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Open AccessArticle

Synthesis, APPI Mass-Spectrometric Characterization, and Polymerization Studies of Group 4 Dinuclear Bis(ansa-metallocene) Complexes

1
Univ Rennes, CNRS, ISCR (Institut des Sciences Chimiques de Rennes), UMR 6226, F-35000 Rennes, France
2
CNRS, COBRA, Univ Rouen, UMR 6014, F-76821 Mont Saint Aignan, France
3
Total Research and Technologies Gonfreville, BP 27, F-76700 Harfleur, France
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Total Raffinage Chimie, Joint Laboratory C2MC (Complex Matrices Molecular Characterization), Univ Pau, Univ Rouen, CNRS, F-64053 Pau, France
5
Total Research and Technologies Feluy, Zone Industrielle C, B-7181 Feluy, Belgium
6
Total SA, Direction scientifique, F-92069 Paris La Défense, France
*
Authors to whom correspondence should be addressed.
Catalysts 2018, 8(11), 558; https://doi.org/10.3390/catal8110558
Received: 25 October 2018 / Revised: 11 November 2018 / Accepted: 13 November 2018 / Published: 19 November 2018
(This article belongs to the Section Catalysis in Organic and Polymer Chemistry)
New ligand platforms of the type p- or m-Ph{-CR(3,6-tBu2Flu)(Cp)}2 (para-, R = Me (2a), H (2b); meta-, R = Me (2c)) were synthesized via nucleophilic addition of the 3,6-tBu2-fluorenyl-anion onto the parent phenylene-bridged difulvenes (1ac). The corresponding discrete homodinuclear zirconium and hafnium bis(dichloro ansa-metallocene) complexes, Ph[{-CR(3,6-tBu2Flu)(Cp)}MCl2]2 (p-, R = Me (3a-Zr2, 3a-Hf2), R = H (3b-Zr2); m-, R = Me (3c-Zr2), were prepared by salt metathesis reactions. An attempt to generate in situ a heterodinuclear complex 3a-Zr-Hf was also undertaken. For the first time, Atmospheric Pressure PhotoIonization (APPI) mass-spectrometric data were obtained for all dinuclear compounds and found to be in excellent agreement with the simulated ones. Preliminary studies on the catalytic performances of these dinuclear complexes, upon activation with MAO, in ethylene homopolymerization and ethylene/1-hexene copolymerization revealed a few differences as compared to those of the monometallic analogues. In particular, slightly lower molecular weights and a greater formation of short methyl and ethyl branches were obtained with the dinuclear systems. View Full-Text
Keywords: metallocene catalysts; mass-spectroscopy; olefin polymerization metallocene catalysts; mass-spectroscopy; olefin polymerization
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MDPI and ACS Style

Schnee, G.; Farenc, M.; Bitard, L.; Vantomme, A.; Welle, A.; Brusson, J.-M.; Afonso, C.; Giusti, P.; Carpentier, J.-F.; Kirillov, E. Synthesis, APPI Mass-Spectrometric Characterization, and Polymerization Studies of Group 4 Dinuclear Bis(ansa-metallocene) Complexes. Catalysts 2018, 8, 558. https://doi.org/10.3390/catal8110558

AMA Style

Schnee G, Farenc M, Bitard L, Vantomme A, Welle A, Brusson J-M, Afonso C, Giusti P, Carpentier J-F, Kirillov E. Synthesis, APPI Mass-Spectrometric Characterization, and Polymerization Studies of Group 4 Dinuclear Bis(ansa-metallocene) Complexes. Catalysts. 2018; 8(11):558. https://doi.org/10.3390/catal8110558

Chicago/Turabian Style

Schnee, Gilles; Farenc, Mathilde; Bitard, Leslie; Vantomme, Aurelien; Welle, Alexandre; Brusson, Jean-Michel; Afonso, Carlos; Giusti, Pierre; Carpentier, Jean-François; Kirillov, Evgueni. 2018. "Synthesis, APPI Mass-Spectrometric Characterization, and Polymerization Studies of Group 4 Dinuclear Bis(ansa-metallocene) Complexes" Catalysts 8, no. 11: 558. https://doi.org/10.3390/catal8110558

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