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Article: Ferrocenyl phosphine mobility, positional isomerism and NMR fluxionality in triangular palladium sulfide aggregates. Crystal and molecular structures of [Pd3Cl2(η2-dppf)(μ-dppf)(μ 3-S)2] and [Pd3Cl(η2-dppf)2(PPh3)(μ 3-S)2]X [X = Cl or NO3, dppf = ...

TitleFerrocenyl phosphine mobility, positional isomerism and NMR fluxionality in triangular palladium sulfide aggregates. Crystal and molecular structures of [Pd3Cl2(η2-dppf)(μ-dppf)(μ 3-S)2] and [Pd3Cl(η2-dppf)2(PPh3)(μ 3-S)2]X [X = Cl or NO3, dppf = ...
Authors
Issue Date1999
Citation
Journal of the Chemical Society - Dalton Transactions, 1999, n. 3, p. 435-441 How to Cite?
AbstractTitle full: Ferrocenyl phosphine mobility, positional isomerism and NMR fluxionality in triangular palladium sulfide aggregates. Crystal and molecular structures of [Pd3Cl2(η2-dppf)(μ-dppf)(μ 3-S)2] and [Pd3Cl(η2-dppf)2(PPh3)(μ 3-S)2]X [X = Cl or NO3, dppf = Fe(η5-C5H4PPh2)2]. Three {Pd3S2} aggregates, [Pd3Cl2(η2-dppf)(μ-dppf)(μ 3-S)2] and [Pd3Cl(η2-dppf)2(PPh3)(μ 3-S)2]X [X = Cl or NO3, dppf = 1,1′-bis(diphenylphosphino)ferrocene] have been synthesized from metal addition to a {Pd2S2} molecular core in [Pd2(dppf)2(μ-S)2]. X-Ray single-crystal crystallographic analysis revealed a common sulfide-bicapped triangle with insignificant Pd ⋯ Pd interactions. The former is neutral with a bridging and a chelating dppf ligand as well as two terminal chlorides. The dynamic behaviour has been studied by variable temperature 31P and 2-D COSY NMR. A phosphine-chloride interchange and phosphine-phosphine exchanges enable the two dppf ligands to migrate around the Pd3 plane. The solid-state structure corresponds to the static structure in solution at 198 K. The mixed phosphine complex Sa (X = Cl) is ionic with two Pd-dppf chelating rings and a {Pd(PPh3)Cl} moiety. With a PPh3 group taking up one site, it is stereochemically rigid. The other two complexes were studied by electrospray mass spectrometry (ESMS) in solution. The {Pd3S2} core in the mixed phosphine (X = NO3) is relatively stable to fragmentation under ESMS conditions.
Persistent Identifierhttp://hdl.handle.net/10722/219533
ISSN
1999 Impact Factor: 2.31

 

DC FieldValueLanguage
dc.contributor.authorYeo, Jeremy S L-
dc.contributor.authorLi, Guangming-
dc.contributor.authorYip, Wai Hing-
dc.contributor.authorHenderson, William-
dc.contributor.authorMak, Thomas C W-
dc.contributor.authorHor, T. S Andy-
dc.date.accessioned2015-09-23T02:57:19Z-
dc.date.available2015-09-23T02:57:19Z-
dc.date.issued1999-
dc.identifier.citationJournal of the Chemical Society - Dalton Transactions, 1999, n. 3, p. 435-441-
dc.identifier.issn0300-9246-
dc.identifier.urihttp://hdl.handle.net/10722/219533-
dc.description.abstractTitle full: Ferrocenyl phosphine mobility, positional isomerism and NMR fluxionality in triangular palladium sulfide aggregates. Crystal and molecular structures of [Pd3Cl2(η2-dppf)(μ-dppf)(μ 3-S)2] and [Pd3Cl(η2-dppf)2(PPh3)(μ 3-S)2]X [X = Cl or NO3, dppf = Fe(η5-C5H4PPh2)2]. Three {Pd3S2} aggregates, [Pd3Cl2(η2-dppf)(μ-dppf)(μ 3-S)2] and [Pd3Cl(η2-dppf)2(PPh3)(μ 3-S)2]X [X = Cl or NO3, dppf = 1,1′-bis(diphenylphosphino)ferrocene] have been synthesized from metal addition to a {Pd2S2} molecular core in [Pd2(dppf)2(μ-S)2]. X-Ray single-crystal crystallographic analysis revealed a common sulfide-bicapped triangle with insignificant Pd ⋯ Pd interactions. The former is neutral with a bridging and a chelating dppf ligand as well as two terminal chlorides. The dynamic behaviour has been studied by variable temperature 31P and 2-D COSY NMR. A phosphine-chloride interchange and phosphine-phosphine exchanges enable the two dppf ligands to migrate around the Pd3 plane. The solid-state structure corresponds to the static structure in solution at 198 K. The mixed phosphine complex Sa (X = Cl) is ionic with two Pd-dppf chelating rings and a {Pd(PPh3)Cl} moiety. With a PPh3 group taking up one site, it is stereochemically rigid. The other two complexes were studied by electrospray mass spectrometry (ESMS) in solution. The {Pd3S2} core in the mixed phosphine (X = NO3) is relatively stable to fragmentation under ESMS conditions.-
dc.languageeng-
dc.relation.ispartofJournal of the Chemical Society - Dalton Transactions-
dc.titleFerrocenyl phosphine mobility, positional isomerism and NMR fluxionality in triangular palladium sulfide aggregates. Crystal and molecular structures of [Pd3Cl2(η2-dppf)(μ-dppf)(μ 3-S)2] and [Pd3Cl(η2-dppf)2(PPh3)(μ 3-S)2]X [X = Cl or NO3, dppf = ...-
dc.typeArticle-
dc.description.natureLink_to_subscribed_fulltext-
dc.identifier.scopuseid_2-s2.0-33947543401-
dc.identifier.issue3-
dc.identifier.spage435-
dc.identifier.epage441-

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