The organometallic complex Fe[subscript 2](µ-S[subscript 2])(CO)[subscript 6] has interesting biological implications. The concepts of bio-organometallic chemistry are rarely discussed at the undergraduate level, but this experiment can start such a conversation and, in addition, teach valuable synthetic techniques. The lab experiment takes a total of five, 3-h lab periods and includes synthesis, purification, and characterization of the title molecule. The synthesis is done using standard Schlenk line techniques, but the product is air stable, which allows for standard benchtop purification. The compound is characterized using UV-vis spectroscopy, Fourier transform infrared spectroscopy, [superscript 13]C NMR spectroscopy, and mass spectrometry.