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

The novel functionalized ferrocene alkyne Ph₂P(S)fcCCH (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{CCfcP(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)fcCHCBr₂ (7), and 9 were determined by single-crystal X-ray diffraction.