A mixture of pyridoxalrhodanine, triethylphosphinegold(I) chloride,and sodium methoxide in methanol unexpectedly afforded theazacoumarin complex [Au(TS)(PEt
3)] [HTS = 5-(hydroxymethyl)-8-methyl-3-thiol-7-azacoumarin], which was characterized by X-raydiffractometry. Its crystals consist of independent molecules in whichthe metal atom is bound to the azacoumarin [Au-S = 2.9458(18)Å] and the phosphine [Au-P = 2.262(2) Å] in an almost lineararrangement [P1-Au1-S1 = 176.93(7)
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]. The complex showedbetter in vitro antitumor activity than cisplatin against the cisplatin-resistant cell line A2780cis.