Synthesis of [1′-(diphenylthiophosphoryl)ferrocenyl]ethyne and alkyne-metal complexes thereof

The novel functionalized ferrocene alkyne Ph2P(S)fcCtriple bond; length of mdashCH (1; fc = ferrocene-1,1′-diyl) was synthesized from Ph2P(S)fcCHO (6) via the Corey–Fuchs reaction. It was further reacted with K2[HgI4]/KOH to give mercury(II) acetylide Hg{Ctriple bond; length of mdashCfcP(S)Ph2}2 (8), and with [Co2(CO)8] to afford the trimetallic Co2Fe complex [(μ-η2:η2-1){Co(CO)3}2](Co–Co) (9). All compounds were characterized by spectral methods (IR, NMR, and MS) and by combustion or high-resolution MS elemental analyses. In addition, the crystal structures of 1, Ph2PfcBr (5), 6, Ph2P(S)fcCHdouble bond; length as m-dashCBr2 (7), and 9 were determined by single-crystal X-ray diffraction.