| Synthesis and Reactivity of Boron-, Silicon-, and Tin-Bridged ansa-Cyclopentadienyl-Cycloheptatrienyl Titanium Complexes (Troticenophanes). | |
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MedLine Citation:
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PMID: 20803585 Owner: NLM Status: In-Data-Review |
Abstract/OtherAbstract:
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A novel one-pot method was developed for the preparation of [Ti(η(5) -C(5) H(5) )(η(7) -C(7) H(7) )] (troticene, 1) by reaction of sodium cyclopentadienide (NaCp) with [TiCl(4) (thf)(2) ], followed by reduction of the intermediate [(η(5) -C(5) H(5) )(2) TiCl(2) ] with magnesium in the presence of cycloheptatriene (C(7) H(8) ). The [n]troticenophanes 3 (n=1), 4, 8, 10 (n=2), and 11 (n=3) were synthesized by salt elimination reactions between dilithiated troticene, [Ti(η(5) -C(5) H(4) Li)(η(7) -C(7) H(6) Li)]⋅pmdta (2) (pmdta=N,N',N',N'',N''-pentamethyldiethylenetriamine), and the appropriate organoelement dichlorides Cl(2) Sn(Mes)(2) (Mes=2,4,6-trimethylphenyl), Cl(2) Sn(2) (tBu)(4) , Cl(2) B(2) (NMe(2) )(2) , Cl(2) Si(2) Me(4) , and (ClSiMe(2) )(2) CH(2) , respectively. Their structural characterization was carried out by single-crystal X-ray diffraction and multinuclear NMR spectroscopy. The stanna[1]- and stanna[2]troticenophanes 3 and 4 represent the first heteroleptic sandwich complexes bearing Sn atoms in the ansa bridge. The reaction of 3 with [Pt(PEt(3) )(3) ] resulted in regioselective insertion of the [Pt(PEt(3) )(2) ] fragment into the SnC(ipso) bond between the tin atom and the seven-membered ring, which afforded the platinastanna[2]troticenophane 5. Oxidative addition was also observed upon treatment of 4 with elemental sulfur or selenium, to produce the [3]troticenophanes [Ti(η(5) -C(5) H(4) SntBu(2) )(η(7) -C(7) H(6) SntBu(2) )E] (6: E=S; 7: E=Se). The BB bond of the bora[2]troticenophane 8 was readily cleaved by reaction with [Pt(PEt(3) )(3) ] to form the corresponding oxidative addition product [Ti(η(5) -C(5) H(4) BNMe(2) )(η(7) -C(7) H(6) BNMe(2) )Pt(PEt(3) )(2) ] (9). The solid-state structures of compounds 5, 6, and 9 were also determined by single-crystal X-ray diffraction. |
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Authors:
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Holger Braunschweig; Marco Fuß; Swagat K Mohapatra; Katharina Kraft; Thomas Kupfer; Melanie Lang; Krzysztof Radacki; Constantin G Daniliuc; Peter G Jones; Matthias Tamm |
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Publication Detail:
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Type: Journal Article Date: 2010-08-27 |
Journal Detail:
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Title: Chemistry (Weinheim an der Bergstrasse, Germany) Volume: 16 ISSN: 1521-3765 ISO Abbreviation: Chemistry Publication Date: 2010 Oct |
Date Detail:
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Created Date: 2012-10-05 Completed Date: - Revised Date: - |
Medline Journal Info:
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Nlm Unique ID: 9513783 Medline TA: Chemistry Country: Germany |
Other Details:
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Languages: eng Pagination: 11732-43 Citation Subset: IM |
Copyright Information:
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Copyright © 2010 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim. |
Affiliation:
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Institut für Anorganische Chemie, Julius Maximilians-Universität Würzburg, Am Hubland, 97074 Würzburg (Germany), Fax: (+49) 931-31-84623. h.braunschweig@mail.uni-wuerzburg.de. |
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From MEDLINE®/PubMed®, a database of the U.S. National Library of Medicine
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