Targeted Synthesis Of A Polypyridyl Polyoxometalate Coordination Complex Using Microwave-Assisted Reaction Conditions

In this article, we build upon our recent efforts that have focused on demonstrating the value of microwave-assisted synthesis in polyoxometalate (POM) chemistry. Herein, we report for the first time a microwave-assisted approach that enabled the facile preparation and crystallization of a large POM-containing coordination complex. The judicious selection and reaction of a sparingly water-soluble transition-metal-substituted polyanion (TMSP) salt with the tritopic ligand 2,4,6-tris(4-pyridyl)-1,3,5-triazine (TPT) in a mixed solvent system under moderately forcing conditions yields Ba-9[((BW11O39CoIII)-W-III-O-VI)(3)- C18H12N6)]center dot 38H(2)O in moderate yield. Crystallographic analysis reveals significant intermolecular interactions between the organic ligand and neighbouring polyanions, predominantly C-H center dot center dot center dot O(water) in nature; meanwhile, the solvated regions of the crystal show significant disorder. To supplement the crystallographic study, combustion analysis, and IR and H-1 NMR spectroscopic analyses were conducted, revealing good bulk purity and the stability of the complex in aqueous media.