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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: The Chemistry of Metal Carbonyls and Cyano Complexes in Liquid Ammonia. XXXII. On the Reaction of η5-C5H5Mo(CO)3CH3 and η5-C5H5Fe(CO)2CH3 with Liquid Ammoniaη5-C5H5Mo(CO)3CH3 reacts with liquid NH3 to give η5-C5H5Mo(CO)2(NH3)H and acetamide:In contrast, η5-C5H5Fe(CO)2CH3 undergoes a carbonyl insertion to give the acetyl complex η5-C5H5Fe(CO)(NH3)COCH3:The NH3 ligand in η5-C5H5Fe(CO)(NH3)COCH3 can be substituted by pyridine.
    Notes: Während sich η5-C5H5Mo(CO)3CH3 mit flüssigem NH3 gemäß, , zu η5-C5H5Mo(CO)2(NH3)H und Acetamid umsetzt, entsteht mit η5-C5H5Fe(CO)2CH3 im Sinne einer CO-Insertierungsreaktion der Acetylkomplex η5-C5H5Fe(CO)(NH3)COCH3:Im Hydridokomplex η5-C5H5Mo(CO)2(NH3)H läßt sich der NH3-Ligand durch py substituieren.
    Additional Material: 3 Tab.
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  • 2
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Chemistry of Metal Carbonyls and Cyano Complexes in Liquid Ammonia. XXXI. On the Reactions of Cationic η5-Cyclopentadienyl-molybdenumcarbonyl Complexes with Liquid AmmoniaDepending on the reaction conditions, the cationic complexes [η5-C5H5Mo(CO)3L]+ (L = NH3, PPh3, CO) react with liquid ammonia according to:The characteristics and reactivities of the new carbomoyl derivatives are described.
    Notes: Die Umsetzungen der Kationkomplexe [η5-C5H5Mo(CO)3L]+ (L = NH3, PPh3, CO) mit flüssigem NH3 verlaufen je nach Reaktionsbedingungen gemäß:Eigenschaften und Reaktionsweisen der neuen Carbamoylderivate werden beschrieben.
    Additional Material: 1 Ill.
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  • 3
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: About Chemistry and Structure of Olefin-monocyano-dicarbonyl-ferrate AnionsBy the reactions of olenFe(CO)3 [olen = C5H8(isoprene), C7H10(cycloheptadiene-1,3), C8H14(2,5-dimethylhexadiene-1,3)] with sodium bis [trimethylsilyl]amide the new anions [olenFe(CO)2CN]- are formed. All so far known [olenFe(CO)2CN]- complexes [olen = C5H8(isoprene), C7H10[cycloheptadiene-1,3], C4H6(butadiene), C5H8(pentadiene-1,3), C6H8(cyclohexadine-1,3), C6H10(2,3-dimethylbutadiene), C8H8(cyclooctatetraene)] have fluctional structures in solution as shown by 13C NMR spectroscopic investigations. At low temperatures only the isomer exists, in which the CN- ligand and one of the two CO molecules occuppy the basal positions of a square pyramide together with 2 C atoms of the diene part.
    Notes: Bei der Umsetzung von olenFe(CO)3 [olen = C5H8(Isopren), C7H10(Cycloheptadien-1,3), C8H14(2,5-Dimethylhexadien-1,3)] mit Natrium-bis[trimethylsily]-amid werden die neuen Anionen [olenFe(CO)2CN]- gebildet. 13C-NMR-spektroskopische Untersuchungen an sämtlichen bisher bekannten [olenFe(CO)2CN]--Komplexen [olen = C5H8(Isopren), C7H10(Cycloheptadien-1,3), C4H6(Butadien), C5H8(Pentadien-1,3), C6H8(Cyclohexadien-1,3), C6H10(2,3-Dimethylbutadien), C8H8(Cyclooctatetraen)] zeigen, daß diese Anionen in Lösung fluktuierende Strukturen besitzen. Erst bei tiefen Temperaturen tritt jeweils das Isomere auf, bei dem der CN--Ligand und eines der beiden CO-Moleküle in einer quadratischen Pyramide neben 2 C-Atomen des Dienteiles die beiden übrigen basalen Positionen besetzen.
    Additional Material: 3 Ill.
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  • 4
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Chemistry of Polyfunctional Molecules. 93. Halogenating Ring Cleavage of As3-Nortricyclane 4-Methyl-1,2,6-triarsatricyclo[2.2.1.02,6]heptane. Preparation and Properties of 2,6-Dihalogeno-4-methyl-1,2,6-triarsabicyclo[2.2.1]heptanesThe reaction of the As3-nortricyclane CH3C(CH2As)3 (1) with PCl5, Br2, or I2 in a molar ratio of 1:1 leads to the new 2,6-dihalogeno-4-methyl-1,2,6-triarsabicyclo[2.2.1]heptanes CH3C(CH2As)3X2 (X = Cl, Br, I; 2a-c). Application of a molar ratio of 1:2 results in the formation of 1,1,1-tris(dihalogenoarsinomethyl)ethanes CH3C(CH2AsX2)3 (4a-c) in rather poor yields; 1H-NMR spectroscopic studies suggest that 4a-c are formed via 2a-c and the tetrahalogenodiarsacyclopentane derivatives (3a-c); the latter can not be isolated from their solutions. 4a-c are obtained in very good yields by treatment of 1 with the halogenating agents in a molar ratio of 1:3 Comproportionation of 1 with 4a-c (molar ratio of 2:1) gives also 2a-c. Whereas in CD2Cl2 or CS2 disproportionation of 2a leads to an equilibrium between 1 and 4a, which is formed via the intermediate 3a. The homologues 2b, c are stable with respect to disproportionation in both solvents.
    Notes: Das As3-Nortricyclan CH3C(CH2As)3 (1) reagiert mit PCl5, Br2 oder I2 (Molverhältnis jeweils 1:1) zu den neuen 2,6-Dihalogen-4-methyl-1,2,6-triarsabicyclo[2.2.1]heptanen CH3C(CH2As)3X2 (X = Cl, Br, I; 2a-c). Bei Anwendung eines Molverhältnisses von 1:2 erhält man, über die 1H-NMR-spektroskopisch nachweisbaren, aber nicht isolierbaren Tetrahalogendiarsacyclopentan-Derivate (3a-c), bereits die 1,1,1-Tris(dihalogenarsinomethyl)ethane CH3C(CH2AsX2)3 (4a-c) in mäßigen Ausbeuten. Letztere sind in sehr guten Ausbeuten zugänglich, wenn man 1 und Halogenierungsmittel im Molverhältnis 1:3 umsetzt. 2a-c sind auch durch Synproportionierung von 1 mit 4a-c (Molverhältnis 2:1) darstellbar. Während 2a in CD2Cl2 oder CS2 wiederum in 1 und 4a disproportioniert, und sich hierbei über das Zwischenprodukt 3a ein Gleichgewicht einstellt, sind 2b, c in diesen Lösungsmitteln stabil.
    Additional Material: 4 Ill.
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  • 5
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: About New Cyanocarbonyl Metallates of Chromium and IronCr(CO)5L (L = pyridine, cyclohexylisonitrile) and (olen)Fe(CO)3 (olen = buta diene C4H6, 1,3-cyclohexadiene C6H8, cyclooctatetraene C8H8) react with sodium-bis[trimethylsilyl]-amide to give cyano-carbonylmetallates Na[Cr(CO)4(CN)L] and Na[(olen)Fe(CO)2CN] respectively. Structures based on I.R. and 1H-NMR results are discussed.
    Notes: Cr(CO)5L (L = Pyridin, Cyclohexylisonitril) und (olen)Fe(CO)3 (olen = Butadien C4H6, 1,3-Cyclohexadien C6H8, Cyclooctatetraen C8H8) reagieren mit Natrium-bis[tri-methylsilyl]-amid zu den Cyano-carbonylmetallaten Na[Cr(CO)4(CN)L] bzw. Na[(olen)Fe(CO)2CN], deren Strukturen anhand ihrer IR- und 1H-NMR-Spektren diskutiert werden.
    Additional Material: 6 Tab.
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  • 6
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Characterization of New Chloro Bis(carbonylmetallato) Tin(IV) CompoundsThe trichloro(carbonylmetallato) tin(IV) compounds Cl3SnMn(CO)4L (L = CO, PEt2Ph) and Cl3SnFe(CO)2Cp (Cp = η5-C5H5) react with the thallium(I) carbonylmetallates TlCo(CO)4, and TlCr(CO)3Cp (molar ratio of 1:1) to yield the new dichloro bis(carbonylmetallato)-tin(IV) complexes listed in Table 1. Their mass-, IR-, and FIR-spectra are discussed.
    Notes: Bei der Umsetzung der Trichloro-(carbonylmetallato)-zinn(IV)-Verbindungen Cl3SnMn(CO)4L (L = CO, PEt2Ph) und Cl3SnFe(CO)2Cp (Cp = η5-C5H5) mit den Thallium(I)-carrbonylmetallaten TlCo(CO)4 und TlCr(CO)3Cp im Molverhältnis 1:1 entstehen in gezielter Synthese die in Tab. 1 aufgeführten Bis(carbonylmetallato)-zinn(IV)-Komplexe, deren Massen-, IR- und IR-Spektren diskutiert werden.
    Additional Material: 2 Ill.
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  • 7
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: About the Reactivity of Na [Mn2(CO)9CN]The reactions of Na[Mn2(CO)9CN] with Et3OBF4, Me3SiCl, Me3GeCl, Me3SnCl, PPh2Cl, or MeCOCl lead to the dinuclear monoisonitrile complexes Mn2(CO)9CNR (R = Et, SiMe3, GeMe3, SnMe3, PPh2, COMe) which are characterized by their mass, vibrational, and n.m.r. spectra. However the solvates Na[Mn2(CO)9CN] · CH3COCH2Cl and Na[Mn2(CO)9CN] · NCCH2Cl are formed with CH3COCH2Cl and NCCH2Cl. Similar adducts are obtained with the Lewis bases CH3COCH3, NCCH3, and O(C2H5)2.
    Notes: Bei den Reaktionen von Na[Mn2(CO)9CN] mit Et3OBF4, Me3SiCl, Me3GeCl, Me3SnCl, PPh2Cl bzw. MeCOCl, werden die zweikernigen Monoisonitril-Komplexe Mn2(CO)9CNR (R = Et, SiMe3, GeMe3, SnMe3, PPh2, COMe) gebildet, die anhand ihrer Massen-, Schwingungs- und NMR-Spektren charakterisiert werden. Dagegen führen die entsprechenden Umsetzungen mit CH3COCH2Cl bzw. NCCH2Cl zu den Solvaten Na[Mn2(CO)9CN] · CH3COCH2Cl und Na[Mn2(CO)9CN] · NCCH2Cl. Eine ähnliche Adduktbildung erfolgt auch mit den Lewisbasen CH3COCH3, NCCH3 und O(C2H5)2.
    Additional Material: 3 Ill.
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  • 8
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Properties of New Cationic Dienyl-isonitrile-dicarbonyl Complexes of Iron and RutheniumThe hydride abstraction from the η4-diene isonitrile metal dicarbonyls M(η4-dien)(CNR)(CO)2 (M = Fe, Ru; dien = C6H8 cyclohexadiene-1.3; C7H10 cycloheptadiene-1.3; R = Me, Et) with [Ph3C]BF4 lead to the η5-dienyl isonitrile dicarbonyl metal cations [M(η5-dienyl)(CNR)(CO)2]+ [dienyl = cyclohexa-2.4-dien-1-yl (C6H7), cyclohepta-2.4-dien-1-yl (C7H9)]. [Fe(η5—C8H9)(CNMe)(CO)2]+ (C8H9 = bicyclo[5.1.0]octa-3.5-dien-2-yl) is formed by protonation of Fe(η4—C8H8)(CNMe)(CO)2 (C8H8 = COT) under valency isomerization. The two cations [Fe(η5—C7H9)(CNMe)(CO)2]+ and [Fe(η5—C8H9)(CNMe)(CO)2]+ can be deprotonated with NEt3 to the neutral cycloheptatriene respectively COT complexes Fe(η4—C7H8)(CNMe)(CO)2 and Fe(η4—C8H8)(CNMe)(CO)2. The temperature dependent 13C-NMR spectra of [Fe(η5—C7H9)(CNMe)(CO)2]+ and [Ru(η5—C6H7)(CNMe)(CO)2]+ show the fluctional behaviour of these cations in solution. At low temperatures one CO group occupies the apical position of a square pyramid whereas the isonitrile ligand, the other CO group and the dienyl part are in the basal positions. The ΔGc≠ values of the CP exchange points out a higher activation energy as in the corresponding η4-diene metal complexes.
    Notes: Die Reaktionen der η4-Dien-isonitril-metall-dicarbonyle M(η4-dien)(CNR)(CO)2 (M = Fe, Ru; dien = C6H8 Cyclohexadien-1.3, C7H10 Cycloheptadien-1.3; R = Me, Et) mit [Ph3C]BF4 führen unter H--Abspaltung zu den η5-Dienyl-isonitril-dicarbonylmetall-Kationen [M(η5-dienyl)(CNR)(CO)2]+ [dienyl = Cyclohexa-2.4-dien-1-yl (C6H7), Cyclohepta-2.4-dien-1-yl (C7H9)]. [Fe(η5—C8H9)(CNMe)(CO)2]+ (C8H9 = Bicyclo[5.1.0]octa-3.5-dien-2-yl) entsteht bei der Protonierung von Fe(η4—C8H8)(CNMe)(CO)2 (C8H8 = COT) mit HBF4 unter Valenzisomerisierung. Durch NEt3 werden die beiden Kationen [Fe(η5—C7H9)(CNMe)(CO)2]+ und [Fe(η5—C8H9)(CNMe)(CO)2]+ zu den neutralen Cycloheptatrien- bzw. COT-Komplexen Fe(η4—C7H8)(CNMe)(CO)2 bzw. zu Fe(η4—C8H8)(CNMe)(CO)2 deprotoniert. Die temperaturabhängigen 13C-NMR-Spektren von [Fe(η5—C7H9)(CNMe)(CO)2]+ und [Ru(η5—C6H7)(CNMe)(CO)2]+ zeigen das fluktuierende Verhalten dieser Kationen in Lösung. Bei tiefen Temperaturen wird dabei in einer quadratischen Pyramide stets diejenige Ligandenanordnung bevorzugt, bei der eine CO-Gruppe die apikale Position, der Isonitrilligand, die andere CO-Gruppe und das Dienyl-System die basalen Positionen besetzen. Die ΔGc≠-Werte des CO-Austausches weisen auf eine höhere Aktivierungsenergie als bei den entsprechenden η4-Dienmetallkomplexen hin.
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