Study of N,N′-dihydroxyethyldithiooxamide by X-ray diffraction, u.v.-vis, NMR, Raman and i.r. spectroscopy

Abstract The vibrational, NMR and electronic spectra of HO(CH 2 ) x NHCSCSNH(CH 2 ) x OH ( x = 2,3,5,6) are discussed. A vibrational analysis has been proposed for the N,N ′-dihydroxyethyldithiooxamide ( x = 2) and its deuterated (NH/ND, OH/OD) analogue. The structure of N,N ′-DHEDTO was solved by X-ray analysis. M r = 208, monoclinic, space group P 2 1 / n, a = 9.8800(5) A, b = 11.3260(7) A, c = 9.7806(8) A, β = 119.366(5)°, V = 953.8 A 3 , Z = 4, Dc = 1.365 Mgm −1 ,μ(CuKα) = 0.47 mm −1 , F (000) = 440.00, T = 300 K. Final conventional R -factor = 0.036, R w = 0.037, for 1608 unique reflections with I > 3.σ( I ) out of 1800 measurements. The structure was solved using the automatic programs PATSYS and DIRDIF. The two νOH bands in the i.r. spectrum are in agreement with the crystallographic structure, which proposes that the unit cell of the compound consists of two independent molecules.