analysis, and IR spectroscopic studies of (HN(CH2CH2)3NH)2(Na(H2O)2)(HV10O28)*2H2O (1) and (H3N-4-C5H4N)2(NH4)4(V10O28)*xH2O (2) has been described. The structure of 1 consists of alternating layers composed of two-dimensional arrays of decavanadate clusters (HV10O28)5- interlinked by the [Na(H2O)2O4] moieties, separated by the doubly protonated DABCO cations-- (HN(CH2CH2)3NH)2+. The structure exhibits a fascinating network of hydrogen bonds between cations, solvate water molecules and anion clusters. The crystal structure of 2 contains three-dimensional arrays of (V10O28)6- cluster anions, protonated 4-aminopyridinium groups, ammonium ions, and water molecules. Crystal data for 1: C12H37N4Na2O32V10, Monoclinic space group C2/m, a = 20.4242(8), b = 8.4550(3), c = 11.9255(5)A , beta = 122.0500(10) degrees, Volume = 1745.49(12)(A3), Z = 2, Dcalc = 2.439 Mg/m3. Crystal data for 2: Triclinic space group Pi, a =14.911(2), b = 16.928(2), c = 39.714(5)A, a = 84.454(2), (beta = 84.895(2), ?= 79.603(2) degrees, Volume = 9787.4(13) A3, Z = 8.