Hydrothermal synthesis and characterization of two new bicapped Keggin heteropoly tungstovanadated derivatives

Two new heteropoly tungstovanadate derivatives, [Fe(phen)3]2[W10.5V4.5O42]·3H2O (1) and [Fe(phen)3]2[W10V5O42].6H2O (2) (phen=1,10′-phenanthroline), have been synthesized under hydrothermal conditions by using different starting materials, and characterized by elemental analysis, IR, ESR, XPS, TGA and single-crystal X-ray diffraction analysis. Crystal data for compound 1: C72H54Fe2N12O45V4.5W10.5, monoclinic, space group C2/c, image, image, image, image(8)°, image(5) Å3, image; for compound 2, C72H60Fe2N12O48V5W10, monoclinic, space group C2/c, image(6) Å, image, image(5) Å, image(3)°, image(4) Å3, image. The crystal structure analysis reveals that both polyoxoanions are decorated with the [Fe(phen)3]2+ cations, and that they have analogous structure to each other with slightly different packing modes of the polyoxoanions, [Fe(phen)3]2+ cations and water molecules. They are further linked to form two-dimensional (2D) supramolecular networks through extensive hydrogen bonding.