Methyl-Substituted Zirconocene−Bis(trimethylsilyl)acetylene Complexes (C5H5 - n Me n )2Zr(η2-Me3SiC⋮CSiMe3) (n = 2−5)

The (C5H5 - n Me n )2Zr[η2-C2(SiMe3)2] (n = 2−5; 1,3-dimethyl, 1,2,3-trimethyl) (2C−F) complexes were prepared by the reduction of corresponding zirconocene dichlorides with magnesium in THF in the presence of bis(trimethylsilyl)acetylene (BTMSA). All of them are stable in the absence of THF. Crysta...

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Published in:Organometallics 1996-08, Vol.15 (17), p.3752-3759
Main Authors: Hiller, Jörg, Thewalt, Ulf, Polášek, Miroslav, Petrusová, Lidmila, Varga, Vojtech, Sedmera, Petr, Mach, Karel
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container_issue 17
container_start_page 3752
container_title Organometallics
container_volume 15
creator Hiller, Jörg
Thewalt, Ulf
Polášek, Miroslav
Petrusová, Lidmila
Varga, Vojtech
Sedmera, Petr
Mach, Karel
description The (C5H5 - n Me n )2Zr[η2-C2(SiMe3)2] (n = 2−5; 1,3-dimethyl, 1,2,3-trimethyl) (2C−F) complexes were prepared by the reduction of corresponding zirconocene dichlorides with magnesium in THF in the presence of bis(trimethylsilyl)acetylene (BTMSA). All of them are stable in the absence of THF. Crystal structures of (C5HMe4)2Zr[η2-C2(SiMe3)2] (2E) and (C5Me5)2Zr[η2-C2(SiMe3)2] (2F) and of the analogous titanium complexes are isomorphous. The red shift of the ν(C⋮C) vibration and the downfield shift of 13C δ(C⋮C) indicate that BTMSA in 2C−F is more strongly coordinated than in analogous titanocene complexes. The nonisolated complex (C5H4Me)2Zr[η2-C2(SiMe3)2](THF) (2 B·THF) rearranges after the loss of THF to give the dimer [(η5-C5H4Me)(η1-C(SiMe3)CH(SiMe3)Zr(μ-η1:η5-C5H3Me)]2 (3B).
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All of them are stable in the absence of THF. Crystal structures of (C5HMe4)2Zr[η2-C2(SiMe3)2] (2E) and (C5Me5)2Zr[η2-C2(SiMe3)2] (2F) and of the analogous titanium complexes are isomorphous. The red shift of the ν(C⋮C) vibration and the downfield shift of 13C δ(C⋮C) indicate that BTMSA in 2C−F is more strongly coordinated than in analogous titanocene complexes. The nonisolated complex (C5H4Me)2Zr[η2-C2(SiMe3)2](THF) (2 B·THF) rearranges after the loss of THF to give the dimer [(η5-C5H4Me)(η1-C(SiMe3)CH(SiMe3)Zr(μ-η1:η5-C5H3Me)]2 (3B).</description><identifier>ISSN: 0276-7333</identifier><identifier>EISSN: 1520-6041</identifier><identifier>DOI: 10.1021/om960184j</identifier><language>eng</language><publisher>American Chemical Society</publisher><ispartof>Organometallics, 1996-08, Vol.15 (17), p.3752-3759</ispartof><rights>Copyright © 1996 American Chemical Society</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><link.rule.ids>314,776,780,27903,27904</link.rule.ids></links><search><creatorcontrib>Hiller, Jörg</creatorcontrib><creatorcontrib>Thewalt, Ulf</creatorcontrib><creatorcontrib>Polášek, Miroslav</creatorcontrib><creatorcontrib>Petrusová, Lidmila</creatorcontrib><creatorcontrib>Varga, Vojtech</creatorcontrib><creatorcontrib>Sedmera, Petr</creatorcontrib><creatorcontrib>Mach, Karel</creatorcontrib><title>Methyl-Substituted Zirconocene−Bis(trimethylsilyl)acetylene Complexes (C5H5 - n Me n )2Zr(η2-Me3SiC⋮CSiMe3) (n = 2−5)</title><title>Organometallics</title><addtitle>Organometallics</addtitle><description>The (C5H5 - n Me n )2Zr[η2-C2(SiMe3)2] (n = 2−5; 1,3-dimethyl, 1,2,3-trimethyl) (2C−F) complexes were prepared by the reduction of corresponding zirconocene dichlorides with magnesium in THF in the presence of bis(trimethylsilyl)acetylene (BTMSA). 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All of them are stable in the absence of THF. Crystal structures of (C5HMe4)2Zr[η2-C2(SiMe3)2] (2E) and (C5Me5)2Zr[η2-C2(SiMe3)2] (2F) and of the analogous titanium complexes are isomorphous. The red shift of the ν(C⋮C) vibration and the downfield shift of 13C δ(C⋮C) indicate that BTMSA in 2C−F is more strongly coordinated than in analogous titanocene complexes. The nonisolated complex (C5H4Me)2Zr[η2-C2(SiMe3)2](THF) (2 B·THF) rearranges after the loss of THF to give the dimer [(η5-C5H4Me)(η1-C(SiMe3)CH(SiMe3)Zr(μ-η1:η5-C5H3Me)]2 (3B).</abstract><pub>American Chemical Society</pub><doi>10.1021/om960184j</doi><tpages>8</tpages></addata></record>
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title Methyl-Substituted Zirconocene−Bis(trimethylsilyl)acetylene Complexes (C5H5 - n Me n )2Zr(η2-Me3SiC⋮CSiMe3) (n = 2−5)
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