Synthesis and characterization of vanadium and molybdenum compounds containing ligands with oxygen groups

In this study, organic or inorganic ligands containing oxo and/or polyoxo groups tried to incorporate with vanadium/molybdenum precursors to obtain new polyoxometalates, heteropolyoxometalates and inorganic-organic hybrid compounds. Multifunctional rigid type carboxylate ligands as tethers for the construction of solid phases were used to obtain diverse and unusual topologies. Selected inorganic and organic polyoxo ligands in this study were sulfate, 1,2,4,5-Benzenetetracarboxylic acid (BTCA), 1,4-cyclohexanedicarboxylic acid (CHDC) and 2,6-naphthalenedicarboxylic acid (NDC) to reach the purposes. The successful reactions gave one heteropolyoxomolybdate containing compound, two inorganic-organic hybrid compounds and one V/O/SO4 solid-state compound. Among these compounds, only (N(C2H5)4)4[VMo12V2O44] has been fully characterized including single crystal x-ray structural analysis. The other compounds were formulated as [V2O2(OH)2SO4], [VOC6H10(COO)2] and [V2O2(C10H6(COO)2)] by characterization methods excluding single crystal x-ray structural analysis: determination of the physical properties of the compound, infrared spectroscopy (FTIR), manganometric titration, element analysis (CHNS analysis), Thermogravimetric Analysis (TGA) and x-ray diffraction pattern determination (XRD powder).In this study, several synthesis methods like reflux and hydrothermal/solvothermal synthetic methods have been applied. However, the hydrothermal synthetic methods to prepare novel reduced oxovanadium/oxomolybdenum phases and HPOM incorporating polyoxo ligands were successful. Result of this study could be summarized as ?Vanadium and Molybden always have more tendencies to form POM and/or HPOM than to form hybrid solids. Hydrothermal reaction methods are still promising techniques to synthesize new hybrid solids, POMs and HPOMs?.