Improved synthesis and structure of solvated and unsolvated forms of cyclooctatetraene-zirconium and -hafnium dichloride
Abstract
An improved synthesis for [M(η8-C8H8)Cl2(thf)](M = Zr or Hf) and their unsolvated forms [M(η8-C8H8)Cl2] has been developed based on a ligand redistribution reaction between [M(η8-C8H8)(η4-C8H8)] and [MCl4(thf)2](thf = tetrahydrofuran). This reaction was proven to be valuable also in the case of substituted cyclooctatetraenes, as shown in the synthesis of [{Zr[η8-C8H6(SiMe3)2]Cl}2(µ-Cl)2]. Crystallographic details: [Hf(η8-C8H8)Cl2(thf)], space group Cmca, a= 12.308(1), b= 12.005(1), c= 17.470(2)Å, α=β=γ= 90°, Z= 8, and R= 0.032 for 771 independent observed reflections; [{Zr[η8-C8H6(SiMe3)2]Cl}2(µ-Cl)2], space group C2221, a= 10.498(1), b= 23.253(2), c= 15.830(1)Å, α=β=γ= 90°, Z= 4 and R= 0.048 for 3121 independent observed reflections.
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