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

摘要

Two new heteropoly tungstovanadate derivatives, [Fe(phen)(3)](2)[W10.5V4.5O42] (.) 3H(2)O (1) and [Fe(phen)(3)](2)[W10V5O42].6H(2)O (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)angstrom, b = 13.586(3)angstrom, c = 24.707 angstrom, beta = 99.882(8)degrees, V = 10002(5) angstrom(3), Z = 4; for compound 2, C72H60Fe2N12O48V5W10, monoclinic, space group C2/c, a = 30.246(6)angstrom, b = 13.909(3)angstrom, c = 25.329(5)angstrom, beta = 100.34(3)degrees, V = 10483(4)angstrom(3), Z = 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. (c) 2005 Elsevier Inc. All rights reserved.