7783-86-0Relevant articles and documents
The use of trimethylsilyl iodide as a synthon in coordination chemistry
Leigh,Sanders,Hitchcock, Peter B.,Fernandes, Jaisa Soares,Togrou, Maria
, p. 197 - 212 (2002)
Trimethylsilyl iodide is shown to be an efficient metathetical reagent for preparing transition-metal iodides from the corresponding chlorides, though often complications can cause problems. These include reduction of the starting metal chloride when its oxidation state is high, due to the reaction of iodide, and even oxidation of low-oxidation-state compounds, presumably by incipient silyl cations. Finally, some very inert chlorides, such as of iridium(III), react too slowly with the iodide under the experimental conditions, and simple reaction with solvent becomes predominant.
New high-spin iron complexes based on bis(imino)acenaphthenes (BIAN): Synthesis, structure, and magnetic properties
Fedushkin,Skatova,Khvoinova,Lukoyanov,Fukin,Ketkov,Maslov,Bogomyakov,Makarov
, (2013)
The reactions of iron diiodide with one and two equivalents of the monopotassium salt of 1,2-bis[(2,6-diisopropylphenyl)imino]acenaphthene (dpp-BIAN) in diethyl ether gave the com-plexes [(dpp-BIAN)FeI]2 (1) and (dpp-BIAN)2Fe (2), re
Insights into the naphthalenide-driven synthesis and reactivity of zerovalent iron nanoparticles
Donsbach, Carsten,Feldmann, Claus,Rei?, Andreas
, p. 16343 - 16352 (2021/11/27)
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 FeCl3 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 ([FeI2(MeOH)2], ([MePPh3][FeI3(Ph3P)])4·PPh3·6C7H8, [FeI2(PPh3)2], and [FeI2(18-crown-6)]). Accordingly, reactive Fe(0) nanoparticles can be obtained in the liquid phase via [LiNaph]-driven reduction and instantaneously reacted to give new compounds without remains of the initial reduction (e.g. LiCl, naphthalene, and THF). This journal is
Room-temperature synthesis, hydrothermal recrystallization, and properties of metastable stoichiometric FeSe
Nitsche,Goltz,Klauss,Isaeva,Mueller,Schnelle,Simon,Doert, Th.,Ruck
, p. 7370 - 7376 (2012/07/28)
Room-temperature precipitation from aqueous solutions yields the hitherto unknown metastable stoichiometric iron selenide (ms-FeSe) with tetragonal anti-PbO type structure. Samples with improved crystallinity are obtained by diffusion-controlled precipitation or hydrothermal recrystallization. The relations of ms-FeSe to superconducting η-FeSe1-x and other neighbor phases of the iron-selenium system are established by high-temperature X-ray diffraction, DSC/TG/MS (differential scanning calorimetry/ thermogravimetry/mass spectroscopy), 57Fe Moessbauer spectroscopy, magnetization measurements, and transmission electron microscopy. Above 300 °C, ms-FeSe decomposes irreversibly to η-FeSe1-x and Fe7Se8. The structural parameters of ms-FeSe (P4/nmm, a = 377.90(1) pm, c = 551.11(3) pm, Z = 2), obtained by Rietveld refinement, differ significantly from literature data for η-FeSe1-x. The Moessbauer spectrum rules out interstitial iron atoms or additional phases. Magnetization data suggest canted antiferromagnetism below TN = 50 K. Stoichiometric non-superconducting ms-FeSe can be regarded as the true parent compound for the 11 iron-chalcogenide superconductors and may serve as starting point for new chemical modifications.