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Synthesis and Structural Characterization of New Zirconium(IV) Bent Metallocenes comprising η 8 ‐Cyclooctatetraenyl and Bulky Cyclopentadienyl Ligands
Author(s) -
Rausch Janek,
Liebing Phil,
Kühling Marcel,
Lorenz Volker,
Hrib Cristian G.,
Hilfert Liane,
Edelmann Frank T.
Publication year - 2017
Publication title -
zeitschrift für anorganische und allgemeine chemie
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.354
H-Index - 66
eISSN - 1521-3749
pISSN - 0044-2313
DOI - 10.1002/zaac.201700188
Subject(s) - cyclopentadienyl complex , zirconium , phenyllithium , crystallography , crystal structure , trimethylsilyl , derivative (finance) , chemistry , yield (engineering) , stereochemistry , medicinal chemistry , materials science , inorganic chemistry , organic chemistry , catalysis , financial economics , economics , metallurgy
The new zirconium bent metallocenes (COT)Zr(Cp t Bu2 )Cl ( 1 ) and (COT)Zr(Cp′′)Cl ( 2 ) were synthesized in a straightforward manner and in high yields ( 1 : 91 %, 2 : 86 %) by treatment of in situ ‐prepared (COT)ZrCl 2 (THF) with 1 equiv. of K(Cp t Bu2 ) or K(Cp′′), respectively (COT = η 8 ‐cyclooctatetraenyl; Cp t Bu2 = η 5 ‐1,3‐di‐ tert ‐butylcyclopentadienyl; Cp′′ = η 5 ‐1,3‐bis(trimethylsilyl)cyclopentadienyl). Subsequent reaction of 1 with 1 equiv. of phenyllithium afforded the σ ‐phenyl derivative (Cp t Bu2 )Zr(COT)Ph ( 3 ) as orange crystals in 83 % isolated yield. All three new compounds were structurally characterized through single‐crystal X‐ray diffraction.