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  • 1
    Electronic Resource
    Electronic Resource
    Cycloadditionsreaktionen von Organometallkomplexen, I. Die Synthese viergliedriger Metalla-Heterocyclen durch [2 + 2]-Cycloaddition aus (Isonitril)cobalt-Komplexen und Isocyanaten sowie Isothiocyanaten (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 3069-3084 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Cycloaddition Reactions of Organometal Complexes, I. The Synthesis of Four-membered Metalla-Heterocycles by [2 + 2] Cycloaddition of (Isonitrile)-cobalt Complexes and Isocyanates or IsothiocyanatesThe reaction of C5H5(PMe3)CoCNR (R = Me, Ph) with isocyanates OCNR' (R' = Me, Ph) leads to the metalla-heterocycles in nearly quantitative yields. The analogous four-membered ring compounds (4-6) are obtained from C5H5(PMe3)CoCNR (R = Me, Ph, c-C6H11) and SCNMe. In the reactions of C5H5(PMe3)CoCNtBu with SCNMe and of C5H5(PMe3)CoCNMe with SCNtBu the complex (4) is also formed. The X-ray structure analyses of 4 and 5 show the presence of planar four-membered CoCNC rings together with a trigonal-planar coordination of the corresponding C, N and C ring atoms. The protonation and methylation reactions of the metalla-heterocycles 1-5 yield diaminocarbene complexes, in most cases by preserving the four-membered CoCNC-ring. The structure of these complexes is discussed on the basis of their IR and NMR data.
    Notes: Die Reaktion von C5H5(PMe3)CoCNR (R = Me, Ph) mit Isocyanaten OCNR' (R' = Me, Ph) führt nahezu quantitativ zu den Metalla-Heterocyclen (1-3). Die analogen Vierring-Verbindungen (4-6) sind ausgehend von C5H5(PMe3)CoCNR (R = Me, Ph, c-C6H11) und SCNMe zugänglich. Bei den Umsetzungen von C5H5(PMe3)CoCNtBu mit SCNMe und von C5H5(PMe3)CoCNMe mit SCNtBu bildet sich ebenfalls der Komplex (4). Die Röntgenstrukturanalysen von 4 und 5 beweisen das Vorliegen planarer CoCNC-Vierringe mit ebenfalls trigonal-planar koordinierten C-, N- und C-Atomen. Die Protonierungs- und Methylierungsreaktionen der Metalla-Heterocyclen 1-5 ergeben -- in den meisten Fällen unter Erhalt der CoCNC-Vierringstruktur - Diaminocarben-Komplexe. Ihre Struktur wird anhand der IR- und NMR-Daten diskutiert.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19821150913
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  • 2
    Electronic Resource
    Electronic Resource
    Azobrücken aus Azinen, IV. Intramolekulare [2 + 2]-Photocycloaddition zwischen parallelen C=C- und N=N-Bindungen (1984)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 117 (1984), S. 1465-1475 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Azo Bridges from Azines, IV1). Intramolecular [2 + 2] Photocycloaddition of Parallel C=C and N=N BondsThe parallel C=C and N=N bonds in the rigid molecules 1 - 10 photocyclize nearly quantitatively, forming 1,2-diazetidines 11 - 20. Their structure is confirmed by spectroscopic methods and for 13 by X-ray analysis. Radiation induced denitrogenation, the normal reaction for similar compounds without neighbouring C=C bonds, is suppressed even with the sensitive derivatives of 2,3-diazabicyclo[2.2.1]heptene. Photocyclization of 6, carrying two neighbouring C=C bonds, includes only the norbornene bond.
    Notes: In den starren Molekülen 1 - 10 reagieren die benachbarten parallelen C=C- und N=N-Bindungen nahezu quantitativ unter Photocyclisierung zu den 1,2-Diazetidinen 11 - 20, deren Struktur spektroskopisch und für 13 durch Kristallstrukturanalyse bewiesen wird. Die in Abwesenheit der C=C-Bindung beobachtete Photo-Denitrogenierung unterbleibt selbst bei den empfindlichen Derivaten des 2,3-Diazabicyclo[2.2.1]heptens. Photocyclisierung von 6 mit zwei zur N=N-Bindung benachbarten C=C-Bindungen tritt nur mit der Norbornendoppelbindung ein.
    Additional Material: 5 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19841170416
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  • 3
    Electronic Resource
    Electronic Resource
    Strukturdynamische Organometall-Komplexe, II. Synthese, Struktur und Dynamik der Komplexe C5H5M(2-R′C3H4)PR3 (M=Pd, Pt) (1980)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 2291-2307 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Structurally Dynamical Organometal Complexes, II. Synthesis, Structure, and Dynamics of the Complexes C5H5M(2-R′C3H4)PR3 (M=Pd, Pt)The complexes C5H5M(2-R′C3H4)(M=Pd with R′=Me, t-Bu; M=Pt with R′=Me) react with an equimolar amount of PR3 (PR3=P(i-Pr)3, P(i-Bu)3, PPh2 (t-Bu), PCy3, PPhCy2) to form the compounds C5H5M(2-R′C3H4)PR3. The 1H and 13C NMR spectra indicate that in the complexes C5H5Pd(2-t-BuC3H4)PR3 and C5H5Pt(2-MeC3H4)PR3 within the temperature range of - 60 to +60°C the cyclopentadienyl ligand is monohapto-(σ-)and the allylic ligand trihapto-(π-)bonded. The complexes C5H5Pd(2-MeC3H4)PR3 exist in solution as a mixture of two isomers, (h5-C5H5)Pd(h1-allyl)PR3 (A) and (h1-C5H5)Pd(h3-allyl)PR3 (B). For complex 14 (PR3=PPhCy2) the thermodynamic and kinetic data of the intramolecular isomerisation process A ⇌ B have been determined. The X-ray structural analysis of 5 proves that the monohapto coordination of the C5H5 and the trihapto coordination of the 2-t-BuC3H4 ligand is retained in the crystal.
    Notes: Die Komplexe C5H5M(2-R′C3H4) (M=Pd mit R′=Me, t-Bu; M=Pt mit R′=Me) reagieren mit einer äquimolaren Menge PR3 (PR3=P(i-Pr)3, P(i-Bu)3, PPh2(t-Bu), PCy3, PPhCy2) zu den Verbindungen C5H5M(2-R′C3H4)PR3. Die 1H- und 13C-NMR-Spektren weisen daraufhin, daß in den Komplexen C(5H5Pd(2-t-BuC3H4)PR3 und C5H5Pt(2-MeC3H4)PR3 im Temperaturbereich von -60 bis +60°C der Cyclopentadienylligand monohapto- (σ-) und der Allylligand trihapto- (π-) gebunden ist. Die Komplexe C5H5Pd(2-MeC3H4)PR3 liegen in Lösung als Isomerengemisch von (h5-C5H5)Pd(h1-allyl)PR3 (A) und (h1-C5H5)Pd(h3-ally)PR3 (B) vor. Für 14 (PR3=PPhCy2) werden die thermodynamischen und kinetischen Daten der intramolekularen Isomerisierung A ⇌ B ermittelt. Die Röntgenstrukturanalyse zeigt, daß in 5 auch im Kristall der C5H5-monohapto- und der 2-t-BuC3H4-Ligand trihapto-koordiniert sind.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19801130622
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  • 4
    Electronic Resource
    Electronic Resource
    Transanulare Wechselwirkung des Azo-Chromophors in isodrinanalogen Systemen1) (1981)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 114 (1981), S. 423-432 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Transanular Interactions of the Azo Chromophore in Isodrin-type Systems1)The unusual transanular photoreactivity of the azo-compound 5 is also reflected in its photoelectron spectrum. The investigation of compounds 5, 13 and 14 reveals an effective interaction in 5 (through-bond and through-space) with H ij = -0.62 eV between πNN and πCC. This experimental value fits in well with known parameters of analogous isodrin-type systems. The excited states are looked into by means of semiempirical calculations with model compounds 17 and 19. Both the n-π+* and (at shorter wavelength) the π-π+* transition are conducive to an intramolecular photocycloaddition. X-ray diffraction has been used to determine the πNN,πCC-transanular distance (2.91Å).
    Notes: Die ungewöhnliche transanulare Photoreaktivität der Azoverbindung 5 spiegelt sich auch im Photoelektronenspektrum wider. Die Untersuchung der Verbindungen 5, 13 und 14 läßt eine effektive Wechselwirkung (through-bond und through-space) von Hij = -0.62 eV zwischen πNN und πNN in 5 erkennen. Dieser experimentelle Wert steht in ausgezeichneter Übereinstimmung mit bekannten Parametern analoger isodrinartiger Systeme. An den Modellverbindungen 17 und 19 werden die angeregten Zustände mit Hilfe semiempirischer Rechnungen untersucht. Sowohl der n-;π+* - als auch der kurzwellige π-π+* Übergang sind einer intramolekularen Photocycloaddition förderlich. Durch Röntgenbeugung wird der πNN, πCC-Transanularabstand zu 2.91 Å ermittelt.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19811140203
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  • 5
    Electronic Resource
    Electronic Resource
    Aromaten(phosphan)metall-Komplexe, V. Zur Addition von Carbanionen an (Benzol)ruthenium(II)- und -osmium(II)-Komplexe. Kristall- und Molekülstruktur von (exo-6-n-C4H9-η5-C6H6)OsI(PMe3)2 (1984)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 117 (1984), S. 152-160 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Arene(phosphane)metal Complexes, V1). On the Addition of Carbanions to (Benzene)ruthenium(II) and -osmium(II) Complexes. The Crystal and Molecular Structure of (exo-6-n-C4H9-η5-C6H6)OsI(PMe3)2The complex [C6H6RuCl(PMe3)2]PF6 (1) reacts with methyllithium to give a mixture of products that contains (η5-C6H6CH3)RuCH3(PMe3)2 (2) as the main component. From 1 and LiC6H5/LiBr the bromide 3 is primarily formed but the final product is (η5-C6H6C6)H5RuC6H5(PMe3)2 (4). Reaction of [C6H6OsI(PMe3)2]PF6 (5) with organyllithium compounds LiR (R = CH3, C2H5, n-C3H7, n-C4H9, t-C4H9, C6H5) yields the complexes (η5-C6H6R)OsI(PMe3)2 (6 - 11). 31P NMR spectra of 6 - 11 indicate restricted rotation at low temperatures around the metal-ring axis. According to X-ray structure analysis of 9 (R = n-C4H9) the cyclohexadienyl ring possesses an envelope conformation. The n-butyl group occupies the exo-position at the sp3-C atom.
    Notes: Der Komplex [C6H6RuCl(PMe3)2]PF6 (1) reagiert mit Methyllithium zu einem Produktgemisch, welches (η5-C6H6CH3)RuCH3(PMe3)2 (2) als Hauptkomponente enthält. Aus 1 und LiC6H5/LiBr entsteht über 3 bei längeren Reaktionszeiten (η5-C6H6C6H5)RuC6H5(PMe3)2 (4). Die Umsetzung von [C6H6OsI(PMe3)2]PF6 (5) mit Organyllithium-Verbindungen LiR (R = CH3, C2H5, n-C3H7, n-C4H9, t-C4H9, C6H5 ergibt die Komplexe (η5-C6H6R)OsI(PMe3)2 (6 - 11), in denen nach den 31P-NMR-Spektren die Rotation um die Metall-Ring-Bindung bei tiefen Temperaturen stark eingeschränkt ist. Die Röntgenstrukturanalyse von 9 (R = n-C4H9) beweist die „Envelope“-Konformation des Cyclohexadienylrings. Die n-Butylgruppe befindet sich in der exo-Position am sp3-C-Atom.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19841170112
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  • 6
    Electronic Resource
    Electronic Resource
    Stereoisomere Aromastoffe, XVI. Struktur und Eigenschaften optisch reiner 2-Methyl-4-propyl-1,3-oxathian-3-oxide (1987)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 1987 (1987), S. 451-453 
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    ISSN: 0170-2041
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Stereoisomeric Flavor Compounds, XVI. - Structure and Properties of Optically Pure 2-Methyl-4-propyl-1,3-oxathiane 3-OxidesOxidation of cis-2-methyl-4-propyl-1,3-oxathiane (1) by NaIO4 yields diastereomeric sulfoxides (equatorial/axial relation 3:1), which were separated by liquid chromatography. From optically pure (2S,4R)-1 the sulfoxides 2 (75%) and 3 (25%) and from (2R,4S)-1 the sulfoxides 2′ (75%) and 3′ (25%) were generated. For 3 an X-ray structure analysis was performed.
    Notes: Durch Oxidation von cis-2-Methyl-4-propyl-1,3-oxathian (1) mit NaIO4 entstehen diastereomere Sulfoxide (äquatorial/axial-Verhältnis 3:1), die flüssigkeitschromatographisch rein erhalten werden. Aus optisch reinem (2S,4R)-1 werden die Sulfoxide 2 (75%) und 3 (25%), aus (2R,4S)-1 die Sulfoxide 2′ (75%) und 3′ (25%) erhalten. Für 3 wurde eine Röntgenstrukturanalyse durchgeführt.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jlac.198719870352
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  • 7
    Electronic Resource
    Electronic Resource
    Novel Concepts in Directed Biaryl Synthesis, IX. Synthesis and Structure of Benzonaphthopyranones, Useful Bridged Model Precursors for Stereoselective Biaryl Syntheses (1992)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 1992 (1992), S. 225-232 
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    ISSN: 0170-2041
    Keywords: Aryl coupling, intramolecular ; Biaryls, ester-type bridged, preparation and stereostructure of ; Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A practicable two-step procedure for the preparation of a series of lactone-type bridged biaryls 7 as favorable substrates for subsequent atropisomer-selective ring-opening reactions is described. Due to the efficiency of the coupling step, which tolerates even a tert-butyl group next to the biaryl axis and avoids problems of regioselectivity, a variety of differently substituted representatives is prepared. These cover a broad range of steric hindrance and thus molecular distortion. The structures are investigated mainly by NMR spectroscopy and X-ray diffraction, showing the lactones 7 to be helically distorted, depending on the size of the residues R.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jlac.199219920141
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  • 8
    Electronic Resource
    Electronic Resource
    Organometall-Imide - höhervalente Derivate der d-Metall-Säuren, 3. Synthese und Reaktionen von (Pentamethylcyclopentadienyl)(imido)-Komplexen des Molybdäns und Wolframs und eine effiziente Strategie zur Synthese der Organometallate NBu4[Cp*MO3] (M = Mo, W) (1992)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 125 (1992), S. 2379-2384 
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    ISSN: 0009-2940
    Keywords: Imido ligands ; Oxo ligands ; Pentamethylcyclopentadienyl ligand ; Molybdenum complexes ; Tungsten complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Organometallic Imido Complexes - Highervalent Derivatives of the d-Metal Acids, 3[4b]. - Synthesis and Reactions of Pentamethylcyclopentadienyl Imido Complexes of Molybdenum and Tungsten and an Efficient Strategy for the Synthesis of the Organometallates NBu4[Cp*MO3] (M = Mo, W)A convenient and new entry into the chemistry of highvalent pentamethylcyclopentadienyl halfsandwich complexes of molybdenum and tungsten is described. The reaction of Mo-(NtBu)2Cl2 or W(NtBu)2Cl2(py)2 with Cp*Li (Cp* = η5-C5Me5) provides a high-yield route to new complexes Cp*Mo-(NtBu)2Cl (1a) and Cp*W(NtBu)2Cl (1b) which are converted into a variety of diimido, monoimido, and oxo derivatives. Treatment of 1a,b with MeLi yields the highly volatile methyl derivatives Cp*Mo(NtBu)2Me (2a) and Cp*W(NtBu)2Me (2b), while protolysis of 1a,b with an excess of HCl gas leads to selective cleavage of only one imido function with formation of Cp*Mo(NtBu)Cl3 (3a) and Cp*W(NtBu)Cl3 (3b). In contrast, protolysis of 1a,b with aqueous HCl provides a high-yield route to the well-known organometallic oxides [Cp*MoO2]-(μ-O) (4a) and [Cp*WO2](μ-O) (4b). These two key compounds are easily converted into the organomolybdate and organotungstate salts NBu4[Cp*MoO3] (5a) and NBu4[Cp*WO3] (5b) by cleavage of the M-O-M bridge with NBu4[OH]. The X-ray structure of 3a is reported.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19921251109
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  • 9
    Electronic Resource
    Electronic Resource
    Hauptgruppenelement-Übergangsmetall-Mehrfachbindungen, IV. Katalytische Assistenz von [Cp(CO)3Mo]2 bei der Aggregation von Metallo-arsanen über Arsen-Metall-Doppelbindungskomplexe (1986)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 119 (1986), S. 378-382 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Main Group Element Transition Metal Multiple Bonds, IV. Catalytic Assistance by [Cp(CO)3Mo]2 in the Aggregation of Metallo-arsanes via Arsenic Metal Double Bond Complexes2)The metallo-arsanes Cp(CO)3M—AsMe2 (1a, b) (M = Mo, W) are converted to the double arsenido-bridged dinuclear complexes [(μ-AsMe2)Mo(CO)2Cp]2 (3a, b) in the presence of [Cp(CO)3Mo]2. Due to the unusual mild conditions of aggregation the intermediate formation of the double bonded species Cp(CO)2M=AsMe2 (2a, b) is postulated. The crystal structure of 3a is reported, which shows mutual trans arrangement of the cyclopentadienyl and CO ligands.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19861190133
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  • 10
    Electronic Resource
    Electronic Resource
    (I2GaS-i-C3H7)2, das erste „butterfly“-Molekül mit vierfach koordiniertem GalliumDiese Arbeit wurde vom Fonds der Chemischen Industrie unterstützt. Prof. Dr. M. Schmidt danken wir für die Ermöglichung dieser Untersuchungen.Professor Max Schmidt zum 60. Geburtstag gewidmet (1985)
    Weinheim : Wiley-Blackwell
    Zeitschrift für die chemische Industrie 97 (1985), S. 965-966 
    Details
    ISSN: 0044-8249
    Keywords: Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/ange.19850971111
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