Structural, spectroscopic characterization and EPR studies of tetramethylammonium-hydrogen fumarate-fumaric acid complex

Abstract

The tetramethylammonium-hydrogen fumarate-fumaric acid (hereafter, [TMAHF-FA]) complex was synthesized and characterized by spectroscopic (IR), structural (XRD) and electron paramagnetic resonance (EPR) techniques. In the crystal structure, tetramethylammonium cation lies on a mirror plane of the space group P2(1)/m. Crystal structure analysis reveals that there is a large degree of proton sharing between the fumaric acid and hydrogen fumarate, with the H atom lying almost symmetrically between the donor and acceptor sites, as evidenced by the long O-H and short H center dot center dot center dot O distances [1.19(3)angstrom, 1.26(3)angstrom], respectively. gamma-Irradiation damage centers in [TMAHF-FA] single crystal have been investigated by EPR at room temperature. The spectra indicated the existence of C(alpha)H(alpha)C(beta)H(beta)COO(-) radical. The EPR spectra recorded in the three mutually perpendicular planes have shown two magnetically distinct paramagnetic sites in monoclinic lattice. The principal values of g and hyperfine constants for both sites were calculated. IR spectrum was resolved and transitions were assigned based on the molecular structure. (c) 2008 Elsevier Ltd. All rights reserved.