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Title: Synthesis of hydride and alkyl compounds containing the Cp*Os({eta}{sup 3}-allyl) fragment. Crystal structures of Cp*Os({eta}{sup 3}-C{sub 8}H{sub 13})Br{sub 2} and [Cp*Os({eta}{sup 3}-C{sub 4}H{sub 7})Me(H{sub 2}O)][BF{sub 4}]

Abstract

Treatment of Cp*{sub 2}Os{sub 2}Br{sub 4} with 3-bromo-2-methylpropene or 1,3-cyclooctadiene affords the 2-methylpropenyl and cyclooctenyl products Cp*Os({eta}{sup 3}-C{sub 4}H{sub 7})Br{sub 2} and Cp*Os({eta}{sup 3}-C{sub 8}H{sub 13})Br{sub 2}, respectively. The monoalkyl complexes Cp*Os({eta}{sup 3}-C{sub 4}H{sub 7})MeBr and Cp*Os({eta}{sup 3}-C{sub 4}H{sub 7})(CH{sub 2}SiMe{sub 3})-Br can be generated by treating Cp*Os({eta}{sup 3}-C{sub 4}H{sub 7})Br{sub 2} with MgMe{sub 2} or LiCH{sub 2}SiMe{sub 3}. The dimethyl complex Cp*Os({eta}{sup 3}-C{sub 4}H{sub 7})Me{sub 2} can be synthesized from Cp*Os({eta}{sup 3}-C{sub 4}H{sub 7})Br{sub 2} by addition of methyllithium. In contrast, addition of ethyllithium to Cp*Os({eta}{sup 3}-C{sub 4}H{sub 7})Br{sub 2} yields the ethylene complex Cp*Os({eta}{sup 3}-C{sub 4}H{sub 7})({eta}{sup 2}-C{sub 2}H{sub 4}) and a small amount of Cp*Os({eta}{sup 3}-C{sub 4}H{sub 7})H{sub 2}. The latter dihydride can be synthesized in better yield by treating Cp*Os({eta}{sup 3}-C{sub 4}H{sub 7})Br{sub 2} with LiAlH{sub 4}. When the dimethyl complex Cp*Os({eta}{sup 3}-C{sub 4}H{sub 7})Me{sub 2} is protonated with HBF{sub 4} in the presence of H{sub 2}O the aqua complex [Cp*Os({eta}{sup 3}-C{sub 4}H{sub 7})Me(H{sub 2}O)][BF{sub 4}] is formed.

Authors:
; ; ;  [1]
  1. Univ. of Illinois, Urbana, IL (United States). School of Chemical Sciences
Publication Date:
Sponsoring Org.:
USDOE, Washington, DC (United States)
OSTI Identifier:
696629
Resource Type:
Journal Article
Journal Name:
Organometallics
Additional Journal Information:
Journal Volume: 18; Journal Issue: 17; Other Information: PBD: 16 Aug 1999
Country of Publication:
United States
Language:
English
Subject:
40 CHEMISTRY; OSMIUM COMPLEXES; FLUOROBORATES; BROMIDES; CHEMICAL PREPARATION; CRYSTAL STRUCTURE; HYDRIDES

Citation Formats

Mui, H.D., Brumaghim, J.L., Gross, C.L., and Girolami, G.S. Synthesis of hydride and alkyl compounds containing the Cp*Os({eta}{sup 3}-allyl) fragment. Crystal structures of Cp*Os({eta}{sup 3}-C{sub 8}H{sub 13})Br{sub 2} and [Cp*Os({eta}{sup 3}-C{sub 4}H{sub 7})Me(H{sub 2}O)][BF{sub 4}]. United States: N. p., 1999. Web. doi:10.1021/om990150m.
Mui, H.D., Brumaghim, J.L., Gross, C.L., & Girolami, G.S. Synthesis of hydride and alkyl compounds containing the Cp*Os({eta}{sup 3}-allyl) fragment. Crystal structures of Cp*Os({eta}{sup 3}-C{sub 8}H{sub 13})Br{sub 2} and [Cp*Os({eta}{sup 3}-C{sub 4}H{sub 7})Me(H{sub 2}O)][BF{sub 4}]. United States. doi:10.1021/om990150m.
Mui, H.D., Brumaghim, J.L., Gross, C.L., and Girolami, G.S. Mon . "Synthesis of hydride and alkyl compounds containing the Cp*Os({eta}{sup 3}-allyl) fragment. Crystal structures of Cp*Os({eta}{sup 3}-C{sub 8}H{sub 13})Br{sub 2} and [Cp*Os({eta}{sup 3}-C{sub 4}H{sub 7})Me(H{sub 2}O)][BF{sub 4}]". United States. doi:10.1021/om990150m.
@article{osti_696629,
title = {Synthesis of hydride and alkyl compounds containing the Cp*Os({eta}{sup 3}-allyl) fragment. Crystal structures of Cp*Os({eta}{sup 3}-C{sub 8}H{sub 13})Br{sub 2} and [Cp*Os({eta}{sup 3}-C{sub 4}H{sub 7})Me(H{sub 2}O)][BF{sub 4}]},
author = {Mui, H.D. and Brumaghim, J.L. and Gross, C.L. and Girolami, G.S.},
abstractNote = {Treatment of Cp*{sub 2}Os{sub 2}Br{sub 4} with 3-bromo-2-methylpropene or 1,3-cyclooctadiene affords the 2-methylpropenyl and cyclooctenyl products Cp*Os({eta}{sup 3}-C{sub 4}H{sub 7})Br{sub 2} and Cp*Os({eta}{sup 3}-C{sub 8}H{sub 13})Br{sub 2}, respectively. The monoalkyl complexes Cp*Os({eta}{sup 3}-C{sub 4}H{sub 7})MeBr and Cp*Os({eta}{sup 3}-C{sub 4}H{sub 7})(CH{sub 2}SiMe{sub 3})-Br can be generated by treating Cp*Os({eta}{sup 3}-C{sub 4}H{sub 7})Br{sub 2} with MgMe{sub 2} or LiCH{sub 2}SiMe{sub 3}. The dimethyl complex Cp*Os({eta}{sup 3}-C{sub 4}H{sub 7})Me{sub 2} can be synthesized from Cp*Os({eta}{sup 3}-C{sub 4}H{sub 7})Br{sub 2} by addition of methyllithium. In contrast, addition of ethyllithium to Cp*Os({eta}{sup 3}-C{sub 4}H{sub 7})Br{sub 2} yields the ethylene complex Cp*Os({eta}{sup 3}-C{sub 4}H{sub 7})({eta}{sup 2}-C{sub 2}H{sub 4}) and a small amount of Cp*Os({eta}{sup 3}-C{sub 4}H{sub 7})H{sub 2}. The latter dihydride can be synthesized in better yield by treating Cp*Os({eta}{sup 3}-C{sub 4}H{sub 7})Br{sub 2} with LiAlH{sub 4}. When the dimethyl complex Cp*Os({eta}{sup 3}-C{sub 4}H{sub 7})Me{sub 2} is protonated with HBF{sub 4} in the presence of H{sub 2}O the aqua complex [Cp*Os({eta}{sup 3}-C{sub 4}H{sub 7})Me(H{sub 2}O)][BF{sub 4}] is formed.},
doi = {10.1021/om990150m},
journal = {Organometallics},
number = 17,
volume = 18,
place = {United States},
year = {1999},
month = {8}
}