Molybdocene dichloride intercalation into zirconium phosphate nanoparticles

Molybdocene dichloride (Cp2MoCl2), a metallocene dichloride currently being evaluated as potential anti-cancer drug, has been intercalated into zirconium phosphate, an inorganic layered nanomaterial. Hydrolysis of the chloride ligands appears to occur, leading to the formation of the monocation species ([Cp2Mo(H2O)(OH)](+)), which intercalates into the ZrP layers by ion exchange. IR spectroscopy, X-ray powder diffraction (XRPD), UV-Vis spectrophotometry, scanning electron microscopy with energy dispersive X-ray spectroscopy, NMR spectroscopy, and thermogravimetric analysis were used to confirm the presence of the metallocene between the layers of zirconium phosphate. The XRPD data indicates that a new intercalated phase with an expanded interlayer distance of 11.0 angstrom was obtained; thermogravimetric analysis indicates up to 64% loading in the context of molar ratio (0.64 mol per ZrP formula unit) or 32% exchange capacity. Further evidence for intercalation was obtained from P-31 MAS NMR experiments. IR spectroscopy confirms the presence of the cyclopentadienyl bearing metallocene in the layers. (C) 2015 Elsevier B.V. All rights reserved.