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Insights into the naphthalenide-driven synthesis and reactivity of zerovalent iron nanoparticles

Reiß, A.; Donsbach, C.; Feldmann, C.


The chemical and thermal stability of alkali metal naphthalenides as powerful reducing agents are examined, including the type of alkali metal ([LiNaph] and [NaNaph]), the type of solvent (THF, DME), the temperature (−30 to +50 °C), and the time of storage (0 to 12 hours). The stability and concentration of [LiNaph]/[NaNaph] are quantified via UV-Vis spectroscopy and the Lambert–Beer law. As a result, the solutions of [LiNaph] in THF at low temperature turn out to be most stable. The decomposition can be related to a reductive polymerization of the solvent. The most stable [LiNaph] solutions in THF are exemplarily used to prepare reactive zerovalent iron nanoparticles, 2.3 ± 0.3 nm in size, by reduction of FeCl$_{3}$ in THF. Finally, the influence of [LiNaph] and/or remains of the starting materials and solvents upon controlled oxidation of the as-prepared Fe(0) nanoparticles with iodine in the presence of selected ligands is evaluated and results in four novel, single-crystalline iron compounds ([FeI$_{2}$(MeOH)$_{2}$], ([MePPh$_{3}$][FeI$_{3}$(Ph$_{3}$P)])$_{4}$·PPh$_{3}$·6C$_{7}$H$_{8}$, [FeI$_{2}$(PPh$_{3}$)$_{2}$], and [FeI$_{2}$(18-crown-6)]). ... mehr

Verlagsausgabe §
DOI: 10.5445/IR/1000140517
Veröffentlicht am 03.12.2021
DOI: 10.1039/d1dt02523f
Zitationen: 3
Web of Science
Zitationen: 3
Zitationen: 4
Cover der Publikation
Zugehörige Institution(en) am KIT Institut für Anorganische Chemie (AOC)
Publikationstyp Zeitschriftenaufsatz
Publikationsjahr 2021
Sprache Englisch
Identifikator ISSN: 1477-9226, 0300-9246, 1470-479X, 1477-9234, 2050-5671
KITopen-ID: 1000140517
Erschienen in Dalton Transactions
Verlag Royal Society of Chemistry (RSC)
Band 50
Heft 44
Seiten 16343-16352
Vorab online veröffentlicht am 14.10.2021
Nachgewiesen in Dimensions
Web of Science
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