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  , a=30.244(9)Å, b=13.586(3)Å, c=24.707Å, β=99.882β=99.882(8)°, V=10002V=10002(5) Å3, Z=4Z=4; for compound 2, C72H60Fe2N12O48V5W10, monoclinic, space group C2/c  , a=30.246a=30.246(6) Å, b=13.909(3)Å, c=25.329c=25.329(5) Å, β=100.34β=100.34(3)°, V=10483V=10483(4) Å3, Z=4Z=4. 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.

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 synthesis under hydrothermal conditions by using different starting materials. Compound 1 is the first example of discrete bicapped Keggin heteropoly tungstovanadates. Polyoxoanions, [Fe(phen)3]2+ cations and water molecules act as building blocks to form two-dimensional (2-D) supramolecular layers through extensive hydrogen bonding.Figure optionsDownload as PowerPoint slide