A1 Vertaisarvioitu alkuperäisartikkeli tieteellisessä lehdessä
Bis[2-(tert-butyldimethylsiloxy)-4,7-dimethylindenyl]zirconium dichloride, synthesis, torsional isomerism and olefin polymerization catalysis
Tekijät: Leino R, Luttikhedde HJG, Lehtonen A, Sillanpaa R, Penninkangas A, Stranden J, Mattinen J, Nasman JH
Kustantaja: ELSEVIER SCIENCE SA
Julkaisuvuosi: 1998
Lehti:: Journal of Organometallic Chemistry
Tietokannassa oleva lehden nimi: JOURNAL OF ORGANOMETALLIC CHEMISTRY
Lehden akronyymi: J ORGANOMET CHEM
Vuosikerta: 558
Numero: 1-2
Aloitussivu: 171
Lopetussivu: 179
Sivujen määrä: 9
ISSN: 0022-328X
DOI: https://doi.org/10.1016/S0022-328X(98)00368-4
Tiivistelmä
The synthesis and characterization of an unbridged metallocene catalyst precursor bis[2-(tert-butyldimethylsiloxy)-4:7-dimethylindenyl]zirconium dichloride (3) is reported. The solid state structure of 3 reveals two different rotamers in the asymmetric unit corresponding to a C-1 symmetric, 'central/lateral:gauche'-like conformation, and a C-2 symmetric, 'central:syn' conformation, respectively. The H-1 and C-13 NMR spectra of 3 are, at ambient temperature, consistent with time-averaged molecular C-2v symmetry. Dynamic NMR measurements show splitting of the H-1 resonances at 173 K indicating that a single C-2 symmetric bent-metallocene conformation is observed. Upon activation with methylaluminoxane, 3 polymerizes ethylene with an activity of 500 kg PE/mol Zr/h (T-p = 80 degrees C; P(C2H4) = 1.6 bar; [Al]:[Zr] = 3000:1; M-w = 43000; M-w/M-n = 2.2; T-m = 133 degrees C). (C) 1998 Elsevier Science S.A. All rights reserved.
The synthesis and characterization of an unbridged metallocene catalyst precursor bis[2-(tert-butyldimethylsiloxy)-4:7-dimethylindenyl]zirconium dichloride (3) is reported. The solid state structure of 3 reveals two different rotamers in the asymmetric unit corresponding to a C-1 symmetric, 'central/lateral:gauche'-like conformation, and a C-2 symmetric, 'central:syn' conformation, respectively. The H-1 and C-13 NMR spectra of 3 are, at ambient temperature, consistent with time-averaged molecular C-2v symmetry. Dynamic NMR measurements show splitting of the H-1 resonances at 173 K indicating that a single C-2 symmetric bent-metallocene conformation is observed. Upon activation with methylaluminoxane, 3 polymerizes ethylene with an activity of 500 kg PE/mol Zr/h (T-p = 80 degrees C; P(C2H4) = 1.6 bar; [Al]:[Zr] = 3000:1; M-w = 43000; M-w/M-n = 2.2; T-m = 133 degrees C). (C) 1998 Elsevier Science S.A. All rights reserved.
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