Journal article
New ligand environments for soluble Zieglernatta olefin polymerization catalyst precursors. X-ray structures of
Polyhedron, Vol.14(1), pp.1-10
1995
DOI: 10.1016/0277-5387(94)00321-5
Abstract
Treatment of dimethyl(tetramethylcyclopentadieny)chloro silane with S-(-) pyrolidine methanol provided the O-silylated ligand(C
5Me
4H)SiMe
2OCH
2(C
4H
7NH),
1, (Cp∗SiProH
2) as a 90% pure, thermally unstable oil in 65% yield. Reaction of
1 with Zr(NMe
2)
4 resulted in attachment of
1 to the zirconium center with elimination of HNMe
2, yielding (Cp∗SiPro)Zr(NMe
2)
2,
2, as a viscous oil in high yield (95%). Compound
2 was converted to the trichloride derivative (Cp∗SiProH)ZrCl
3,
3, in 75% yield by treatment with three equivalents of HCl·HNMe
2: compound is a mixture of diastereomers; the major species was characterized by X-ray crystallography, revealing a Cp∗ON coordination mode for the Cp∗SiProH ligand. (
3:
orthorhombic; space group P
2
12
12
1, a = 10.0009(13), b = 12.7597(12), c = 16.2749(15) Å, V=2076.8(4) Å
3, Z = 4,
R = 0.043,
r
w = 0.041.) Deprotonation of
3 (diastereomeric mixture) with LiN(SiMe
3)
2 produced the dichloride (Cp∗SiPro)ZrCl
2,
4, in 71% yield. Alkylation of either
3 or
4 resulted in SiO bond cleavage in the Cp∗SiPro ligand and gave a dimeric complex
5 which was characterized by X-ray crystallograhy. (
5
: monoclinic, space group P2
1,
a = 9.1285(10), b = 20.2197(22), c = 11.0214(14)
A
̊
, β = 90.38(7)°, V = 2034.2(4)
A
̊
3, Z = 2, R = 0.040, R
w
= 0.042
. Limited ethylene polymerization activity was observed for
3 and
4 in the presence of MAO co-catalyst.
Details
- Title: Subtitle
- New ligand environments for soluble Zieglernatta olefin polymerization catalyst precursors. X-ray structures of
- Creators
- Ying MuWarren E PiersLeonard R MacgillivrayMichael J Zaworotko
- Resource Type
- Journal article
- Publication Details
- Polyhedron, Vol.14(1), pp.1-10
- Publisher
- Elsevier Ltd
- DOI
- 10.1016/0277-5387(94)00321-5
- ISSN
- 0277-5387
- Language
- English
- Date published
- 1995
- Academic Unit
- Chemistry; Pharmaceutical Sciences and Experimental Therapeutics
- Record Identifier
- 9984216607502771
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