Deacon, Glen B., Forsyth, Craig M., Jaroschik, Florian, Junk, Peter C., Kay, Danielle L., Maschmeyer, Thomas, Masters, Anthony F., Wang, Jun, and Field, Leslie D. (2008) Accessing decaphenylmetallocenes of ytterbium, calcium, and barium by desolvation of solvent-separated ion pairs: overcoming adverse solubility properties. Organometallics, 27 (18). pp. 4772-4778.

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Abstract

The redox-transmetalation ligand-exchange reaction of ytterbium or calcium metal with 2 equiv of pentaphenylcyclopentadiene (C5Ph5H) and 1 equiv of HgPh2 in thf afforded the solvent-separated ion pairs (SSIPs) [M(thf)6][C5Ph5]2 (M = Yb, Ca), which were characterized by single-crystal X-ray analyses. Addition of toluene to the isolated SSIPs led to the precipitation of the homoleptic sandwich complexes [M(C5Ph5)2] (M = Yb, Ca). In the reaction of barium metal with C5Ph5H and HgPh2 the corresponding SSIP was observed in situ, and only the sandwich complex [Ba(C5Ph5)2] could be isolated. Single-crystal X-ray analyses were carried out for [M(C5Ph5)2] (M = Yb, Ba), which confirmed the highly symmetric structure of these complexes with two parallel cyclopentadienyl ligands. Oxidation and metal-ligand exchange reactions were investigated for the divalent ytterbium complexes.

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