745015-53-6Relevant academic research and scientific papers
Novel synthesis of zirconocene difluoride and alkyl monofluoride complexes
Spannenberg, Anke,Arndt, Perdita,Baumann, Wolfgang,Burlakov, Vladimir V.,Rosenthal, Uwe,Becke, Sigurd,Weiss, Thomas
, p. 3819 - 3825 (2004)
Starting from zirconocene bis(trimethylsilyl)acetylene complexes Cp′2Zr(L)(η2btmsa) via the 2-vinylpyridine complexes Cp′2Zr(2-vipy) a novel synthetic method for zirconocene difluoride and alkyl monofluoride complexes was elaborated. Examples with selected different ligand systems Cp′2 [Cp2 = bis(η5-cyclopentadienyl); ebthi = 1,2-ethylene-1,1′- bis(η5-tetrahydroindenyl); (thi)2 = bis(η5-tetrahydroindenyl); Me2Si(η5- C5H4)2 = dimethylsilylbis-(η5- cyclopentadienyl); (i)2 = bis(η5-indenyl); ebi = 1,2-ethylene-1,1′-bis(η5-indenyl); and Me 2Si(η5-C9H10)2 = dimethylsilyl-1,1′-bis(η5-tetrahydroindenyl)] were synthesized. In the series of these investigations new complexes (i) 2Zr(THF)(η2-btmsa) (1), rac-(ebi)Zr(THF) (η2-btmsa) (2), (thi)2Zr(2-vipy) (3), Me 2Si(η5-C5H4)2Zr(2- vipy) (4), (i)2Zr(2-vipy) (5), and rac-(ebthi)-Zr(2-Ph-vipy) (6) were prepared as starting materials. Different methods for preparation of the zirconocene difluorides rac-(ebthi)ZrF2 (7), (thi) 2ZrF2 (8), Me4C2(η5- C5H4)2ZrF2 (9), and Me 2Si(η5-C9H10) 2ZrF2 (10) and the monofluorides Cp2Zr(F) (CH2CH2-2-Py) (11), rac-(ebthi)-Zr(F)(CH 2CH2-2-Py) (12), (thi)2Zr(F)(CH 2CH2-2-py) (13), Me2Si(η5-C 5H4)2Zr(F)(CH2CH2-2-py) (14), and Me2Si(η5-C9H10) 2ZrF(Me) (15) are reported and compared. The molecular structures of the bis-η5-tetrahydroindenyl complexes 3, 8, and 13 were confirmed by X-ray crystal structure analysis.
