Hydrothermal synthesis and characterization of two novel tungstovanadophosphate derivatives

作者:Ma Feng Xia; Chen Ya Guang*; Shi Dong Mei; Meng Fan Xia; Pang Hai Jun
来源:Transition Metal Chemistry, 2008, 33(6): 697-703.
DOI:10.1007/s11243-008-9099-2

摘要

Two novel tungstovanadophosphate derivatives, namely [Fe(phen)(3)](2)[PW(8)(vi)V(V)V(5)(IV)O(42)] center dot H(2)O (1) and [Fe(phen)(3)](2)[PW(9)V(3)O(40)] (2), were synthesized under hydrothermal conditions, and characterized by elemental analysis, IR, ESR, XPS, TGA, and single-crystal X-ray diffraction analysis. The crystal structure analyses reveal that the 'mixed-addenda' Keggin polyoxoanion in 1 is decorated with VO(2+) units, such that four V atoms are disordered over eight metal sites; the anion in compound 2 has a typical Keggin structure with three V atoms disordered over 12 metal sites. The two compounds are ionic crystals with slightly different packing modes for the polyoxoanions and [Fe(phen)(3)](3+) cations. pi-pi stacking interactions between phen molecules, weak hydrogen bonding interactions between phen ligands and polyoxoanions, and electrostatic forces lead to an extended 3D supramolecular framework.