Crystal structure, IR Data, Raman Data, Mass Spectrum, Bis(/2-pentanethiolato)mercury(II)The preparation of bis(/?-pentanethiolato)mercury(II), Hg(SC5Hn)2, and n-pentanethiolatomercury(II) iodide, IH gSC sH n, starting from H gl2 and rc-pentanethiol, is presented; the X-ray crystal structure determination of Hg(SC5H n)2 reveals a layered structure of the bis(thiolate) molecule. With 178.69(1.02)° the S-H g-S moiety is nearly linear. The Hg-S bond length is shorter then the sum of the covalent radii of sulphur and mercury atoms indicating a primary co-ordination number of two, which is supported by the IR and Raman spectra. Assignments of i/Sym(Hg-S) and i'asym(Hg-S) are given. The mass spectrum reveals the title compound to be monomeric in the gas phase. Melting and thermal decomposition have been investigated by DTA methods. The behaviour towards organic thiols is discussed. In addition, IR and Raman spectroscopic data of IH gSCsHn are presented and discussed.