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  • 1
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Polymeric Thiolato Complexes [M(SPh)3]∞ of the Metals Mo, W, Fe, and Ru with Linear Metal Chains. Synthesis and Crystal Structure of (OC)3Fe(SPh)3Fe(SPh)3Fe(CO)3 · 2(CH3)2COAt high temperature the reaction of the metal carbonyls Mo(CO)6, W(CO)6 and Fe(CO)5 with S2Ph2 (Ph = C6H5) yields the polymeric complexes [M(SPh)3]∞. Similarly [Ru(SPh)3]∞ can be obtained from ruthenium(III) acetylacetonate and HSPh. At room temperature under UV-irradiation Fe(CO)5 reacts with S2Ph2 to form the oligomeric complex (OC)3Fe(SPh)3Fe(SPh)3Fe(CO)3.The polymeric complexes [M(SPh)3]∞ (M = Mo, W, Fe, Ru) are composed of linear chains with bridging SPh-ligands between the metal atoms. Of these complexes [Fe(SPh)3]∞ is paramagnetic, whereas the others exhibit antiferromagnetic behaviour. The spin coupling is presumably connected with the formation of metal pairs, resulting in alternating shortened and extended distances in the metal chain. The oligomeric complex (OC)3Fe(SPh)3Fe(SPh)3Fe(CO)3 crystallizes triclinic in the space group P1 with z = 2. It has almost the symmetry D3d with a linear arrangement of the Fe atoms. The paramagnetism of Fe3(CO)6(SPh)6 can be explained by a d6 high spin configuration of the central atom and low spin behaviour of the two other Fe atoms, which are bonded to CO.
    Notes: Bei höherer Temperatur reagieren die Metallcarbonyle Mo(CO)6, W(CO)6 und Fe(CO)5 mit S2Ph2 (Ph = C6H5) unter Bildung der polymeren Komplexe [M(SPh)3]∞. Aufähnliche Weise kann [Ru(SPh)3]∞ aus Ruthenium (III)-acetylacetonat und HSPh erhalten werden. Bei Raumtemperatur unter UV-Bestrahlung führt die Reaktion von Fe(CO)5 mit S2Ph2 zum oligomeren Komplex (OC)3Fe(SPh)3Fe(SPh)3Fe(CO)3. Die polymeren Komplexe [M(SPh)3]∞ bestehen aus linearen Ketten, in denen die Metallatome durch SPh-Brücken verknüpft sind. [Fe(SPh)3]∞ ist paramagnetisch mit μ = 5,2 B.M., während die Komplexe des Mo, W und Ru antiferromagnetisches Verhalten zeigen. Die Spinkopplung ist vermutlich mit der Ausbildung von Metallpaaren verbunden, die alternierend lange Abstände in der Metallkette bewirken. Der oligomere Komplex (OC)3Fe(SPh)3Fe(SPh)3Fe(CO)3 kristallisiert triklin in der Raumgruppe P1 mit z = 2. Er hat nahezu die Symmetrie D3d, wobei die Fe-Atome eine lineare Anordnung bilden. Der Paramagnetismus von Fe3(CO)6(SPh)6 (μ = 6,15 B.M.) kann mit einer d6 high spin Konfiguration des Zentralatoms und low spin Verhalten der endständigen Fe-Atome erklärt werden.
    Additional Material: 21 Ill.
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  • 2
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Contributions to the Chemistry of Boron, CII. Synthesis and Reactions of 1-Stanna-4-bora-2,5-cyclohexadienesHydrostannation of (dialkylamino)dialkinylboranes 1 with dimethylstannane yields 1,1-dimethyl-1-stanna-4-bora-2,5-cyclohexadienes 2. Additional 4-amino derivatives are accessible via trans-amination reactions. Solvolysis of the amino derivatives by alcohols leads to alkoxy derivatives 3. These are alkylated by aluminium alkyls or tert-butyllithium to 4-alkyl-1,1-dimethyl-1-stanna-4-boracyclohexadienes 5. A considerable difference in the chemical behaviour of the 1,1-dimethyl-and the 1,1,2,6-tetramethyl derivatives has been observed.
    Notes: Die Hydrostannierung von (Dialkylamino)dialkinylboranen 1 mit Dimethylstannan führt zu 1,1-Dimethyl-1-stanna-4-bora-2,5-cyclohexadienen 2. Über Transaminierung sind weitere 4-Amino-Derivate zugänglich. Die Solvolyse der Amino-Derivate mit Alkoholen liefert die Alkoxyderivate 3, die mit Aluminiumalkylen bzw. mit tert-Butyllithium zu 4-Alkyl-1,1-dimethyl-1-stanna-4-boracyclohexadienen 5 alkyliert werden. Zwischen den 1,1-Dimethyl- und den 1,1,2,6-Tetramethyl-Derivaten bestehen beträchtliche Unterschiede im chemischen Verhalten.
    Type of Medium: Electronic Resource
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  • 3
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Oxepins, VI1). Dehydration Products of 2,5-Cyclohexadiene-1,4-diols; the Crystal Structure of 3,7-Di-tert-butyl-5-phenyl-2-(p-tolyl)oxepinX-ray analysis of the product of dehydration of 2,6-di-tert-butyl-4-phenyl-1-(p-tolyl)-2,5-cyclohexadiene-1,4-diol (4a) proves the structure as 3,7-di-tert-butyl-5-phenyl-2-(p-tolyl)oxepin (1a), in agreement with former IR, 1H NMR and 13C NMR spectroscopic results. The double and single bond distances show a certain degree of equalization.
    Additional Material: 2 Tab.
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