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  • Life and Medical Sciences  (2,718)
  • Inorganic Chemistry  (1,273)
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  • 1982  (2,137)
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  • 1995-1999  (2,633)
  • 1980-1984  (2,137)
  • 1965-1969
  • 1955-1959
  • 1940-1944
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  • 1
    Electronic Resource
    Electronic Resource
    Synthese von 3-Oxo-8-oxabicyclo[3.2.1]oct-6-en-2-carbonitrilen aus γ-Brom-β-oxonitrilen und Furan via [4 + 3]-Cycloaddition von 1-Cyanallylium-2-olaten (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 355-380 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis of 3-Oxo-8-oxabicyclo[3.2.1]oct-6-ene-2-carbonitriles from γ-Bromo-β-oxonitriles and Furan via [4 + 3] Cycloaddition of 1-Cyanoallylium-2-olatesSome γ-bromo-β-oxonitriles 3 react with furan in the presence of silver oxide to form stereoselectively the title compounds 7. Satisfying yields are obtained only with those bromides 3, whose γ-carbon ist tertiary or which are monoalkylated both at the α- and γ-carbon atoms. The results are explained by a [4 + 3] cycloaddition of 1-cyanoallylium-2-olate intermediates (14) to the 1,3-diene system of the furan. With cyclic γ-bromo-β-oxonitriles (6) two types of cycloadducts were observed: 3-bromo-3-methyl-2-oxocyclohexanecarbonitrile (6b) and 3-bromo-2-oxocyclododecanecarbonitrile (6d) form the tricyclic [4 + 3] cycloadducts 10b and d, analogs of the bicyclic adducts 7. With 3-bromo-2-oxocyclohexanecarbonitrile (6a) and 3-bromo-5-tert-butyl-2-oxocyclohexanecarbonitrile (6e), however, the carbonyl oxygen is connected with an α-carbon of the furan to give the tricyclic [3 + 2] cycloadducts 12Aa and Ae. The structure of endo-2,endo-4-dimethyl-3-oxo-8-oxabicyclo[3.2.1]oct-6-ene-exo-2-carbonitrile (7eα) was determined by X-ray analysis.
    Notes: Verschiedene γ-Brom-β-oxonitrile 3 reagieren in Gegenwart von Silberoxid mit Furan stereoselektiv zu den Titelverbindungen 7. Befriedigende Ausbeuten werden nur mit solchen Bromiden 3 erhalten, deren γ-Kohlenstoff tertiär ist oder die sowohl am α- als auch γ-Kohlenstoff monoalkyliert sind (3c, e-h). Die Befunde werden durch eine [4 + 3]-Cycloaddition von intermediären 1-Cyanallylium-2-olaten (14) an das 1,3-Dien-System des Furans erklärt. Mit cyclischen γ-Brom-β-oxonitrilen (6) wurden zwei Typen von Cycloaddukten beobachtet: 3-Brom-3-methyl-2-oxocyclohexancarbonitril (6b) und 3-Brom-2-oxocyclododecancarbonitril (6d) reagieren zu den tricyclischen [4 + 3]-Cycloaddukten 10b und d, Analoga der Bicyclen 7. Bei 3-Brom-2-oxocyclohexancarbonitril (6a) und 3-Brom-5-tert-butyl-2-oxocyclohexancarbonitril (6e) wurde jedoch der Carbonyl-Sauerstoff mit einem α-Kohlenstoffatom des Furans verknüpft, wobei die tricyclischen [3 + 2]-Cycloaddukte 12Aa und Ae entstanden. Die Struktur von endo-2,endo-4-Dimetyl-3-oxo-8-oxabicyclo[3.2.1]oct-6-en-exo-2-carbonitril (7eα) wurde durch eine Röntgenstrukturanalyse bestimmt.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19821150132
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  • 2
    Electronic Resource
    Electronic Resource
    Metall-π-Komplexe von Benzolderivaten, XV. Bis(η6-naphthalin)chrom(0): Röntgenstrukturbestimmung und kernresonanzspektroskopische Untersuchung (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 334-345 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Metal-π-Complexes of Benzene Derivatives, XV. Bis(η6-naphthalene)chromium(0): X-Ray Structure Determination and Investigation by Nuclear Magnetic Resonance SpectroscopyBis(η6-naphthalene)chromium(0) (2) crystallizes in the space group P21/n with two molecules in the unit cell. The ligands in individual molecules of 2 are syn-oriented. The implied presence of a center of symmetry in 2 is caused by disorder that consists in the statistical occupation by chromium atoms of two equivalent sites between the six membered ring of pairs of parallel naphthalene ligands. The 1H and 13C NMR spectra of 2 are analysed and the spectroscopic parameters are discussed with reference to the respective data of free naphthalene as well as other (η-naphthalene)metal complexes.
    Notes: Bis(η6-naphthalin)chrom(0) (2) kristallisiert in der Raumgruppe P21/n mit zwei Molekülen in der Elementarzelle. Die Liganden in individuellen Molekülen von 2 nehmen dabei eine syn-Anordnung ein. Das Vorliegen eines Symmetriezentrums in 2 wird durch eine Fehlordnung vorgetäuscht, die darin besteht, daß in Paaren parallel angeordneter Naphthalin-Liganden linke und rechte Lücken zwischen den Sechsringen statistisch mit Chromatomen besetzt sind. Die 1H- und 13C-NMR-Spektren von 2 werden analysiert, und die spektroskopischen Parameter werden im Vergleich mit entsprechenden Daten des freien Naphthalins sowie anderer (η-Naphthalin)metall-Komplexe diskutiert.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19821150130
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  • 3
    Electronic Resource
    Electronic Resource
    Verfeinerung der Kristallstruktur von (Ethylendiamin)zink(II)-benzohydroxamat-hydrat, ZnC23H29N5O7 (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 393-395 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Refinement of the Crystal Structure of (Ethylenediamine)zinc(II) Benzohydroxamate Hydrate, ZnC23H29N5O7The already known structure1) of the title compound has been refined and slightly corrected from new data.
    Additional Material: 3 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19821150136
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  • 4
    Electronic Resource
    Electronic Resource
    Masthead (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982) 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19821150201
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  • 5
    Electronic Resource
    Electronic Resource
    Reaktionen von Allylidenphosphoranen mit Heterokumulenen, II. Neue Synthesen von 1,2,4-Pentatrienen und 2-Penten-1,5-dionen (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 3904-3907 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reactions of Allylidenephosphoranes with Heterocumulenes, II. New Syntheses of 1,2,4-Pentatrienes and 2-Pentene-1,5-dionesCinnamylidenetriphenylphosphorane (2a) undergoes Wittig reaction with ketenes to afford monomeric and dimeric 1,2,4-pentatrienes 4 and 5, resp. 4b reacts further with an excess of ketene via a [2 + 2]-cycloaddition, whereby the 3-styryl-1-naphthyl diphenylacetate 12 is formed. In contrast, with the α-phenylsubstituted phosphorane 2b, instead of the Wittig reaction addition of ketene takes place at both the α- and the γ-positions. The 1,3-diacyl-3-triphenylphosphonio-1-propen-3-enolate 6 readily hydrolyzes to the 2-pentene-1,5-dione 9.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19821151224
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  • 6
    Electronic Resource
    Electronic Resource
    Beiträge zur Chemie des Bors, 127. Hexamethylborazin-Galliumtrichlorid: Struktur in Lösung und in festem Zustand (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 2668-2673 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Contributions to the Chemistry of Boron, 127. Hexamethylborazine-Gallium Trichloride: Structure in Solution and in the Solid StateHexamethylborazine forms a 1:1 adduct 1 with gallium trichloride. It is isostructural with hexamethylborazine-aluminium tribromide. The BN heterocycle is no longer planer, and the molecule adapts almost Cs symmetry and contains a tetracoordinated nitrogen atom. 1 shows fluctional behavior in toluene solution at room temperature. The coordinated GaCl3 will no longer change its coordination site at T 〈 220 K (two signals each for the CH3N-and CH3B-protons). However, at T 〈 195 K an additional splitting of the signals is observed - three signals for each type of CH3 groups: this would be consistent with a pentacoordinated gallium atom and a bidentate borazine ligand.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19821150730
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  • 7
    Electronic Resource
    Electronic Resource
    Masthead (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982) 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19821150801
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  • 8
    Electronic Resource
    Electronic Resource
    Darstellung cyclischer Nitrone aus heterocyclischen N-(Benzyloxy)aminen (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 2679-2681 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Preparation of Cyclic Nitrones from Heterocyclic N-(Benzyloxy)aminesTreatment of heterocyclic N-(benzyloxy)amines 1 with concentrated hydrogen peroxide solution in acetic acid enables the preparation of 7-membered cyclic nitrones in respectable yields. This one-pot procedure offers some advantages compared with conventional routes.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19821150732
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  • 9
    Electronic Resource
    Electronic Resource
    Vinylcarbanionen, 13. Einfache Synthese von Oxalessigsäure-Derivaten (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 2674-2678 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Vinyl Carbanions, 13. Convenient Synthesis of Oxaloacetic Acid DerivativesThe vinyllithium derivatives 2a, b and 9a, b, obtained by direct lithiation of the functionally substituted acrylic acid derivatives 1a, b and 8a, b, respectively, react with heterocumulenes A-E such as phenyl isocyanate, phenyl isothiocyanate, and carbon dioxide to give derivatives of oxaloacetic acid. In a single step reaction the oxaloacetic acid monoester 6a and monoamide 6b were synthesized.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19821150731
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  • 10
    Electronic Resource
    Electronic Resource
    Synthese eines [3]-Praecatenans (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 2683-2696 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis of a [3]-PrecatenaneStarting from the previously synthesised compound 9a, the cyclophane 13 is prepared. Acetalisation with 1,25-dichloro-13-pentacosanone followed by nitration and reduction afforded the diamine 16. By cyclization of this compound in isoamyl alcohol with sodium carbonate and sodium iodide under high dilution conditions the monomeric products 17, 18, and 19 are obtained in yields of 5.0, 2.4, and 0.1%, respectively. On the basis of mass, 13C and 1H NMR spectra the structures of these compounds are discussed. The attempted transformation of the [3]-precatenane 17 into the [3]-catenane 24 gives a mixture of products among which 24 could not be identified with certainty.
    Notes: Ausgehend von der bereits früher hergestellten Verbindung 9a wird das Cyclophan 13 synthetisiert. Durch dessen Acetalisierung mit 1,25-Dichlor-13-pentacosanon, nachfolgende Nitrierung und Reduktion wird das Diamin 16 erhalten. Dessen Cyclisierung in Isoamylalkohol in Gegenwart von Natriumcarbonat und Natriumiodid unter Verdünnungsbedingungen ergibt die monomeren Cyclisierungsprodukte 17, 18 und 19 in Ausbeuten von 5.0, 2.4 und 0.1%. Die Struktur dieser Verbindungen wird anhand der Massen-, 13C-und 1H-NMR-Spektren diskutiert. Die versuchte Umwandlung des [3]-Praecatenans 17 in das [3]-Catenan 24 führt zu einem Produktgemisch, in dem 24 nicht mit Sicherheit identifiziert werden konnte.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19821150802
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  • 11
    Electronic Resource
    Electronic Resource
    Ozonolyse von symmetrisch 1,2-disubstituierten Ethylenen in salzsaurem Methanol: Säurekatalysierte Folgereaktionen von Primärspaltprodukten (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 2697-2706 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ozonolysis of Symmetrically 1,2-Disubstituted Ethylenes in HCl/Methanol Solutions: Acid Catalyzed Reactions of Primary Cleavage ProductsThe ozonolysis of olefins in 1 M anhydrous solutions of hydrogen chloride in methanol at ≤ 0°C was investigated. Upon warm-up of the ozonolysis products, the peroxidic primary fragmentation products were converted into non-peroxidic end-products by HCl-catalyzed reactions. Cyclopentene (1a) and cyclohexene (1b), e.g., afforded mixtures of the corresponding α,ω-dialdehyde-bis(dimethyl acetals) (8), dimethyl α,ω-dicarboxylates (9), and methyl ω-aldehyde dimethyl acetal carboxylates (10). Norbornene (1c) gave a mixture of the correspondingly substituted 1,3-cyclopentane compounds (8c-10c), phenanthrene (22) gave a mixture of methyl 2′-formyl-2-biphenyl-carboxylate (24a), 2,2′-biphenyldicarbaldehyde (24b), and dimethyl 2,2′-biphenyldicarboxylate (24c). A reaction scheme was advanced for the rationalization of the types and the distribution of the products. It was partly substantiated by model reactions.
    Notes: Die Ozonolyse von Olefinen in wasserfreien 1 M Lösungen von Chlorwasserstoff in Methanol bei ≤ 0°C wurde untersucht. Beim Erwärmen der Ozonolyseprodukte traten HCI-katalysierte Folgereaktionen ein, in deren Verlauf die peroxidischen Primärspaltprodukte in peroxidfreie Endprodukte umgewandelt wurden. Z. B. lieferten Cyclopenten (1a) und Cyclohexen (1b) Gemische der entsprechenden α,ω-Dialdehyd-bis(dimethylacetale) (8), α,ω-Dicarbonsäure-dimethylester (9) und ω-Aldehyd-dimethylacetal-carbonsäure-methylester (10). Norbornen (1c) ergab ein Gemisch der entsprechend substituierten 1,3-Cyclopentanverbindungen (8c-10c), Phenanthren (22) ein Gemisch von 2′-Formyl-2-biphenylcarbonsäure-methylester (24a), 2,2′-Biphenyldicarbaldehyd (24b) und 2,2′-Biphenyldicarbonsäure-dimethylester (24c). Für die Entstehungsweise und die Verteilung der Produkte wurde ein Reaktionsweg formuliert, welcher z. T. durch Modellreaktionen bestätigt wurde.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19821150803
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  • 12
    Electronic Resource
    Electronic Resource
    Triarylmethyl-Systeme, III. Synthese von α-Aryl[1.n]paracyclophanen (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 1755-1764 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Triarylmethyl Systems, III. Synthesis of α-Aryl[1.n]paracyclophanesAs triarylmethyl systems with unusual sterical orientation of the aryl rings α-aryl[1.n]paracyclophanes with n = 5-8 (1a-d, 8a,b) were synthesized via the corresponding dithia[1.(n + 2)]-paracyclophanes (2a-d, 6a,b) and the disulfones (3a-d, 7a,b) derived therefrom. The sterical situation in these α-aryl[1.n]paracyclophanes is discussed, especially on the basis of 1H NMR data.
    Notes: Als Triarylmethyl-Systeme mit ungewöhnlicher räumlicher Orientierung der Aryl-Ringe wurden α-Aryl[1.n]paracyclophane mit n = 5-8 (1a-d, 8a,b) über die entsprechenden Dithia-[1.(n + 2)]paracyclophane (2a-d, 6a,b) und die davon abgeleiteten Disulfone (3a-d, 7a,b) dargestellt. Die sterischen Verhältnisse dieser α-Aryl[1.n]paracyclophane werden, besonders anhand von 1H-NMR-Spektren, diskutiert.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19821150510
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  • 13
    Electronic Resource
    Electronic Resource
    Desulfurierungsreaktionen mit Eisencarbonyl-Verbindungen: Carbonyl(dioxolanyliden)eisen-Komplexe aus Thionocarbonaten (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 1787-1809 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Desulfurization Reactions with Iron Carbonyl Compounds: Carbonyl(dioxolanylidene)iron Complexes from ThionocarbonatesDesulfurizations of thionocarbonates 3 with Fe(CO)5 and Fe2(CO)9 yield tetracarbonyl(dioxolanylidene)iron(0) complexes 4 and olefins 2 under thermal conditions. Photochemical conditions lead to 4 and cluster compounds with the formula Fe3(CO)9S(dioxolanylidene) (5). In all reactions Fe3(CO)9S2 (6) was also isolated. The carbene complexes are characterized spectroscopically. An X-ray structure analysis of the tetracarbonyliron carbene complex 4j shows the dioxolanylidene ligand in the axial position of a distorted trigonal bipyramid. (Dioxolanylidene)iron(0) complexes are „ylides with inverse bond polarizations“ (15).
    Notes: Die Desulfurierung von Thionocarbonaten 3 mit Fe(CO)5 und Fe2(CO)9 gibt je nach Energiequelle unterschiedliche Reaktionsprodukte. Bei der thermischen Reaktion (105°C, Toluol) entstehen Tetracarbonyl(dioxolanyliden)eisen(0)-Komplexe 4 und Olefine 2. Durch Bestrahlung entsteht ebenfalls 4, außerdem werden Clusterverbindungen der Zusammensetzung Fe3(CO)9S(dioxolanyliden) (5) isoliert. Bei allen Reaktionen wird außerdem Fe3(CO)9S2 (6) gebildet. Eine Röntgenstrukturanalyse von 4j zeigte den Dioxolanyliden-Liganden in der axialen Position einer trigonalen Bipyramide. (Dioxolanyliden)eisen(0)-Verbindungen sind „Ylide mit inverser Bindungspolarisation“ (15).
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19821150513
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  • 14
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    Electronic Resource
    Neue Reagenzien, XX. (Triphenylstannyl)methyllithium und analoge Trialkylstannyl-Verbindungen, Synthese und Reaktionen (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 1810-1817 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New Reagents, XX. (Triphenylstannyl)methyllithium and Analogous Trialkylstannyl Compounds, Synthesis and Reactions(Triphenylstannyl)methyllithium (1a) and analogous trialkylstannyl compounds (1b, c) were synthesized by halogen-lithium exchange reactions from 3a-c. As shown by high yields, stannyl groups are capable of stabilizing a carbanionic centre. 1a reacts with aldehydes and ketones to give β-hydroxystannanes 5 which tend to form olefins.
    Notes: (Triphenylstannyl)methyllithium (1a) sowie analoge Trialkylstannyl-Verbindungen (1b, c) wurden durch Halogen-Lithium-Austausch aus 3a-c synthetisiert. Die erzielten hohen Ausbeuten zeigen, daß Stannylgruppen ein carbanionisches Zentrum stabilisieren. 1a reagiert mit Aldehyden und Ketonen zu β-Hydroxystannanen 5, die zur Olefinbildung neigen.
    Additional Material: 1 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19821150514
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  • 15
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    Electronic Resource
    Triarylmethyl-Systeme, IV. Synthese und Reaktionen von α-Hydroxy- und α-Halogen-α-aryl[1.n]paracyclophanen (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 1765-1774 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Triarylmethyl Systems, IV. Synthesis and Reactions of α-Hydroxy- and α-Halo-α-aryl[1.n]paracyclophanesBy bromination of hydrocarbons 1a-d and 6 α-bromo-α-aryl[1.n]paracyclophanes with n = 5-8 (2a-d, 7) were prepared. Via 2a-d α-hydroxy-α-aryl[1.n]paracyclophanes 3a-d were obtained, starting from which the α-chloro and α-fluoro derivatives 4a-d and 5a,b, resp., were synthesized. - Compounds of the types 2-5 were of interest as representatives of a special triarylmethyl system for which, due to the [1.n]paracyclophane structure, unusual steric and electronic effects were to be expected. The formation of p,p′-bridged triarylmethyl radicals 8 from 2a-d and their dimerisation were investigated. Rate constants for the hydrolysis of α-bromo and α-chloro compounds 2a-d and 4a-d proceeding via the carbenium ions 9 were determined in water/acetone by conductivity measurements. Stabilities of 9 (n = 5-8), formed from the hydroxy compounds 3a-d in conc. sulfuric acid, were determined; their dependence on n is discussed in terms of specific steric and electronic effects of the α-aryl[1.n]paracyclophane system. Some spectroscopic data are reported for the carbanions 10.
    Notes: Durch Bromierung der Kohlenwasserstoffe 1a-d und 6 wurden α-Brom-α-aryl[1.n]paracyclophane mit n = 5-8 (2a-d,7) dargestellt. Aus 2a-d erhielt man die α-Hydroxy-Verbindungen 3a-d, von denen aus die α-Chlor- und α-Fluor-Derivate 4a-d bzw. 5a,b zugänglich waren. - Verbindungen des Typs 2-5 interessierten als Vertreter eines besonderen Triarylmethyl-Systems, für das als Folge der [1.n]Paracyclophan-Struktur ungewöhnliche sterische und elektronische Effekte zu erwarten waren. Die Bildung der p,p′-überbrückten Triarylmethyl-Radikale 8 aus 2a-d und ihre Dimerisierung wurden untersucht. Die Geschwindigkeiten der über Carbenium-Ionen 9 verlaufenden Hydrolysen der α-Brom- und α-Chlor-Verbindungen 2a-d bzw. 4a-d in Wasser/Aceton wurden durch Leitfähigkeitsmessungen bestimmt und mit denen der entsprechenden Di- und Triphenylmethyl-Derivate verglichen. Die Stabilitäten der aus den α-Hydroxy-Verbindungen 3a-d in konz. Schwefelsäure erzeugten Carbenium-Ionen 9 mit n = 5-8 wurden ermittelt; ihre Abhängigkeit von n wird unter dem Gesichtspunkt der sterischen und elektronischen Effekte des α-Aryl[1.n]paracyclophan-Systems diskutiert. Einige spektroskopische Daten der Carbanionen 10 werden mitgeteilt.
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    Protophane und Polyaromaten, XXVI. Synthese und Eigenschaften von Dehydrooligomeren von 2-(3-Thienyl)- und 2-(Benzo[b]thien-3-yl)chinoxalin (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 1825-1834 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Protophanes and Polyaromatics, XXVI. Synthesis and Properties of Dehydrooligomers of 2-(3-Thienyl)- and 2-(Benzo[b]thien-3-yl)quinoxalineMonolithiated 2-(3-thienyl)- (1a′) and 2-(benzo[b]thien-3-yl)quinoxaline (2a′) react in each case by selfaddition to polyadducts from which polyaromatics can be prepared by hydrolysis and subsequent oxidation. From the reaction mixtures open-chain polyaromatics with 4 to 12 aromatic units (1b-f, 2b-d) were isolated. Starting from 2a′, in addition to open-chain polyaromatics the cyclotetraaromatic 7 has been obtained in low yield.
    Notes: Monolithiiertes 2-(3-Thienyl)- (1a′) und 2-(Benzo[b]thien-3-yl)chinoxalin (2a′) reagieren jeweils durch Selbstaddition zu Polyaddukten, aus denen durch Hydrolyse und anschließende Oxidation Polyaromaten entstehen. Aus den Reaktionsgemischen konnten offenkettige Polyaromaten mit 4-12 Aromateneinheiten (1b-f, 2b-d) isoliert werden. Aus 2a′ entstand zusätzlich zu den offenkettigen Polyaromaten in geringer Ausbeute der Cyclotetraaromat 7.
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    Zur Chemie des Biquadricyclanylidens Inter- und Intramolekulare [π2+σ2+σ2]-Cycloadditionen (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 1835-1856 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Chemistry of Biquadricyclanylidene Inter- and Intramolecular [π2+σ2+σ2]-Cycloaddition ReactionsThe value of biquadricyclanylidene 6 for the synthesis of polychromophoric frameworks of the type 1-5 through [π2+σ2+σ2]-cycloaddition of bishomodienophilic partners is elucidated. Thus, dimethyl acetylenedicarboxylate, dicyanoacetylene, maleic anhydride, and dimethyl azodicarboxylate are added with very good to good yields (90-50%) exo-specifically and in the case of the bis-adducts with high anti-selectivity. N-Phenyl-1,2,4-triazolinedione, however, attacks the central C=C-double bond of 6 forming a 1:1-adduct considered to be the 1,2,4-triazolium-3-olate 40. With the conversion of 41 into 42 an intramolecular [π2+σ2+σ2]-cycloaddition has been realized for the first time. X-ray structural analyses of tetramethyl anti-9,9′-bi[(1α,2β,5β,6α)-tricyclo[4.2.1.02,5]nona-3,7-dienylidene]-3,3′,4,4′-tetracarboxylate (14a) and its exo-epoxide 23 have been performed.
    Notes: Die Brauchbarkeit des Biquadricyclanylidens 6 zum Aufbau polychromophorer Gerüste vom Typ 1-5 durch [π2+σ2+σ2]-Cycloaddition von bishomodienophilen Partnern wird untersucht. Acetylendicarbonsäure-dimethylester, Dicyanacetylen, Maleinsäureanhydrid und Azodicarbonsäure-dimethylester werden in diesem Sinn mit sehr guten bis guten Gesamtausbeuten (90-50%) exo-spezifisch, bei zweifacher Addition mit hoher Bevorzugung der anti-Isomeren, addiert. N-Phenyl-1,2,4-triazolindion greift 6 an der zentralen C=C-Doppelbindung unter Ausbildung eines vorläufig als 1,2,4-Triazolium-3-olat 40 angesprochenen 1:1-Adduktes an. Mit der Umwandlung 41 → 42 wird erstmals eine intramolekulare [π2+σ2+σ2]-Thermocycloaddition verwirklicht. Von anti-9,9′-Bi[(1α,2β,5β,6α)-tricyclo[4.2.1.02,5]nona-3,7-dienyliden]-3,3′,4,4′-tetracarbonsäuretetramethylester (14a) und seinem exo-Epoxid 23 wurden Röntgenstrukturanalysen durchgeführt.
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    Thermolyse des anti-9,9′-Bi[(1α,2β,5β,6α)-tricyclo[4.2.1.02,5]nona-3, 7-dienyliden]-3,3′,4,4′-tetracarbonsäure-tetramethylesters Eine effiziente intramolekulare 1,4-Cyclohexandiyl-Abfangreaktion - Eine vielstufige Isomerisierungssequenz (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 1857-1874 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Thermolysis of Tetramethyl anti-9,9′-Bi[(1α,2β,5β,6α)-tricyclo[4.2.1.02,5]nona-3,7-dienylidene]-3,3′,4,4′-tetracarboxylate An Efficient Intramolecular 1,4-Cyclohexanediyl Interception - A Multistep Isomerisation SequenceThe thermolysis of the anti-pentaene-tetraester 1, which is of interest in connection with its photochemistry, is examined. At 120°C 1 undergoes a uniform isomerisation with participation of four bonds to the octacycle 4. From the behaviour of several model compounds (2, 10-14) it is concluded that the transformation 1 → 4 begins with the 1,6-bridging between one of the orthogonal 1,5-diene segments and proceeds via a cascade of stabilised diradicals (5-7). This implies a quantitative, intramolecular interception of the 1,4-diyl intermediate (5) of the Cope reaction. Starting from 4 four additional, consecutively formed hepta- and hexacyclic isomerisation products (21 and 24-26) are isolated between 160 and 210°C. An x-ray structural analysis confirms the structure of 24.
    Notes: Die im Zusammenhang mit der Photochemie interessierende Thermolyse des anti-Pentaen-tetraesters 1 wird untersucht. 1 geht bei 120°C unter Beteiligung von vier Bindungen einheitlich in den isomeren Octacyclus 4 über. Aus dem Verhalten mehrerer Modellverbindungen (2, 10-14) wird geschlossen, daß die Umwandlung 1 → 4 mit der 1,6-Überbrückung in einem der orthogonalen 1,5-Diensegmente eingesetzt und über eine Kaskade stabilisierter Diradikale (5-7) abläuft. Damit ist impliziert, daß die 1,4-Diyl-Vorstufe der Cope-Reaktion (5) quantitativ intramolekular abgefangen wird. Ausgehend von 4 werden zwischen 160 und 210°C mit 21 und 24-26 vier weitere konsekutiv gebildete hepta- bzw. hexacyclische Isomerisierungsprodukte isoliert. Davon ist die Struktur 24 durch Röntgenstrukturanalyse bewiesen.
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    Polycyclische Verbindungen, XXI. Synthese konstitutionsisomerer Benz[c]azepin-Derivate durch 1,3-Transposition des Stickstoffs im Siebenring (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 2125-2134 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Polycyclic Compounds, XXI. Synthesis of Isomeric Benz[c]azepine Derivatives by 1,3-Transposition of the Nitrogen Function in the Seven-membered Ring SystemThe easily available oxanorbornadienes 1a and 1b are converted to various isomeric benz[c]azepine derivatives. The change of the position of the acetylated nitrogen in the seven-membered ring relative to the methoxycarbonyl groups in the six-membered ring by the reaction sequence 1 → 4 → 5 can be considered as a 1,3-transposition of the nitrogen function.
    Notes: Die leicht zugänglichen Oxanorbornadiene 1a und 1b können zu verschiedenen isomeren Benz[c]azepin-Derivaten abgewandelt werden. Die Änderung der Stellung des acetylierten Stickstoffs im Siebenring relative zu den Methoxycarbonylgruppen im Sechsring durch die Reaktionsfolge 1 → 4 → 5 kann als 1,3-Transposition der Stickstoff-Funktion aufgefaßt werden.
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    Elementorganische Amin/Imin-Verbindungen, XXIII. Aminophosphan- und Aminophosphoran-Rotamere (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 2076-2124 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Element-Organic Amine/Imine Compounds, XXIII. Rotamers of Aminophosphanes and AminophosphoranesThe diazaphosphasiletidines 3a-h can be synthesized from R2Si(NCR3Li)2 and Cl2PNR1R2 (1) as well as from (2) and MNR1R2 (R = CH3). At ambient temperature they show hindered rotation about the P—NR1R2 bond. 3g is separated as a pair of E/Z-rotamers, whose structure has been elucidated by NMR and X-ray analyses. The kinetically measured P—N rotation barriers (ΔG± ≍ 30 kcal · mol-1) are until now the highest that have been measured. The isomerization of 3g(E) → 3g(Z) (P—N) rotation, P inversion, or both) is a P—N rotation which has been established by the synthesis and the NMR spectroscopically measured rearrangement of (3i) (R = CH3, four isomers). The interaction of 3a-h with sulfur, selenium, and methyl iodide gives 4-6a-h. Below 0°C they all show hindered rotation about the P - NR1R2 bond. 4 and 5 are suitable for the study of the structure dependence of 1H NMR ASIS effects. The oxidation of 3g(E/Z) to the isomers 4g-6g(E/Z) occurs with retention of configuration. These compounds show significant differences with respect to their thermal stability and their reaction with methanol. The comparison of the ΔG± values of the P—N rotation barriers of 3-6 shows that the steric influence of the exo-amino substituents R1 and R2 is most important. The E/Z equilibrium of the unsymmetrically substituted compounds gives evidence that the two ground states of P—;N rotation are mostly influenced sterically, possible also electronically.
    Notes: Die Diazaphosphasiletidine 3a-h lassen sich aus R2Si(NCR3Li)2 und Cl2PNR1R2 (1) sowie aus (2) und MNR1R2 (R = CH3) darstellen. Sie weisen bei Raumtemperatur eine Rotationsbehinderung um die P—NR1R2-Bindung auf; 3g wird als E/Z-Rotamerenpaar getrennt und durch NMR- und Röntgenstrukturanalyse charakterisiert. Seine kinetisch ermittelten P—N-Rotationsbarrieren (ΔG± = ca. 30 kcal · mol-1) sind die bislang höchsten bestimmten Werte. Die Umlagerung von 3g(E) → 3g(Z) (P—N-Rotation, P-Inversion oder beides) ist eine P—N-Rotation, was durch Synthese und NMR-spektroskopische Verfolgung der Umlagerung des Isomerengemisches (3i) (R = CH3, vier Isomere) bewiesen wurde. Die Umsetzung von 3a-h mit Schwefel, Selen und Methyliodid ergibt 4-6a-h, die alle unterhalb 0°C eine Rotationsbehinderung um die P—NR1R2-Bindung aufweisen. 4 und 5 sind für das Studium der Strukturabhängigkeit von 1H-NMR-ASIS-Effekten geeignet. Die unter Konfigurationserhalt ablaufende Oxidation von 3g(E/Z) ergibt die Isomerenpaare 4g-6g(E/Z), die bemerkenswerte Unterschiede in bezug auf ihre Methanolyse- bzw. thermische Stabilität aufweisen. Der Vergleich der ΔG±-Werte für die P—N-Rotationsbarriere bei 3-6 zeigt, daß hier vorrangig der sterische Einfluß der exoständigen Aminosubstituenten R1, R2 verantwortlich ist. Aus den E/Z-Gleichgewichtslagen der unsymmetrisch substituierten Verbindungen erkennt man, daß auch die beiden Grundzustände der P—N-Rotation stark sterisch, möglicherweise aber auch elektronisch beeinflußt sind.
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    Fluorierungsreaktionen an 3,4-Dichlor-1,2,5-thiadiazol (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 2135-2140 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Fluorination Reactions at 3,4-Dichloro-1,2,5-thiadiazoleFrom the title compound 1 and KF in sulfolane 3-chloro-4-fluoro- (2) and 3,4-difluoro-1,2,5-thiadiazole (3) are obtained. In the reaction with oxidizing fluorinating agents, e. g. XeF2, BrF3, or AgF2, 2 is the primary product. Cleavage of the ring system at one of the S=N bonds gives the bifunctional ethane derivatives ClNCClCF2NSF2 (5), ClNCFCF2NSF2 (6), Cl2NCF2CF2NSF2 (7), and (=NCF2CF2NSF2)2 (8).
    Notes: Durch Umsetzung der Titelverbindung 1 mit KF in Sulfolan werden 3-Chlor-4-fluor-(2) und 3,4-Difluor-1,2,5-thiadiazol (3) erhalten. Die Reaktionen mit oxidierenden Fluorierungsmitteln wie XeF2, BrF3 oder AgF2 führen über 2 als Zwischenprodukt zur Spaltung des Ringsystems an einer der S=N-Bindungen. Dabei entstehen die bifunktionellen Ethanderivate CINCCICF2NSF2 (5), ClNCFCF2NSF2 (6), Cl2NCF2CF2NSF2 (7) und (=NCF2CF2NSF2)2 (8).
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    Cyclische Diazastannylene, XIII. [SnN2(CH3)2]4 und [SnNCH(CH3)2]4, Moleküle mit Cuban-Struktur (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 2141-2152 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Cyclic Diazastannylenes, XIII. [SnN2(CH3)2]4 and [SnNCH(CH3)2]4, Molecules with Cubane-like Structures1,3-Di-tert-butyl-2,2-dimethyl-1,3,2,4λ2-diazasilastannetidine (1) reacts in benzene with N,N-dimethylhydrazine spontanously and with isopropylamine after warming shortly to yield N,N′-di-tert-butyl-Si,Si-dimethylsilazane (2) and the tetrameric molecules (SnN2Me2)4 (5) and (SnNCHMe2)4 (6). An X-ray structure determination (R = 0.026) proves 5 to be built of a very distorted Sn4N4-cube, the nitrogen atoms being attached to dimethylamino groups. In the crystal the molecules are linked together by Sn—Sn contacts (351 pm) forming a zick-zack band, which runs in the direction of the hexagonal axis. Typical Sn—N bond lengths are found to be 220.9 and 225.1 pm, while the mean N—N distance is 146.2 pm. When heated or by contact with oxygen the crystals of 5 decompose vehemently: the products are found to be β-tin, molecular nitrogen, and varying amounts of methane, ethane, and dimethylamine (by contact with oxygen small amounts of tin(II)-oxide are formed as well).
    Notes: 1,3-Di-tert-butyl-2,2-dimethyl-1,3,2,4λ2-diazasilastannetidin (1) reagiert in Benzol mit N,N-Dimethylhydrazin spontan und mit Isopropylamin nach kurzem Erwärmen zu N,N′-Di-tert-butyl-Si,Si-dimethylsilazan (2) und den Tetrameren (SnN2Me2)4 (5) und (SnNCHMe2)4 (6). Eine Röntgenstrukturbestimmung (R = 0.026) zeigt, daß 5 einen stark verzerrten Sn4N4-Kubus besitzt, an dessen Stickstoffatome Dimethylaminogruppen gebunden sind. Im Kristall sind die Moleküle über Sn—Sn-Kontakte (351 pm) zu einem Zickzack-Band verknüpft, das in Richtung der hexagonalen Achse verläuft. Typische Sn—N-Bindungslängen liegen bei 220.9 und 225.1 pm, während für N—N 146.2 pm ermittelt werden. Beim Erhitzen sowie bei Sauerstoffzufuhr zersetzen sich die Kristalle von 5 heftig: als Produkte erhält man β-Zinn, molekularen Stickstoff und in wechselnden Mengen Methan, Ethan und Dimethylamin (bei Sauerstoffeinwirkung auch geringe Mengen an Zinn(II)-oxid).
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    Phosphinomethyl complexes of zirconium: A molecular orbital study of structure, bonding and reactivity problems (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 2153-2174 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Phosphinomethyl-Komplexe des Zirconiums: Eine MO-Studie über Struktur-, Bindungs- und ReaktivitätsproblemeDie Elektronenstruktur und Geometrie gewinkelter Phosphinomethyl-Sandwichkomplexe von ZrIV und ZrIII wird mit Hilfe von Molekülorbital-Berechnungen untersucht. Fragmentorbital-Betrachtungen und störungstheoretische Argumente werden verwandt, um die ungewöhnliche experimentelle Struktur von Cp2ZrCl(CH2PPh2) (1) zu erklären. Der Einfluß verschiedener Faktoren auf einzähnige (η1) gegenüber zweizähniger (η2) Koordination eines Phosphinomethyl-Liganden in Zirconocenderivaten wird analysiert, eine verallgemeinernde Extrapolation auf andere Cp2M(X)()-Systeme (: potentiell ein- oder zweizähniger Ligand) ist möglich. Strukturelle und chemische Konsequenzen der Ein-Elektronen-Reduktion von 1 werden auf der Basis von MO-Berechnungen interpretiert. besitzt demnach einen η1-Phosphinomethylliganden und erweist sich als instabil gegenüber heterolytischer Abspaltung von Cl- oder CH2PPh2-. Die Berechnungen ergeben für die Grundzustandsstruktur von Cp2Zr(CH2PPh2) η2-Koordination der Phosphinomethylgruppe, diese Struktur ist konsistent mit dem beobachtbaren ESR-Spektrum des Reduktionsproduktes von 1.
    Notes: The electronic structure and geometry of bent sandwich phosphinomethyl complexes of ZrIV and ZrIII have been investigated by means of molecular orbital calculations. A fragment MO approach and perturbation arguments are utilized to explain the unusual experimental structure of Cp2ZrCl(CH2PPh2) (1). Various factors influencing monodentate (η1) vs. bidentate (η2) ligand coordination of a phosphinomethyl ligand in zirconocene derivatives are analyzed, allowing to extrapolate to other Cp2M(X)() systems (: potentially mono- or bidentate ligand) in general. Structural and chemical consequences of one electron reduction of 1 are interpreted on the basis of the MO calculations. is shown to possess an η1-phosphinomethyl ligand and to be unstable towards heterolytic loss of Cl- or CH2—PPh2-. The ground state structure of d1-Cp2Zr(CH2PPh2) is calculated to contain an η2-phosphinomethyl group, consistent with the observed ESR spectrum of the reduction product of 1.
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    Cyclopropene als Komplexliganden: Metallinduzierte Ringöffnung und Carbonylierung eines Bicyclopropenyls unter Bildung eines Tropons. Die Kristallstruktur von Tricarbonyl(4-7-η4-2,3,5,7-tetraphenyl-2,4,6-cycloheptatrien-1-on)eisen, (C6H2Ph4CO)Fe(CO)3 (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 2175-2180 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Cyclopropenes as Complex Ligands: Metal Induced Ring Opening and Carbonylation of a Bicyclopropenyl with Formation of a Tropone Derivative. The Crystal Structure of Tricarbonyl(4-7-η4-2,3,5,7-tetraphenyl-2,4,6-cycloheptatrien-1-one)-iron, (C6H2Ph4CO)Fe(CO)32,2′,3,3′-Tetraphenylbi-2-cyclopropen-1-yl (1) reacts with Fe2(CO)9 at room temperature to form (4-7-η4-2,3,5,7-tetraphenyl-2,4,6-cycloheptatrien-1-one)Fe(CO)3 (3). This unexpected transformation of a bicyclopropenyl derivative into a tropone complex involves the opening of both cyclopropene rings, insertion of CO, and ring closure. Oxidation with Cer(IV) yields the uncomplexed tropone derivative. The crystal structure of the title compound 3 has been determined.
    Notes: 2,2′,3,3′-Tetraphenylbi-2-cyclopropen-1-yl (1) und Fe2(CO)9 reagieren bei Raumtemperatur unter Bildung von (4-7-η4-2,3,5,7-Tetraphenyl-2,4,6-cycloheptatrien-1-on)Fe(CO)3 (3). Diese unerwartete Umlagerung eines Bicyclopropenyl-Derivats in einen Tropon-Komplex verläuft unter Öffnung beider Cyclopropen-Ringe, CO-Einschub und Ringschluß. Oxidation mit Cer(IV) liefert daraus das freie Tropon-Derivat. Die Kristallstruktur der Titelverbindung 3 wurde bestimmt.
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    Kleine Ringe, 41. Oxiren: Zwischenprodukt oder Übergangszustand? - Matrixbestrahlung von Diazoketonen (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 2192-2201 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Small Rings, 41. Oxirene: Intermediate or Transition State? Matrix Irradiation of DiazoketonesOn irradiation of diazoketones - even of those which do not undergo a Wolff rearrangement under standard conditions - in an argon matrix at 10 K oxirenes (or acylcarbenes) cannot be detected directly.
    Notes: Bei der Belichtung von Diazoketonen - auch von solchen, die unter Normalbedingungen keine Wolff-Umlagerung zeigen - in einer Argonmatrix bei 10 K können Oxirene (oder Acylcarbene) nicht direkt beobachtet werden.
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    Kleine Ringe, 42. Versuche zur Darstellung von Oxirenen über photochemische Cycloreversionen (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 2202-2213 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Small Rings, 42. Attempts to Prepare Oxirenes via Photochemical CycloreversionsPhotochemically induced cycloreversions, which are ideally suited for the matrix isolation of cyclobutadienes, cannot be used for an analogous preparation and identification of oxirenes. In some cases ketenes are formed instead.
    Notes: Photochemisch induzierte Cycloreversionen, die sich bei der Matrixisolation von Cyclobutadienen bestens bewährt haben, lassen sich nicht auf eine analoge Erzeugung und den Nachweis von Oxirenen übertragen; stattdessen werden in einigen Fällen Ketene erhalten.
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    Carbonyl-Monoolefin-Derivate des Chroms, Molybdäns und Wolframs, III. Darstellung und Reaktivität von Tricarbonyl-Chelatphosphan-Olefin-Komplexen (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 3618-3630 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Carbonyl Monoolefin Derivatives of the Group VI Transition Metals, III. Preparation and Reaction and Reactivity of Tricarbonyl Chelate Phosphane Olefin DerivativesMonoolefin complexes M(CO)3(R2PC2H4PR2)(ol) (M = Cr, Mo, W; R = CH3, C6H5; ol = maleic anhydride, dimethyl fumarate, dimethyl maleate, methyl acrylate, ethylene, styrene, norbornene) are obtained photochemically from the tetracarbonyl chelate phosphane derivatives. Facial complexes are formed primarily, some of which rearrange intramolecularly to the meridional isomers. The substitution of the olefin proceeds via a dissociative mechanism, the meridional isomers rearrange back to the facial ones prior to the rupture of the metal-olefin bond.
    Notes: Monoolefin-Komplexe M(CO)3(R2PC2H4PR2)(ol) (M = Cr, Mo, W; R = CH3, C6H5; ol = Maleinsäureanhydrid, Dimethylfumarat, Dimethylmaleat, Methylacrylat, Ethylen, Styrol, Norbornen) sind photochemisch aus den Tetracarbonyl-Chelatphosphan-Derivaten zugänglich. Es entstehen zunächst faciale Komplexe, die sich zum Teil rasch intramolekular in die meridionalen Isomeren umlagern. Die Substitution des Olefins verläuft nach einem dissoziativen Mechanismus, der Spaltung der Metall-Olefin-Bindung geht bei den meridionalen Derivaten die intramolekulare meridional-facial-Isomerisierung voraus.
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    Darstellung, Struktur und thermisches Verhalten von (2-Chloracyl)diphenylphosphanen - ein neuer Weg zu Chlorketenen (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 2181-2191 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation, Structure, and Thermal Behaviour of (2-Chloroacyl)diphenylphosphanes - a New Pathway to ChloroketenesThe chlorinated acylphosphanes RC(O)—PPh2 (2a-f) are obtained by the reaction of the acyl chlorides RC(O)Cl (1a-f) with (CH3)3SiPPh2 in ether at -80°C. HCCl2C(O)—PPh2 (2c) crystallizes monoclinicly in the space group P21/c with Z = 8. As a result of steric caused electronic effects with increasing degree of chlorination in the series 2b → 2c → 2d a stepwise high field shift of the signals in the 31P{1H}-NMR spectra is observed. 2b-d,f are thermally labile and decompose with formation of ClPPh2 (3) and ketene at 80°C. The chloroketenes HCClCO (4) and CH3CClCO (5) are detected for the first time directly by means of their 13C NMR spectra. Between 0 and 40°C 2d also yields Cl3PPh2 (6). With cyclohexene or aniline 4 reacts to give the trapping products 8 and 9, respectively.
    Notes: Die chlorierten Acylphosphane RC(O)—PPh2 (2a-f) erhält man bei -80°C durch Umsetzung der Säurechloride RC(O)Cl (1a-f) mit (CH3)3SiPPh2 in Ether. HCCl2C(O)—PPh2 (2c) kristallisiert monoklin in der Raumgruppe P21/c mit Z = 8. Infolge sterisch bedingter elektronischer Effekte beobachtet man mit zunehmendem Chlorierungsgrad in der Reihe 2b ° 2c → 2d eine schrittweise Hochfeldverschiebung der Signale in den 31P{1H}-NMR-Spektren. 2b-d,f sind thermisch labil und zerfallen bei 80°C unter Bildung von ClPPh2 (3) und Keten. Die Chlorketene HCClCO (4) und CH3CClCO (5) konnten erstmals direkt durch ihre 13C-NMR-Spektren nachgewiesen werden. Zwischen 0 und 40°C liefert 2d auch Cl3PPh2 (6). Mit Cyclohexen oder Anilin reagiert 4 zu den Abfangprodukten 8 bzw. 9.
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    1,3-Dipolare Cycloadditionen, 86. Aromatische Azoxyverbindungen und gespannte Cycloalkene (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 2242-2255 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: 1,3-Dipolar Cycloadditions, 86. Aromatic Azoxy Compounds and Strained Cycloalkenes4,4′-Dicyano- and 4,4′-dinitroazoxybenzene as well as benzo[c]cinnoline N-oxide combine with (E)-cyclooctene or (1E, 5Z)-1,5-cyclooctadiene to give bicyclic 1,2,3-oxadiaxolidines which undergo in situ 1,3-dipolar cycloreversion with opening of both rings. Azomethine imines are formed which are connected by a hexamethylene chain with an aldehyde function. These new 1,3-dipoles add to a second molecule of the strained cycloalkene and furnish derivatives of cyclooctapyrazole as 1:2 adducts in high yields. A 1,4 H-shift of the intermediate azomethine imine competes at low concentration of the (E)-cyclooctene and produces an 8-hydrazino-7-octenal as a 1:1 product.
    Notes: 4,4′-Dicyan- und 4,4′-Dinitroazoxybenzol sowie Benzo[c]cinnolin-N-oxid vereinigen sich mit (E)-Cycloocten und (1E, 5Z)-1,5-Cyclooctadien zu bicyclischen 1,2,3-Oxadiazolidinen, die in situ unter Öffnung beider Ringe 1,3-dipolare Cycloreversion erleiden. Die entstehenden Azomethinimine, die über eine Hexamethylen-Kette mit einer Aldehydgruppe verbunden sind, addieren sich an ein zweites Molekül des gespannten Cycloalkens unter Bildung von Derivaten des Cyclooctapyrazols in hoher Ausbeute. Mit der Bildung dieser 1:2-Addukte konkurriert bei niedriger Konzentration des (E)-Cyclooctens eine 1,4-H-Verschiebung des intermediären Azomethin-imins, die zum Enhydrazin als 1:1-Produkt führt.
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    Sterischer Verlauf der Substitution am Cyclopropangerüst durch Cobal(I)oxim Synthese und Charakterisierung von Cyclopropylcobaloximen (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 2229-2241 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Steric Course of the Substitution at the Cyclopropane Skeleton by Cobal(I)oxime. Synthesis and Characterisation of Cyclopropylcobaloximes7,7-Dibromodibenzo[b,d]norcaradiene (1) as well as exo- and endo-7-bromodibenzo[b,d]norcaradiene (2a and b) were synthesized and reacted with cobal(I)oxime. (7-Bromodibenzo[b,d]norcaradien-7-yl)(pyridine)cobaloxime (5) was formed from 1 beside some (dibenzo[b,d]norcaradien-7-yl)(pyridine)cobaloxime (6) and (dibenzo[a,c]cycloheptatrien-6-yl)(pyridine)cobaloxime (4), whereas the reaction of 2a yielded 6 as the sole alkylcobaloxime. Under the same conditions 2b was inert. 4-6 were characterized by X-ray crystallography and spectroscopic methods. The substitution in 2a took place with retention, whereas the analogous substitution in the two enantiomeric 1-bromo-1-methyl-2,2-diphenylcyclopropanes (8a and b) occured with racemisation. This shows that the observed retention was caused merely by steric effects and that cyclopropyl radical intermediates occurred in both cases.
    Notes: 7,7-Dibromdibenzo[b,d]norcaradien (1) sowie exo- und endo-7-Bromdibenzo[b,d]norcaradien (2a und b) wurden synthetisiert und mit Cobal(I)oxim umgesetzt. Aus 1 erhielt man (7-Bromdibenzo[b,d]norcaradien-7-yl)(pyridin)cobaloxim (5) neben (Dibenzo[b,d]norcaradien-7-yl)(pyridin)cobaloxim (6) und (Dibenzo[a,c]cycloheptatrien-6-yl)(pyridin)cobaloxim (4), während aus 2a als einziges Alkylcobaloxim 6 gebildet wurde. 2b war unter denselben Reaktionsbedingungen inert. 4-6 wurden durch Röntgenstrukturanalyse und Spektren charakterisiert. Die Substitution an 2a erfolgte unter Retention, die analoge Substitution an den beiden enantiomeren 1-Brom-1-methyl-2,2-diphenylcyclopropanen (8a und b) dagegen unter Racemisierung. Dies zeigt, daß die im ersten Fall beobachtete Retention lediglich sterischen Effekten zuzuschreiben ist und in beiden Fällen eine freie Cyclopropyl-Radikal-Zwischenstufe auftritt.
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    Antitumor-aktive cis-Platin(II)-Komplexe mit α-Aminosäureestern und Peptidestern. Struktur von cis-Dichlorobis(glycylglycin-ethylester)platin(II) (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 2256-2270 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Antitumor Active cis-Platinum(II) Complexes with α-Amino Acid Esters and Peptide Esters. X-Ray Structure of cis-Dichlorobis(glycylglycine ethyl ester)platinum(II)A series of cis-platinum(II) complexes X2PtL2 (1-4) (X = halide, 2X = oxalate, malonate; L = α-amino acid ester, peptide ester) has been obtained from Pt42- and L. The dipeptide ester complexes are also accessible via peptide synthesis at the complex from Cl2Pt(NH2CHRCO2H)2 and α-amino acid esters using carbodiimide as coupling agent and the platinum atom as amino protecting group. The complexes Cl2PtL2 with α-amino acid ester ligands have also been prepared from the bis(chelate) compounds cis-Pt(NH2CHRCO2)2 and alcohol in the presence of HCl. The complexes have been characterized by their spectroscopic data, cis-Cl2Pt(GlyGlyOEt)2 (2a) by an X-ray analysis.
    Notes: Eine Reihe von cis-Platin(II)-Komplexen X2PtL2(1-4) (X = Halogenid, 2X = Oxalat, Malonat; L = α-Aminosäureester, Peptidester) wird aus PtX42- und L erhalten. Entsprechende Komplexe mit Dipeptidester-Liganden sind auch durch Peptidsynthese am Komplex aus Cl2Pt-(NH2CHRCO2H)2 und α-Aminosäureestern mit Carbodiimid als Kupplungskomponente und Platin als Aminoschutzgruppe zugänglich. Die Verbindungen Cl2PtL2 mit α-Aminosäureester-Liganden lassen sich auch aus den Bis(chelat)-Komplexen cis-Pt(NH2CHRCO2)2 und Alkohol in Gegenwart von HCl gewinnen. Die cis-Struktur der Verbindungen wurde spektroskopisch, die von Cl2Pt(GlyGlyOEt)2 (2a) durch Röntgenstrukturanalyse nachgewiesen.
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    Conformation in solution of tetraaryl-3,7-diazabicyclo[3.3.1]-nonanes and tetra- and pentaaryl-1,3-diazaadamantanes. A nuclear magnetic resonance study (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 2872-2891 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Konformation von Tetraaryl-3,7-diazabicyclo[3.3.1]nonanen und Tetra- und Pentaaryl-1,3-diazaadamantanen in Lösung. Eine NMR-StudieDie 1H-NMR-Spektren einer Reihe von Tetraaryl-3,7-diazabicyclo[3.3.1]nonanen 5-12 wurden mit Hilfe der Kern-Overhauser-Differenz-Spektroskopie zugeordnet. Aufgrund der NOE-Effekte und Spin-Gitter-Relaxationszeiten ließ sich zeigen, daß diese Moleküle die Sessel-Boot-Konformation einnehmen, wobei alle Arylgruppen äquatorial stehen. Diese Konformation und die Torsionswinkel der Arylgruppen ähneln denen, die im festen Zustand gefunden wurden. Analoge Untersuchungen wurden mit den Tetra- und Pentaaryl-1,3-diazaadamantanen 3, 4, 13 und 14 durchgeführt. Die beiden 1,3-diaxial orientierten Arylgruppen zeigen in diesen Systemen eine überraschend niedrige Rotationsbarriere (4b: δG298≠ = 42 kJ. mol-1). Die chemischen Verschiebungen in den 13C-NMR-Spektren aller Verbindungen werden mitgeteilt. Die der 3,7-Diazabicyclo[3.3.1]nonane 5-12 stehen im Einklang mit der vorgeschlagenen Sessel-Boot-Konformation. Das gleiche gilt für die chemischen Verschiebungen in den 15N-NMR-Spektren und die 13C-15N-Kopplungskonstanten. Die Reduktion des 4,8,9,10-Tetrakis(3,5-dimethylphenyl)-1,3-diaza-6-adamantanons (4b) führt stereoselektiv zum Alkohol 15, der sich säurekatalysiert leicht in 16 umlagert, den ersten Vertreter des 9-Oxa-1,5-diazatricyclo[5.3.1.03,8]undecan-Ringsystems.
    Notes: The proton NMR spectra of a series of tetraaryl-3,7-diazabicyclo[3.3.1]nonanes, 5-12, have been assigned with the aid of nuclear Overhauser difference spectroscopy. The NOE's together with spin lattice relaxation times have been used to show that these molecules adopt the chair-boat conformation with all aryl groups being equatorial. This conformation and the torsional angles of the aryl groups are similar to those found in the solid state. Analogous studies have been carried out with tetra- and pentaaryl-1,3-diazaadamantanes, 3, 4, 13, and 14. A surprisingly low barrier of rotation (4b: δG298≠ = 42 kJ. mol-1) has been found for the two 1,3-diaxially oriented aryl groups in these systems. Carbon-13 chemical shift data are reported for the above compounds. Those of the 3,7-diazabicyclononanes 5-12 are found to be consistent with the proposed chair-boat conformation. Nitrogen-15 chemical shift data and 13C-15N coupling constants are also in accord with this conformation. A stereoselective reduction of 4,8,9,10-tetrakis(3,5-dimethylphenyl)-1,3-diaza-6-adamantanone (4b) to the corresponding alcohol 15 and the ready acidcatalyzed rearrangement of this alcohol to 16, the first example of the 9-oxa-1,5-diazatricyclo-[5.3.1.03,8]undecane ring system, is described.
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    Zur Beweglichkeit im Ionenpaar bei der aromatischen Umlagerung von O-Sulfonyl-N-phenylhydroxylaminen (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 2865-2871 
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    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Internal Mobility in the Ion Pairs during Aromatic Rearrangement of O-Sulfonyl-N-phenylhydroxylaminesIn the rearrangement of O-alkyl- or O-arylsulfonyl-N-benzoyl-N-phenylhydroxylamines 3 to aminophenols 4, the internal mobility in the ion pair intermediates depends both on the size of the alkyl groups and on the interaction with the protic solvent, as was shown by 18O labeled educts.
    Notes: Bei der Umlagerung von O-Alkyl- bzw. O-Arylsulfonyl-N-benzoyl-N-phenylhydroxylaminen 3 in Aminophenole 4 wird durch 18O-Indizierung gezeigt, daß die Beweglichkeit in den intermediär gebildeten Ionenpaaren durch große Alkylreste sowie durch Wechselwirkung mit einem protischen Lösungsmittel in typischer Weise verändert wird.
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    Lösliche Perylen-Fluoreszenzfarbstoffe mit hoher Photostabilität (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 2927-2934 
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    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Soluble Perylene Fluorescent Dyes with High PhotostabilityThe preparation of several 3,4,9,10-perylenebis(dicarboximides) 1 is described and their photostability quantitatively determined and discussed. It is shown, that substitution of the insoluble perylene dye pigments with tert-butyl groups causes solubility in organic solvents leading to high quantum yields of these dyes.
    Notes: Die Darstellung einer Reihe von 3,4,9,10-Perylentetracarbonsäurediimiden 1 wird beschrieben und deren Lichtechtheit quantitativ untersucht und diskutiert. Es läß sich zeigen, daß durch Einführung von tert-Butyl-Substituenten die als sehr schwerlöslich bekannten Perylen-Pigmentfarbstoffe in organischen Solventien leicht löslich werden und mit hohen Quantenausbeuten fluoreszieren.
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    Untersuchungen zur Reaktivität von Metall-π-Komplexen, XXXVI. Zweikernige Sandwichkomplexe mit Metall-Metall-Bindung: Synthese und Struktur von (μ-C5H5)2Pd2(PR3)2 (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 2905-2913 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Studies on the Reactivity of Metal π-Complexes, XXXVI. Dinuclear Sandwich Complexes Containing a Metal-Metal Bond: Synthesis and Structure of (μ-C5H5)2Pd2(PR3)2The complexes (C5H5)2Pd2(PR3)2 (1-6) are prepared by reduction of C5H5Pd(PR3)OCOCH3 with NaK2.8 or in a one-pot synthesis by reaction of [(PR3)PdCl]2(μ-OCOCH3)2 with 4 equivalents TlC5H5. The triphenyl phosphite complex (C5H5)2Pd2[P(OPh)3]2 (7) is obtained from [P(OPh)3PdCl2]2 and TlC5H5. The X-ray structure analysis of (C5H5)2Pd2(PEt3)2 (5) shows that the two planar cyclopentadienyl ligands are coordinated sandwich-like to the Pd2(PR3)2 unit; according to the bond angle P—Pd—Pd = 175.45° the P—Pd—Pd—P arrangement is nearly linear. The different C—C distances in the five-membered rings point to the presence of an „allyl-ene“ system and thus to a trihapto- (h3) coordination of the C5H5 ligands.
    Notes: Die Komplexe (C5H5)2Pd2(PR3)2 (1-6) sind durch Reduktion von C5H5Pd(PR3)OCOCH3 mit NaK2.8 oder in einer Eintopfsynthese durch Umsetzung von [(PR3)PdCl]2(μ-OCOCH3)2 mit 4 äquivalenten TlC5H5 erhältlich. Der Triphenylphosphit-Komplex (C5H5)2Pd2[P(OPh)3]2 (7) entsteht aus [P(OPh)3Pdl2]2 und TlC5H5. Die Röntgenstrukturanalyse von (C5H5)2Pd2(PEt3)2 (5) zeigt, daß die beiden planaren Cyclopentadienylliganden sandwich-artig an die Pd2(PR3)2-Einheit koordiniert sind; die Anordnung P—Pd—Pd—P ist mit einem Bindungswinkel P—Pd—Pd von 175.45° nahezu linear. Die unterschiedlichen C—C-Abstände in den Fünfringen weisen auf das Vorliegen eines „allyl-ene“-Systems und damit auf eine trihapto- (h3)-Koordination der C5H5-Liganden hin.
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    Untersuchungen zur Reaktivität von Metall-π-Komplexen, XXXVII. Brückenaustauschreaktionen an zweikernigen μ-(Cyclopentadienyl)-dipalladium-Komplexen: Synthese sandwich-artiger heterometallischer Pd2Cr- und Pd2Mo-Cluster (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 2914-2926 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Studies on the Reactivity of Metal π-Complexes, XXXVII. Bridge-Exchange Reactions with Dinuclear μ-(Cyclopentadienyl)-dipalladium Complexes: Synthesis of Sandwich-like Heterometallic Pd2Cr and Pd2Mo ClustersThe dimetal sandwich complexes (C5H5)2Pd2(PR3)2 (I) react with carboxylic acids R'CO2H and thiols R'SH by exchanging one cyclopentadienyl bridge to yield the compounds (C5H5)(OCOR')-Pd2(PR3)2 (1-6) and (C5H5)(SR')Pd2(PR3)2 (7-12). Displacement of the cyclopentadienyl and not of the allyl ligand also occurs in the reactions of (C5H5)(2-RC3H4)Pd2[P(iPr)3]2 (II) with R'CO2H and R'SH with formation of the dinuclear μ-(allyl)-dipalladium compounds (2-RC3H4)-(OCOR')Pd2[P(iPr)3]2 (13-23) and (2-RC3H4)(SR')Pd2[P(iPr)3)2 (24-27). The reaction of (C5H5)-(2-MeC3H4)Pd2(P(iPr)3]2 (IIa) with terephthalic acid leads to the tetranuclear complex 28. The trinuclear heterometallic clusters 29, 30 are obtained by bridge-exchange starting from (C5H5)(OCO-tBu)Pd2[P(iPr)3]2 (4) and Na[C5H5Cr(CO)3] or Na[C5H5Mo(CO)3], respectively.
    Notes: Die Dimetall-Sandwichkomplexe (C5H5)2Pd2(PR3)2 (I) reagieren mit Carbonsäuren R'CO2H und Thiolen R'SH unter Austausch einer Cyclopentadienyl-Brücke zu den Verbindungen (C5H5)-(OCOR')Pd2(PR3)2 (1-6) und (C5H5)(SR')Pd2(PR3)2 (7-12). Bei den Umsetzungen der Komplexe (C5H5)(2-RC3H4)Pd2[P(iPr)3]2 (II) mit R'CO2H und R'SH wird ebenfalls der Cyclopentadienyl- und nicht der Allyl-Ligand verdrängt, so daß die zweikernigen μ-(Allyl)-dipalladium-Verbindungen (2-RC3H4)(OCOR')Pd2[P(iPr)3]2 (13-23) und (2-RC3H4)(SR')Pd2[P(iPr)3]2 (24-27) entstehen. Die Reaktion von (C5H5)(2-MeC3H4)Pd2[P(iPr)3]2 (IIa) mit Terephthalsäure führt zu dem Vierkernkomplex 28. Durch Brückenaustausch sind aus (C5H5)(OCO-tBu)Pd2[P(iPr)3]2 (4) und Na[C5H5Cr(CO)3] bzw. Na[C5H5Mo(CO)3] die dreikernigen heterometallischen Cluster 29, 30 zugänglich.
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    Untersuchungen an Diazoverbindungen und Aziden, XLII. (Diazomethyl)cyclopropene durch elektrophile Diazoalkan-substitution (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 2965-2980 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Investigations on Diazo Compounds and Azides, XLII. (Diazomethyl)cyclopropenes by Electrophilic Diazoalkane SubstitutionThe (diazomethyl)cyclopropenes 9 and 10 are formed via electrophilic diazoalkane substitution preferably of diazomethylphosphoryl compounds with cyclopropenylium salts. Either the diazomethyl compounds (7a-c) react with the cyclopropenylium salts 6a-e in the presence of triethylamine (method A) or the metallated diazo compounds 8a-d are combined with the cyclopropenylium bromides 6c-e (method B) (details see table 1). The (diazomethyl)cyclopropenes undergo a novel type of isomerization to pyridazines, partly without heating (9d-f → 11b-d), partly by refluxing in toluene (9a,g → 11a,e as well as 10e,f → 12a,b). The bicyclic betaines 15 and 17 are supposed to be intermediates. The diazomethyl compounds 9a and b yield the α,β- unsaturated ketones 20a and b by acid-catalyzed decomposition.
    Notes: Die (Diazomethyl)cyclopropene 9 und 10 entstehen durch elektrophile Substitution vorzugsweise von Diazomethylphosphorylverbindungen mit Cyclopropenyliumsalzen. Man setzt entweder die Diazomethylverbindungen selbst (7a-c) in Gegenwart von Triethylamin mit den Cyclopropenyliumsalzen 6a-e um (Methode A) oder läßt die metallierten Diazoverbindungen 8a-d mit den Cyclopropenyliumbromiden 6c-e reagieren (Methode B) (Details s. Tab. 1). Die (Diazomethyl)-cyclopropene gehen teils ohne Erwärmen (9d-f → 11b-d), teils beim Erhitzen in Toluol (9a,g → 11a,e sowie 10e,f → 12a,b) eine neuartige Isomerisierung zu Pyridazinen ein; Zwischenstufen sind vermutlich die bicyclischen Betaine 15 und 17. Die Diazomethylverbindungen 9a und b liefern bei der säurekatalysierten Zersetzung die α,β-ungesättigten Ketone 20a und b.
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    Strukturchemische Untersuchungen an Verbindungen mit formalen , und -Heteroalleneinheiten (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 2981-2996 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Structural Chemical Investigations on Compounds with Formal , and Heteroallene UnitsX-ray structures and syntheses of an (alkylidenamino)sulfonium salt (8), of an (alkylidenamino)-phosphonium salt (9c), and of a sulfimidophosphonium salt (10) are reported. These compounds which can formally be regarded as heteroallenes , , and , resp., are bent pseudoallenes in the crystal. The C—N—S bond angle of 8 is 118°. The positive charge is located on sulfur. According to 13C DNMR measurements 8 is bent also in solution. The bond angle of the C—N—P unit in solid 9c is 128°. The positive charge is delocalized between P and N. The activation energy of the geometrical isomerization around the C=N double bond in 9a, e in solution has been measured by dynamic 13C NMR spectroscopy to be ΔGTc≠ = 32.5 and 30.6 ± 1 kJmol-1, respectively. The S—N—P bond angle in 10 is 124°. The positive charge is delocalized between S and P.
    Notes: Es werden Synthesen und Röntgenstrukturanalysen eines (Alkylidenamino)sulfoniumsalzes (8), eines (Alkylidenamino)phosphoniumsalzes (9c) und eines Sulfimidophosphoniumsalzes (10) beschrieben. Diese als Heteroallene , bzw. formulierbaren Verbindungen sind im Kristall alle gewinkelte Pseudoallene. Verbindung 8 zeigt einen C-N-S-Bindungswinkel von 118°. Die positive Ladung ist am Schwefel lokalisiert. Nach 13C-DNMR-Messungen liegt 8 auch in Lösung gewinkelt vor. Der Bindungswinkel der C—N—P-Einheit in 9c beträgt im Kristall 128°. Die positive Ladung ist zwischen P und N delokalisiert. Für die Aktivierungsenergie der geometrischen Isomerisierung um die C=N-Doppelbindung in 9a, e werden in Lösung aus temperaturabhängigen 13C-NMR-Spektren δGTc≠ = 32.5 bzw. 30.6 ± 1 kJmol-1 gemessen. Der S—N—P-Bindungswinkel in 10 beträgt 124°. Die positive Ladung ist zwischen S und P delokalisiert.
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    Übergangsmetall-Carben-Komplexe, CXXIV. Ein- und zweikernige Biscarbenkomplexe von Chrom, Molybdän und Wolfram und ihre Umsetzung mit Bortrihalogeniden (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 2951-2964 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Transition Metal Carbene Complexes, CXXIV. Mono- and Binuclear Biscarbene Complexes of Chromium, Molybdenum, and Tungsten and their Reaction with Boron TrihalidesThe reaction of p-phenylenedilithium with hexacarbonylchromium and -tungsten and subsequent alkylation by triethyloxonium tetrafluoroborate yields μ-[p-phenylenebis[(ethoxy)carbene]]-bis-(pentacarbonylmetal) complexes (CO)5MC(OEt)-p-C6H4-(OEt)CM(CO)5 (M = Cr (3a), W (3b)) as well as the mononuclear carbene complexes 4a and 4b. The analogous reaction of o-phenylenedilithium with metalhexacarbonyls of the VI. subgroup affords the expected mononuclear 1,4-chelated biscarbene complexes (M = Cr (5a), Mo (5b), W (5c)), while 1,2-dilithio-1,2-diphenylethane gives a mixture of mononuclear (M = Cr (6a), W (6b)) and binuclear (CO)5MC(OEt)CH(Ph)CH(Ph)-(OEt)CM(CO)5 (M = Cr (7a), W (7b)) biscarbene complexes. The aminolysis of 5a - c with dimethylamine leads to cis-tetracarbonyl[o-phenylenebis[(dimethylamino)carbene]] compounds of chromium, molybdenum, and tungsten (8a - c). 3a, b and 4a, b react with boron trihalides BX3 to form the corresponding trans-halogenocarbyne complexes 9a, b and 10a - c. Properties, spectra, and the results of an X-ray structure analysis of 9b are reported.
    Notes: Die Umsetzung von p-Phenylendilithium mit Hexacarbonylchrom und -wolfram und anschließende Alkylierung mit Triethyloxonium-tetrafluoroborat ergibt μ-[p-Phenylenbis[(ethoxy)carben]]-bis(pentacarbonylmetall)-Komplexe (CO)5MC(OEt)-p-C6H4-(OEt)CM(CO)5 (M = Cr (3a), W (3b)), sowie die einkernigen Carbenkomplexe 4a und 4b. Die analoge Reaktion von o-Phenylendilithium mit Metallhexacarbonylen der VI. Nebengruppe ergibt die erwarteten einkernigen, 1,4-chelatisierten Biscarbenkomplexe (M = Cr (5a), Mo (5b), W (5c)), während 1,2-Dilithio-1,2-diphenylethan ein Gemisch von einkernigen (M = Cr (6a), W (6b)) und zweikernigen (CO)5MC(OEt)CH(Ph)CH(Ph)(OEt)CM(CO)5 (M = Cr (7a), W (7b)) Biscarben-Komplexen liefert. Die Aminolyse von 5a-c mit Dimethylamin führt zu cis-Tetracarbonyl[o-phenylenbis[(dimethylamino)carben]]-Verbindungen von Chrom, Molybdän und Wolfram (8a-c-). 3a, b und 4a, b reagieren mit Bortrihalogeniden BX3 unter Bildung der entsprechenden trans-Halogenocarbin-Komplexe 9a, b und 10a-c. Eigenschaften, Spektren und die Ergebnisse einer Röntgenstrukturuntersuchung an 9b werden beschrieben.
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    Einführung von Sauerstoff-Funktionen in die α-Stellung von β-Diketonen, 8. Ozonspaltung von Sulfonium-Yliden (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 3032-3041 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Introduction of Oxygen Functions into the α-Position of β-Diketones, 8 Ozonolysis of Sulfonium Ylides(Dimethylsulfonio)diacylmethanides 1, prepared by known methods, are cleaved by equimolar amounts of ozone in aprotic medium yielding vicinal triketones 2 and DMSO. Peroxydic reaction products are not detectable.
    Notes: Auf bekannte Weise leicht zugängliche (Dimethylsulfonio)diacylmethanide 1 lassen sich in aprotischem Medium durch äquimolare Mengen Ozon zu vicinalen Triketonen 2 und DMSO spalten. Peroxidische Reaktionsprodukte sind nicht nachweisbar.
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    Addukte von Lewis-Säuren mit 1,2,4λ4,3,5-Trithiadiazol-1-oxid (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 3025-3031 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Adducts of Lewis Acids with 1,2,4λ4,3,5-Trithiadiazole 1-OxideThe tittle compound 1 reacts with the Lewis acids SnCl4 and TiCl4 to yield the 2:1 adducts 1a and b and with AsF5 and SbF5 to form the 1:1 adducts 1c and d. According to the vibrational spectra and an X-ray analysis of 1a the coordination occurs via the oxygen atom. The ligands of 1a and b have cis-configuration. 1a crystallizes in the monoclinic space group P21.
    Notes: Die Titelverbindung 1 reagiert mit den Lewis-Säuren SnCL4 und TiCl4 zu den 2:1-Addukten 1a und b und mit AsF5 und SbF5 zu den 1:1-Addukten 1c und d. Nach den Schwingungsspektren und einer Röntgenstrukturanalyse von 1a erfolgt die Koordination über das Sauerstoffatom, und die Liganden in 1a und b haben cis-Konfiguration. 1a kristallisiert in der monoklinen Raumgruppe P21.
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    Beiträge zur Chemie des Bors, 128. Untersuchungen zum Substituentenaustausch mittels 10B-Isotopenmarkierung: Reaktionen von 1,3,2-Dithiaborolanen und verwandten Heterocyclen mit Bortribromid (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 3011-3024 
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    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, 128. Investigations on Substituent Exchange Reactions using 10B Labelling: Reactions of 1,3,2-Dithiaborolanes and Related Heterocycles with Boron TribromideThe formation of the bromo derivatives from methylated dithiaza- (3) and thiadiazadiborolidines (6) and BBr3 follows the endocyclic reaction mechanism. This holds also for the substituent exchange between some 2-bromo- (9) and 2-(dialkylamino)-1,3,2-dithiaborolanes (15, 18) as demonstrated by the use of 10BBr3. An addition of BBr3 to one of the ring sulfur atoms preceeds the substitution process. Some of these adducts were isolated and the equilibrium constants of the adduct formation were determined. 3,5-Bis(diisopropylamino)-1,2,4,3,5-trithiadiborolane (22) forms also an S-adduct with 10BBr3 (23). The substituent exchange proceeds endocyclically while the same reaction involving the 3,5-bis(dimethylamino) derivative follows the exocyclic route.
    Notes: Die Überführung der methylierten Dithiaza- (3) und Thiadiazadiborolidine (6) in die Brom-Derivate mit BBr3 folgt dem endocyclischen Substitutionsmechanismus. Gleiches gilt für den Substituentenaustausch zwischen einigen 2-Brom- (9) und 2-(Dialkylamino)-1,3,2-dithiaborolanen (15, 18), wie Umsetzungen mit 10BBr3 zeigen. Dem Substitutionsprozeß geht eine Addition des BBr3 an ein Ring-Schwefelatom voraus. Einige dieser Addukte wurden isoliert und die Gleichgewichtskonstanten der Adduktbildung bestimmt. Auch 3,5-Bis(diisopropylamino)-1,2,4,3,5-trithiadiborolan (22) bildet mit 10BBr3 ein S-Addukt (23). Dies führt zur endocyclischen Substitution, während der analoge Substitutionsprozeß bei dem 3,5-Bis(dimethylamino)-Derivat exocyclisch abläuft.
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    Übergangsmetall-Fulven-Komplexe, XX. Carbonylmetallkomplexe mit dimeren Fulvenliganden (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 3049-3062 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Transition Metal Fulvene Complexes, XX. Carbonyl Metal Complexes with Dimeric Fulvene LigandsThe synthesis and structure of four complexes (3a, 7, 9, 10) with dimeric fulvene ligands are reported. The compounds are formed in low yields by reaction of unsubstituted fulvene with Fe2(CO)9 (3a), of 6,6-diethylfulvene with Fe2(CO)9 (7), and of 6,6-bis(methylthio)fulvene with (CH3CN)3Mo(CO)3 (9 and 10), respectively. Moreover the structure of dimeric dimethylfulvene (11) has been determined by X-ray diffraction.
    Notes: Es wird über die Synthese und Struktur von vier Komplexen (3a, 7, 9, 10) mit dimeren Fulvenliganden berichtet. Die Verbindungen entstehen in geringer Ausbeute bei der Reaktion von unsubstituiertem Fulven mit Fe2(CO)9 (3a), von 6,6-Diethylfulven mit Fe2(CO)9 (7) bzw. von 6,6-Bis(methylthio)fulven mit (CH3CN)3Mo(CO)3 (9 und 10). Zusätzlich wurde die Struktur des dimeren Dimethylfulvens (11) röntgenographisch bestimmt.
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    Präparative Enantiomerentrennung von axial- und planarchiralen Benzolderivaten, Metallocenen und Methanoaza[10]annulenen durch Mitteldruckchromatographie an Triacetylcellulose (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 3042-3048 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparative Optical Resolution of Axial- and Planar-chiral Benzene Derivatives, Metallocenes, and Methanoaza[10]annulenes by Medium Pressure Chromatography on TriacetylcelluloseMedium pressure chromatography (at 4-6 bar and 6-40°C) on specially prepared triacetylcellulose in ethanol (or ether) renders possible an efficient preparative optical resolution of chiral benzene derivatives, (benzene)tricarbonylchromium complexes (benchrotrenes), ferrocenes, and azaannulenes. The method is presented for 15 selected examples such as 1,3-diferrocenyl-1,3-diphenylallene (1), 2,2′-spirobiindanes (2, 3), biphenyl derivatives (4-8) and their tricarbonylchromium complexes (9-11), [2.2]metacyclophanes (12-14) and 2,7-methanoaza[10]annulenes (15, 16) as well as for Troeger's base. In ten cases a quantitative separation of the enantiomers and in two an appr. 80 percent enantiomeric enrichment was achieved whereas for three compounds only a partial resolution took place.
    Notes: Mitteldruckchromatographie (bei 4-6 bar und 6-40°C) an speziell präparierter Triacetylcellulose in Ethanol (oder Ether) ermöglicht eine effiziente präparative Enantiomerentrennung chiraler Benzolderivate, (Benzol)tricarbonylchrom-Komplexe (Benchrotrene), Ferrocenderivate und Azaannulene. Die Methode wird an 15 ausgewählten Beispielen wie 1,3-Diferrocenyl-1,3-diphenylallen (1), 2,2′-Spirobiindanen (2, 3), Biphenylderivaten (4-8) und ihren Tricarbonylchrom-Komplexen (9-11), [2.2]Metacyclophanen (12-14) und 2,7-Methanoaza[10]annulenen (15, 16) sowie an der Trögerschen Base präsentiert. In zehn Fällen gelang eine quantitative Enantiomerentrennung, in zwei erfolgte eine etwa 80prozentige enantiomere Anreicherung und bei drei Verbindungen konnte partielle Trennung erzielt werden.
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    Über Thioacyl-isocyanate, XVIII. Reaktion von Ethoxy(thiocarbonyl)-isocyanat mit Aldehyden und Ketonen zu 1,3,5-Oxathiazinonen (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 3063-3068 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Thioacyl Isocyanates, XVIII. Reaction of Ethoxy(thiocarbonyl) Isocyanate with Aldehydes and Ketones to 1,3,5-Oxathiazinones[4 + 2]-Cycloaddition of ethoxy(thiocarbonyl) isocyanate with aldehydes and some ketones affords the oxathiazinones 3. α,β-Unsaturated aldehydes react in the same way, that means with maintenance of their multiple CC-bond. These facts differentiate the thioacyl isocyanates from acyl isocyanates as well as from unpolar dienes.
    Notes: Ethoxy(thiocarbonyl)-isocyanat addiert nach dem [4 + 2]-Prinzip Aldehyde und manche Ketone zu den Oxathiazinonen 3. Auch α,β-ungesättigte Aldehyde reagieren entsprechend, d. h. unter Erhaltung ihrer CC-Mehrfachbindung. Diese Verhaltensweisen unterscheiden die Thioacyl-isocyanate charakteristisch sowohl von Acyl-isocyanaten als auch von unpolaren Dienen.
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    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 
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    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.
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    Thion- und Dithioester, XXX. Reaktionen von Isocyaniden mit Thiooxalestern (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 3107-3114 
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    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Thiono and Dithio Esters, XXX. Reactions of Isocyanides with ThiooxalatesDimethyl tetrathiooxalate (1) reacts with all isocyanides 2 investigated to form 2-imino-1,3-dithioles 4 in high yield. Complex mixtures of products, however, are obtained from O,O-dimethyl dithiooxalate (5) and isocyanides. The main product is always the 1,3-thiazetidine 7, by-products are the azetidinethiones 8 and the 3,3′-biazetidine-2,2′-dithiones 6.
    Notes: Tetrathiooxalsäure-dimethylester (1) bildet mit allen untersuchten Isocyaniden 2 in einheitlicher Reaktion die 2-Imino-1,3-dithiole 4. Komplexe Produktgemische entstehen hingegen bei der Umsetzung von Dithiooxalsäure-O, O-dimethylester (5) mit Isocyaniden. Hauptprodukt ist stets das 1,3-Thiazetidin 7, Nebenprodukte sind die Azetidinthione 8 und 3,3′-Biazetidin-2,2′-dithione 6.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19821150916
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    2-Pyridylphosphane, II. Liganden für extrem kurze Metall-Metall-Kontakte in Goldkomplexen (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 3085-3095 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: 2-Pyridylphosphanes, II. Ligands for Extreme Short Metal-Metal Contacts in Gold Complexes2-C5H4N—P(CH3)2 (1a) and (2-C5H4N)2PCH3 (2a) and the corresponding phosphonium salts, phosphonium methylides, and phosphane-boranes are prepared. These 2-pyridylphosphanes (1a, 2a) and their phenyl homologues (4a, 5a) as well as (2-C5H4N)3P (3a) form stable 1:1 complexes 1e-5e with AuCl in the reaction with (CO)AuCl. CO is liberated in the process and the gold atoms retain coordination number 2 with phosphorus as the exclusive coordination site of the ligand. - Substitution of the chloride ion in 1e and 4e by BF4- or PF6- anions results in a head-to-tail dimerisation of the cations due to the poor donor capacity of the complex fluorides. A salt-like structure with metallacyclic dications is thus formed (1f, 4f, g). X-ray diffraction analysis of 1f shows an almost planar, centrosymmetrical eight-membered ring system, coplanar with the two attached pyridine rings. The two gold atoms are part of almost linear P—Au—N axes and are as close to each other as 277.6(1) pm. This distance is at the lowest limit hitherto found for formally nonbonded gold atoms.
    Notes: 2-C5H4N—P(CH3)2 und (2-C5H4N)2PCH3 sowie die korrespondierenden Phosphoniumsalze, Phosphonium-methylide und Phosphan-Borane werden dargestellt. Diese 2-Pyridylphosphane (1a, 2a) und ihre Phenyl-Homologen (4a, 5a) bilden ebenso wie (2-C5H4N)3P (3a) bei der Umsetzung mit (CO)AuCl stabile 1:1-Komplexe des Gold(I)-chlorids, in denen das Goldatom ausschließlich an das Phosphoratom koordiniert ist (1e-5e). Bei dieser Reaktion wird CO entbunden, und das Metall behält die Koordinationszahl 2 bei. Beim Ersatz der Chlorid-Ionen in 1e und 4e durch BF4- oder PF6-Anionen tritt wegen der geringen Donorstärke der neuen Liganden eine Kopf-Schwanz-Dimerisierung des Kations ein, die zu einer salzartigen Struktur mit metallacyclischen Dikationen führt (1f, 4f, g). Die Röntgenbeugungsanalyse zeigt für 1f ein fast planares, zentrosymmetrisches achtgliedriges Ringsystem, dem coplanar die Pyridinringe angegliedert sind. Die beiden Goldatome sind als Bestandteil zweier fast linearer P—Au—N-Achsen einander auf 277.6(1) pm angenähert. Dieser Abstand liegt an der untersten Grenze für bisher gefundene Distanzen zwischen formal nicht aneinander gebundenen Goldatomen.
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    Masthead (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995) 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280101
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    Tripodal Triamidostannates as Building Blocks in the Generation of Sn - M-Bonded Heterobimetallics (M = Fe, Ru) (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 29-34 
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    ISSN: 0009-2940
    Keywords: Tripodal ligands ; Triamidostannates ; Metal-metal bonds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: By in situ lithiation of the trifunctional amines H3CC(CH2NHSiMe3)3, PhC(CH2NHSiMe3)3, and HC{SiMe2NH(p-Tolyl)}3 and subsequent reaction with SnCl2 the corresponding triamidostannates were obtained. These were coupled with CpM(CO)2Cl (M = Fe, Ru) to yield the M - Sn-bonded heterobimetallics 9-14 of which H3CC(CH2NSiMe3)3SnFe(CO)2Cp (9) was characterized by a single-crystal X-ray structure analysis. Of the in situ-generated amidostannates only [HC{SiMe2N(p-Tolyl)}3Sn][Li(THF)3] (8) could be isolated as a uniform product and characterized analytically and spectroscopically.
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    The Structures of [X2Y—N—YX2]+ Cations (X = F, Cl; Y = S, Se). A Comparison of X-ray and ab Initio Studies[1] (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 35-40 
    Details
    ISSN: 0009-2940
    Keywords: Selenium-nitrogen compounds ; Sulfur-nitrogen compounds ; Calculations, ab initio ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The structures of cationic species of the series [X2Y—N—YX2]+ (X = F, Cl; Y = S, Se) have been computed ab initio using all electron treatments for first-row elements and sulfur and quasi-relativistic pseudopotentials for Se and Cl. Splitvalence basis sets with polarization and diffuse functions were employed. The MP2 results for the (non-isostructural!) cations [Cl2Se—N—SeCl2]+ (1: Cs) and [F2S—N—SF2]+ (2: C2v) are in excellent agreement with the experimental (X-ray) observations. Both structures represent local minima. A deeper minimum for either of the cations is represented by another C2v isomer which for crystal lattice energy reasons is stable in the isolated state only. The geometries of the hitherto unknown species [Cl2S—N—SCl2]+ (3) and [F2Se—N—SeF2]+ (4) have been assessed by ab initio HF calculations. In analogy to 2, cations 3 and 4 are predicted to prefer C2v symmetry. Therefore, 1 exhibits unusual structural features. According to strictly localized natural bond orbital analysis (NBO), the central nitrogen atoms in 1 and 2 possess two lone pairs of electrons (LP: one sp hybrid and one p orbital). The relatively short Se—N and S—N bond distances in 1 (1.741-1.760 Å) and 2 (1.551 Å) can best be attributed to LP(N)→s̰*(Y—X) negative hyperconjugation (1: Y = Se, X = Cl; 2: Y = S, X = F).
    Additional Material: 8 Ill.
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    Die fördernde Rolle von Phosphinoester-Liganden bei der Synthese neutraler Carben-, Vinyliden- und Allenyliden-Ruthenium(II)-KomplexeHerrn Professor Hubert Schmidbaur zum 60. Geburtstag gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 49-62 
    Details
    ISSN: 0009-2940
    Keywords: Ruthenium(II) complexes, octahedral ; Phosphino esters as mono- and bidentate ligands ; Fluxional behaviour ; Carbene complexes ; Vinylidene complexes ; Allenylidene complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Vinylidene Transition-Metal Complexes, XXXV[1].  -  The Supporting Role of Phosphino Ester Ligands for the Synthesis of Neutral Carbene, Vinylidene and Allenylidene Ruthenium(II) ComplexesThe reaction of [RuCl2(PPh3)3] (1) with the phosphino esters iPr2P(CH2)nCO2R (2-4) leads to complete (n = 1; R = CH3, C2H5) or partial (n = 2; R =CH3) displacement of the PPh3 ligands and formation of the octahedral ruthenium(II) complexes [RuCl2{k2(P,O)-iPr2PCH2CO2R}2] (5, 6) and [RuCl2(PPh3){k(P)-iPr2PCH2CH2CO2Me}{k2(P,O)-iPr2PCH2CH2CO2Me}] (7). Treatment of 5 with LiBr and LiI affords the dibromo- and diiodoruthenium derivatives 8 and 9. While compound 5 reacts with CO and SO2 by cleavage of one Ru - O bond to yield the 1:1 adducts [RuCl2(L){k(P)-iPr2PCH2CO2Me}{k2(P,O)-iPr2PCH2CO2Me}] (10, 11), the reaction of the dibromo derivative 8 with CO in solution gives the dicarbonyl complex [RuBr2(CO)2{k(P)-iPr2PCH2CO2Me}2](13). If CO is passed over 8 in the solid state, the corresponding monocarbonyl compound 14 is formed. The hydridoruthenium(II) complex 16, which is obtained from equimolar amounts of [RuHCl(CO)(PiPr3)2] (15) and 2, reacts with HC≡CMe by insertion to give the vinyl derivative [RuCl{E - CH=CHMe}(CO)(PiPr3){k2(P,O)-iPr2CH2CO2Me}] (17). Treatment of 5 with HC̊' (R' = H, Me, tBu, Ph) and of 6, 8, 9 with HC≡CPh affords upon photochemical activation the octahedral vinylidene complexes [RuX2-(=C=CHR){k(P)-iPr2PCH2CO2R}{k2(P,O)-iPr2PCH2CO2R}] (18-21 and 23-25) in good to excellent yield. At room temperature, these compounds (with the exception of 25) are highly fluxional in solution. From 31P-NMR measurements, the free energies of activation ΔG
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    Reaktionen von R2Al—AlR2 (R = CH(SiMe3)2) mit Trimethylsilylazid  -  Insertion in die Al—Al-Bindung und Abbau zum trimeren Dialkylaluminiumazid (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 81-85 
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    ISSN: 0009-2940
    Keywords: Aluminium-aluminium bond ; Insertion of trimethylsilyl azide ; Trimeric dialkylaluminium azide ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reactions of R2Al—AlR2 (R = CH(SiMe3)2) with Trimethylsilyl Azide  -  Insertion into the Al—Al Bond and Formation of a Trimeric Dialkylaluminium AzideTetrakis[bis(trimethylsilyl)methyl]dialuminium(4) (1) reacts with trimethylsilyl azide under insertion of one nitrogen atom into the Al—Al bond. As shown by NMR spectra and crystal structure the product contains three and four coordinated Al atoms due to the coordination of the α-nitrogen atom of the azide group to one of the Al atoms. An electronically delocalized N3-system is formed with a N—N bond length of 132.0 pm and a bond order of 1.5 for both N—N bonds. With an excess of trimethylsilyl azide further reaction is observed only under mild irradiation conditions with an exchange of the azide group between Si and Al and formation of Me6Si2 and the dialkylaluminium azide 3, which is better synthesized by the reaction of Me3Si—N3 with Cl—Al[CH(SiMe3)2]2. The sterically highly shielded aluminium azide 3 is a trimer in the solid state showing a non-planar 12-membered Al3N9 heterocycle with short N—N bonds (114 pm).
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    URL: http://dx.doi.org/10.1002/cber.19951280112
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    Transition-Metal Complexes with the Novel Scorpionate Ligand Dihydrobis-(tetrazolyl)borate: Synthesis and Characterization of Infinite Two-Dimensional Metal-Ligand Frameworks and One-Dimensional Water SubstructuresDedicated to Professor Dr. Herbert Schumann on the occassion of his 60th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 323-328 
    Details
    ISSN: 0009-2940
    Keywords: Poly(azolyl)borates, metal complexes of ; Bis(tetrazolyl)borate, metal complexes of ; Metal-nitrogen coordination ; Coordination polymers ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Dihydrobis(tetrazolyl)borate metal compounds of the composition [M(L)2{μ-H2B(CHN4)2}2]n for M = Mn, Fe, Co, Zn, Cd with L = H2O and for M = Cu with L = NH3 are obtained from metal salts and K[H2B(CHN4)2]. Single-crystal X-ray studies reveal the formation of two-dimensional rhombic grid sheets through the bridging action of the bis(tetrazolyl)borate ligands. Each metal atom is octahedrally coordinated with two trans L ligands and four H2B(CHN4)-2 nitrogen donors. Two additional, hydrogen-bonded water molecules occupy the rhombic openings in the compounds with M = Mn, Fe, Co, Zn, and Cd. The water of crystallization is held in place through hydrogen bonding from the water ligands and to the nitrogen atoms to give a substructure of parallel kinked water chains. Temperature-variable magnetic measurements show a Curie-Weiss behavior for the paramagnetic complexes with M = Mn, Fe, Co, and Cu.
    Additional Material: 8 Ill.
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    New Organophosphorus Ligands: Cyclopropanation and Other Reactions of Cumulenes Bearing Diphenylphosphanyl Substituents (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 365-371 
    Details
    ISSN: 0009-2940
    Keywords: Cumulenes ; Butadienes ; Vinylcyclopropane ; Vinylidenecyclopropane ; Bicyclopropyl, phosphanyl-substituted ; Cyclopropanation ; Phosphane ligands ; Phosphane chalcogenides ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Hydrophosphorylation of 1,4-bis(diphenylphosphanyl)butadiyne with diphenylphosphane leads to the butadiene (Ph2P)2C=CH—CH=C(PPh2)2 (1). Treatment of 1 with dimethylsulfonium methylide gives the vinylcyclopropane (Ph2P)2C=CH—CH(CH2)C(PPh2)2 (2). Compound 2 reacts with aqueous hydrogen peroxide, elemental sulfur, or selenium to afford the tetrachalcogenides (Ph2XP)2C=CH—CH(CH2)C(PXPh2)2 with X = O (3), X = S (4), X = Se (5), respectively. While the tetraphosphane 1 and the vinyl-cyclopropane compound 2 cannot be converted into a bis-(cyclopropyl) compound with an excess of Me2S=CH2, the tetrasulfide 4 readily affords a mixture of (1R,1′R)-/(1S,1′S)-and meso-2,2,2′,2′-tetrakis(diphenylthiophosphinyl)-1,1′-bicyclopropyl (6, 7) in good yield. Treatment of 1,1,4,4-tetrakis-(diphenylphosphanyl)butatriene with dimethylsulfonium methylide leads to the vinylidenecyclopropane (Ph2P)2C=C=C(CH2)C(PPh2)2 (8). Compound 8 is converted into its tetrasulfide (Ph2SP)2C=C=C(CH2)C(PSPh2)2 (9) by treatment with elemental sulfur. The crystal structures of 1, 2, 4, 7, and 8 have been determined by single-crystal X-ray diffraction.
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    Mono- und Diferriophosphane und -thioxophosphoraneHerrn Professor Dr. Ekkehard Lindner zum 60. Geburtstag gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 413-416 
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    ISSN: 0009-2940
    Keywords: Ferriophosphanes ; Ferriophosphoranes ; Thioxophosphane ligand ; Decarbonylation reaction ; Sulfurization ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Mono- and Diferriophosphanes and -thioxophosphoranesHerrn Professor Dr. Ekkehard Lindner zum 60. Geburtstag gewidmet.The substitution of organic substituents in phosphanes or thioxophosphoranes by the 17-electron fragments CpFe-(CO)2 (—Fp) leads to isolobal ferriophosphanes or -thioxophosphoranes. The mono- and diferriophosphanes FpnPPh3-n [n = 1 (3), 2 (4)] are obtained by deprotonation of the mono- and diferriophosphonium salts [FpnPPh3-nH]X [n = 1 (1), 2 (2)] with DBU. They are oxidized by sulfur giving the mono- and diferriothioxophosphoranes FpnPPh3-n(S) [n = 1 (5), 2 (6)]. Sulfide 5 arises also from the reaction of CpFe(CO)2Cl and Ph2PH(S)/DBU. The one-sided decarbonylation reaction of 6 leads to FpFp′PPh(S) (7, Fp′ = CpFeCO). The Fp substituents (17 electrons) in 3-7 coordinate as one-electron donors to the PhnP- or PhnP(S) units (n = 1, 2). The bridging functions in 4 and 6 are hitherto unknown. The molecular structures of the complexes 5-7 were determined by X-ray structure analyses.
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    About some Electrophilic Substitution Reactions with [(CF3S)3C+][AsF-6] (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 435-436 
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    ISSN: 0009-2940
    Keywords: Trifluoromethylthio group ; Carbenium ions ; Diphenylmethane ; Dyes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Tris(trifluoromethylthio)carbenium hexafluoroarsenate (1) reacts with N,N-dimethylaniline and anisole to form the corresponding diphenylmethanes 2, 3 with the SCF3 group at the methine carbon atom. During the reaction of 1 with benzene, compounds such as C6H5C(SCF3)3 and C6H5SCF3 are formed along with benzophenone, a product of hydrolysis of the diphenylmethane compound.
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    Synthesis and Structure of the First Dimetalated Diphosphane Disulfide [(η5-C5Me5)(CO)2FeP(H)(S)]2 (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 441-442 
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    ISSN: 0009-2940
    Keywords: Diphosphane disulfides ; Metallophosphoranes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The first transition metal derivative meso-[(η5-C5Me5)(CO)2FeP(H)(S)]2 (2) of the unknown diphosphane disulfide [PH2(S)]2 results from treatment of (η5-C5Me5)(CO)2FePH2 (1) with 1.5 equivalents of elemental sulfur. Compound 2 was characterized by means of spectroscopy (IR, 31P, 31P{1H}, 13C{1H}, 1H NMR) as well as X-ray diffraction analysis.
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    URL: http://dx.doi.org/10.1002/cber.19951280419
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    Preparation and Molecular Structures of Tetrahydrofuran, Diethylene Diglycol Dimethyl Ether and 18-Crown-6 Complexes of Strontium and Barium TetrahydridoborateDedicated to Prof. Dr. Nils Wiberg on the occasion of his 60th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 455-460 
    Details
    ISSN: 0009-2940
    Keywords: Strontium bis(tetrahydridoborate)-2 tetrahydrofuran, chain polymer of ; Strontium bis(tetrahydridoborate)-bis(diglyme) ; Barium bis(tetrahydridoborate)-bis(diglyme) ; Strontium bis(tetrahydridoborate)-1,4,7,13,16-hexaoxacyclooctadecane ; Metal-hydrogen-boron bridges ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The strontium and barium tetrahydridoborate complexes M(BH4)2 · 2 diglyme and M(BH4)2 · 18-crown-6 (M = Sr, Ba) have been prepared from the solvates M(BH4)2 · 2 THF by ligand displacement. 11B-NMR and IR data reveal strongly polar bonding of the BH4 groups to the metal centers, and X-ray structural analyses of the diglyme and crown ether compounds show molecular units in which the BH4 group is in contact via three H atoms with the metal center. In contrast, M(BH4)2 · 2 THF compounds are chain polymers in the solid state, and each metal center is surrounded by 2 THF molecules in trans position and four BH4- groups each of which forms bridges with two metal centers. Estimations of the effective radius for the BH4 group indicate a high polarity for the M-BH4 interaction.
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    Photochemische Reaktionen von Übergangsmetall-Organyl-Komplexen mit Olefinen, 1312. Mitteilung: Lit.Photochemisch induzierte [5+2],homo[5+21-Cycloaddition von 3-Hexin an Tricarbonyl(η5-2,4-cycloheptadien-l-yl)mangan (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 515-518 
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    ISSN: 0009-2940
    Keywords: Manganese ; Cycloheptadienyl ; Alkyne ; [5+2],homo[5+2] Cycloadditions ; Tricyclo[5.3.1.04,10]undeca-2,5-dien-11-yl ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Photochemical Reactions of Transition Metal Organyl Complexes with Olefins, 1312. Mitteilung: Lit. . - Photochemically Induced [5+2], homo[5+2] Cycloaddition of 3-Hexyne to Tricarbonyl(η 5-2,4-cycloheptadien-1-yl)manganeseTricarbonyl(η5-2,4-cycloheptadien-1-yl)manganese (1) reacts upon UV irradiation in hexane at 243 K with two equivalents of 3-hexyne (2) in successive [5+2],homo[5+2] cycloadditions to give tricarbonyl(η2:2:1-1,2,3,11-tetraethyltricyclo-[5.3.1.04,10]undeca-2,5-dien-11-yl)manganese (3). Its crystal and molecular structure was determined by an X-ray diffraction analysis, in solution it was studied also by IR and NMR spectroscopy.
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    Masthead (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995) 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    URL: http://dx.doi.org/10.1002/cber.19951280601
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    1,4,2-Diazaphospholothiazoles and -pyridines by a Hantzsch-Type Condensation Using Chloromethyldichlorophosphane (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 581-587 
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    ISSN: 0009-2940
    Keywords: Anellated azaphospholes ; Hantzsch-type [3 + 2] cyclocondensation ; Chloromethyldichlorophosphane ; Regioselectivity ; 31P-, 1H-, 13C-NMR spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The [3 + 2] cyclocondensation of 2-amino-1,3-thiazoline, 2-aminopyridines, 2- and 4-aminopyrimidines, 2-aminopyrazine, and 2-aminoquinoline with chloromethyldichlorophosphane in the presence of triethylamine yields regiospecifically 5,6-dihydrothiazolo[2,3-e][1,4,2]diazaphosphole (3), 1,4,2-diazaphospholo[4,5-α]pyridines (12), 1,4,2-diazaphospholo[4,5-α]pyrimidines (15), 1,4,2-diazaphospholo[4,5-e]pyrimidine (17), 1,4,2-diazaphospholo[4,5-α]pyrazine (19), and [1,4,2]diazaphospholo[4,5-α]quinoline (22), respectively. Using 2-amino-1,3-thiazole (4) and 2-aminobenzothiazoles 8, we obtained mixtures of the 1,5- and 4,5-anellated 1,4,2-diazaphospholes 5/6, 9a/10a and 9b/10b, while in the case of the methyl derivative 8c only the [1,4,2]diazaphospholo[5,4-b][1,3]benzothiazole 10c was formed. In the reaction of 2-aminothiazole and 2-aminopyrazine with Chloromethyldichlorophosphane the bis(diazaphospholo)-substituted chloromethylphosphanes 7 and 20 could be detected. The new anellated 1,4,2-diazaphospholes are colorless to pale yellow crystalline moisture-sensitive solids.
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    Reactions at Silicon-Silicon Bonds, V. Selective Trichlorosilylation of Alkyl(diorganylamino)chlorophosphanes with Hexachlorodisilane or with Trichlorosilane/Triethylamine. - Two Routes to New Functional Trichlorosilylphosphanes (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 615-619 
    Details
    ISSN: 0009-2940
    Keywords: Reductive silylation ; Aminochlorophosphanes ; Silylphosphanes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of alkyl(diorganylamino)chlorophosphanes R(R2′N)PCl 1 (1a: R = tBu, R′ = Et, 1b: R = iPr, R′ = iPr; 1c: R = iPr, R′ = Ph) with hexachlorodisilane, afforded alkyl(diorganylamino)trichlorosilylphosphanes R(R2′N)PSiCl3 2 (2a: R = tBu, R′ = Et; 2b: R = iPr, R′ = iPr; 2c: R = iPr, R′ = Ph) and silicon tetrachloride. An intermediate formed in the reaction of 1b with hexachlorodisilane, the adduct iPr(iPr2N)(Cl)P-Si(Cl)3-SiCl3 (3b = 1b · Si2Cl6), was detected by 31P- and 29Si-NMR spectra that indicate pentacoordinated silicon bound to tetracoordinated phosphorus and tetracoordinated silicon. Trichlorosilylphosphanes 2 are also available from 1 under very mild conditions by reductive trichlorosilylation with trichlorosilane in the presence of triethylamine. Compounds 2 were identified analytically, by mass spectroscopy, multinuclear NMR, and an X-ray structure determination of 2c.
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    Reactions of Complex Ligands, LXIVPart LXIII: Ref.. Synthesis of 5,5′-Diphenyl-2,2′-bifuran, a Biaryl Compound with Remarkable Fluorescence Properties (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 641-643 
    Details
    ISSN: 0009-2940
    Keywords: Carbene ligands ; Tungsten complexes ; 2,2′-Bifuran ; Copper coupling reaction ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The 2-oxacyclic α,β-unsaturated carbene complex 1 reacts with an excess of dimethylamine to give the diphenylbifuran 2. The structure of 2 was established by independent synthesis from 2-phenylfuran (4) via regioselective lithiation and transmetalation to zinc and tin organometallics 6a-c and final oxidative copper coupling reactions.
    Additional Material: 1 Tab.
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    URL: http://dx.doi.org/10.1002/cber.19951280618
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    Synthesis of 2- and 3-Stannolenes via Addition of Trimethyltin Alkoxides to 3-Diethylboryl-4-ethyl-1,1-dimethylstannole (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 679-687 
    Details
    ISSN: 0009-2940
    Keywords: Stannole, diethylboryl-substituted ; Trimethyltin alkoxides ; 2-, 3-Stannolenes, organometallic-substituted ; NMR, coupling constants, 2J(Sn,Sn), sign determination ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Trimethyltin alkoxides (2) react stereoselectively with 3-diethylboryl-4-ethyl-1,1-dimethylstannole (1) via addition of the Me3Sn group to C(2) to the C(2) = C(3) bond and a 1,2 shift of an ethyl group from boron to C(3) to give the 2-stannolenes 3. The molecular structure of 3f' [R = (S)-2-Bu] was determined by single-crystal X-ray analysis, confirming the cis positions of the Et(RO)B and the Me3Sn group. These 2-stannolenes 3 undergo, upon heating to ca. 80°C, facile rearrangement by irreversible allylic migration of the Et(RO)B group to the 3-stannolenes 4 in which the cis positions of the boryl and the stannyl group are retained. All 2-stannolenes (in contrast to the 3-stannolenes) are readily deprotoborylated to give the 3-stannolene 5. The structures of 3, 4, and 5 follow conclusively from 1H-, 11B-, 13C-, and 119Sn-NMR spectra. The negative sign of the geminal coupling constants 2J(SnSn) was determined in the case of 3, 4, and 5 by 2D 119Sn/1H heteronuclear shift correlations.
    Additional Material: 3 Ill.
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    Synthesis of Structures of (Acyloxy)boranesDedicated to Prof. Dr. A. Schmidpeter on the occasion of his 65th birthday.Synthesis of Structures of (Acyloxy)boranes (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 751-762 
    Details
    ISSN: 0009-2940
    Keywords: Trifluoroacyloxy-9-borabicyclo[3.3.1]nonane ; Pivaloyloxy-9-borabicyclo[3.3.1]nonane dimer ; Bis(9-borabicyclo[3.3.1]nonyl]oxalate ; Tetrakis(9-borabicyclo[3.3.1]nonyl)-dihydroxyoxalate ; Bis(9-borabicyclo[3.3.1]nonyl)-2,2-dimethylmalonate tetramer ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 9-Borabicyclo[3.3.1]nonane (9-BBNH) reacts with monocarboxylic acids to afford 9-(acyloxy)-9-borabicyclo[3.3.1]nonanes which are dimers in the solid state as shown by X-ray crystal structures of the benzoate and pivalate. More complex reactions were observed by allowing 9-BBNH to react with dicarboxylic acids in THF or monoglyme. Thus, (9-BBN)2 oxalate 3 contains a fully delocalized oxalate unit with equal C-O and B-O bond lengths. Traces of water convert it into the tetrakis(9-BBN) oxalate 5. A rather unusual structure is veryfied by 9-BBN 2,2-dimethylmalonate 7 which according to its molecular structure is a tetramer featuring a 32-membered ring system. In contrast, reactions of oxalic acid with thexylborane leads to reduction of the acid and formation of a bicyclic dioxaborolo-dioxaborolane 10. Several intermediates were detected by 11B-NMR spectroscopy as well as in reactions of BH3 · THF or BH3 · SMe2 with oxalic acid.  -  It follows from the present study that (acyloxy)boranes derived from dicarboxylic acids are strong Lewis acids with an unexpected variety of structural features.
    Additional Material: 7 Ill.
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    A T-Shaped Selenenyl Halide: Synthesis and Characterisation of a Proposed Reaction Intermediate (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 741-742 
    Details
    ISSN: 0009-2940
    Keywords: Selenenyl halides ; Nucleophilic substitution ; Complex intermediate ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The T-shaped selenenyl halide (1), which may be regarded as a model substance for the transition state in nucleophilic displacement at divalent chalcogen atoms, has been isolated and subjected to X-ray structure determination.
    Additional Material: 1 Tab.
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    URL: http://dx.doi.org/10.1002/cber.19951280715
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    Zinc Complexes of Drugs Containing Nitrogen Heterocycles (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 779-785 
    Details
    ISSN: 0009-2940
    Keywords: Zinc complexes ; Drug ligands ; Captopril ; Isoniazid ; Nalidixic acid ; Mercaptopurine ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Four drugs whose actions have a relation to the status of zinccontaining species in the human body were used as ligands in zinc complexes. Captopril (H2Cap) forms the compound [ZnCap] (1) presumed to be a coordination polymer with O and S coordination. Isoniazid, in the presence of zinc salts, is converted to 1,2-diisonicotinoyl hydrazide (H2Nih) which forms polymeric [Zn(Nih)NH3] (2) with trigonal-bipyramidal ZnO2N3 coordination. Nalidixic acid (HNal) and zinc perchlorate yield [Zn(HNal)2(H2O)2](ClO4)2 · 2 H2O (3) containing zinc in an octahedral ZnO6 environment. Mercaptopurine (H2Mer), in the presence of ammonia, forms [Zn(Mer)(NH3)2] . H2O (4) which is a coordination polymer containing tetrahedral ZnN4 units. The structures of [Zn(Nih)NH3], [Zn(HNal)2(H2O)2](ClO4)2 . 2 H2O, and [Zn(Mer)(NH3)2] . 2 H2O were determined diffractometrically.
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    Enantioselective Deprotonation of Benzyl Phosphates by Homochiral Lithium Amide Bases  -  Configurational Stability of Benzyl Carbanions with a Dialkoxyphosphoryloxy Substituent and Their Rearrangement to Optically Active α-Hydroxy Phosphonates (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 823-830 
    Details
    ISSN: 0009-2940
    Keywords: Phosphate-phosphonate rearrangement ; Carbanions, benzylic, configurational stability of ; Phosphonaes Lithium amides, homochiral ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Benzyl dialkyl phosphates are deprotonated enantioselectively by homochiral lithium amides of isopropyl(1-phenylethyl)amine or bis(1-phenylethyl)amine. The short-lived benzylic carbanions formed are virtually configurationally stable relative to the rearrangement to optically active phenyl-hydroxymethylphosphonates. The enantiomeric excesses are up to 50%. The pro-(S) hydrogen is removed by amides having (S) configuration. Homochiral diethyl (S)-phenyl[D1]-methyl phosphate [(S)-16c] is deprotonated by both LDA and n-BuLi with a high primary kinetic isotope effect (kH/D ≍ 50) and isomerizes to the corresponding α-hydroxy phosphonate with an enantiomeric excess of up to 85%.
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    Tris(1,10-phenanthroline)iron(II) Complexes  -  Broad Variation of the Redox Potential by 4,7-Substitution at the Phenanthroline Ligands[1] (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 845-850 
    Details
    ISSN: 0009-2940
    Keywords: Phenanthroline synthesis ; Tris(phenanthroline)iron(II) complexes ; Redox potential ; Cyclic voltammetry ; Electron transfer, outer-sphere ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The new 4,7-donor-substituted phenanthrolines 2a-h were synthesized and the corresponding tris(1,10-phenanthroline)iron(II) complexes 3a-h studied by cyclic voltammetry. In more detail three novel aza-crown ether-linked (phenanthroline)iron complexes were investigated, the redox potentials of which could be fine-tuned by the addition of group-Ia,IIa metal cations. All iron(II) complexes showed reversible waves at scan rates between 50 and 500 mV · s-1 and could be reversibly oxidized and reduced by chemical means.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951280816
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    Bis(cyclopentadienyl)methane-Bridged Dinuclear Complexes, 10Part 9: B. Stempfle, H. Werner, Gazz. Chim. Ital., 1995, 125, in press. The Bis(cyclopentadienyl)methane Link between Lewis Basic and Lewis Acidic Metal CentersDedicated to Prof. Dr. Herbert Schumann on the occasion of his 60th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 877-881 
    Details
    ISSN: 0009-2940
    Keywords: Bis(cyclopentadienyl)methane ; Heterobimetallic complexes ; Imido complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The mononuclear rhodium complexes [(C5H5CH2C5H4)-Rh(CO)2] (1) and [(C5H5CH2C5H4)Rh(PhC≡CPh)(PiPr3)] (2) readily react with nBuLi or TlOEt to yield the corresponding lithium salts 3 and 4 or thallium salts 5 and 6. The reaction of these salts with [(C5H5)Nb(NtBu)Cl2] (7) leads to the formation of the heterodinuclear compounds [{CH2(C5H4)2}-{Rh(CO)2}{(C5H5)Nb(NtBu)Cl}] (8) and [{CH2(C5H4)2}-{Rh(PhC≡CPh)(PiPr3)}{(C5H5)Nb(NtBu)Cl}] (9), respectively. Treatment of 3-6 with [Mo(NtBu)2Cl2] (10) gives the heterodinuclear Rh/Mo complexes [{CH2(C5H4)2}{Rh(CO)2}-{Mo(NtBu)2Cl}] (11) and [{CH2(C5H4)2}{Rh(PhC≡CPh)-(PiPr3)}{Mo(NtBu)2Cl}] (12). The analogous reaction of [Mo(NMes)2Cl2(DME)] (13) with 3-6 yields the corresponding complexes [{CH2(C5H4)2}{Rh(CO)2}{Mo(NMes)2Cl}] (14) and [{CH2(C5H4)2}{Rh(PhC≡CPh)(PiPr3)}{Mo(NMes)2Cl}] (15). From the monometallated ligand [(C5H5CH2C5H4)M] (M = Li: 16; M = Tl: 17) and the imidometal compounds 7, 10 and 13, the mononuclear complexes [(C5H5CH2C5H4)(C5H5)Nb-(NtBu)Cl] (18) and [(C5H5CH2C5H4)Mo(NR)2Cl] (R = tBu: 19; R = Mes: 20) have been obtained.
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    Addition von Hydrofullerid [C60H]- an koordinierte, ungesättigte Kohlenwasserstoffe: Bindung von Fulleren an Metallkomplexe über KohlenwasserstoffbrückenHerrn Professor Herbert Walter Roesky zum 60. Geburtstag gewidmet (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1059-1060 
    Details
    ISSN: 0009-2940
    Keywords: Fullerene ; Hydrofulleride ; Manganese complex ; Rhenium complex ; Iron complexes ; Ruthenium complex ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Addition of Hydrofulleride [C60H]- to Coordinated, Unsaturated Hydrocarbons: Binding of Fullerene to Metal Complexes through Hydrocarbon BridgesHerrn Professor Herbert Walter Roesky zum 60. Geburtstag gewidmet.Hydrofulleride [C60H]- is added to the hydrocarbon ligands of the cationic complexes [(OC)5Re(η2-C2H4)]+, [(OC)3Mn-(η6-C6H6)]+, [(OC)3M(η5-C6H7)]+ (M = Fe, Ru), [(OC)3Fe(η5-C7H9)]+, and [(η5-C5H5)Fe(η6-C5H4CH2)]+.
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    Controlled Conversion of the Transient 2-Mesityl-1,1-bis(trimethylsilyl)silene into a Tetrahydro-2,3-disilanaphthalene, a 1,2-Disilacyclobutane, or a 1,3-Disilacyclobutane (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1083-1088 
    Details
    ISSN: 0009-2940
    Keywords: Silenes ; Silene dimerization ; 1,2-Disilacyclobutanes ; 1,3-Disilacyclobutanes ; 2,3-Disilanaphthalene, tetrahydro- ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Mesityl[tris(trimethylsilyl)silyl]methanol (1) reacts with strong bases with elimination of trimethylsilanolate according to a Peterson-type mechanism, the outcome of the reaction being dependent on solvent, temperature, and nature of the organometallic base applied. Thus, 1 was converted by treatment with MeLi in ether at -78°C to (E)-1,2,3,8a-tetra -hydro-1-mesityl-5,7,8a-trimethyl-2,2,3,3-tetrakis (trimethylsi-lyl)-2,3-disilanaphthalene (3), formally a [2 + 4] cyclodimer of the transient silene (Me3Si)2Si=CHMes (2). The reaction of 1 with PhMgBr in THF after some days resulted in the formation of (Z)-3,4-dimesityl-1,1,2,2-tetrakis(trimethylsilyl) -1,2-disilacyclobutane (6) as the main product besides small quantities of 3, the polysilane (Me3SiSi(SiMe3)2CH2Mes (10), and the alkoxysilane (Me3Si)3SiCH(Mes)OSi(Si-Me3)2CH2Mes (7). Compound 6, the formal [2 + 2] cycloadduct of 2, can also be obtained by thermal treatment of 3 and is considered to be the thermodynamically more stable silene dimer whereas 3 is the kinetically preferred product. At high LiBr concentrations in the reaction mixture 1 was converted by PhMgBr in THF to (E)-2,4-dimesityl-1,1,3,3-tetrakis(tri- methylsilyl)-1,3-disilacyclobutane (13) besides 6 and [bis(tri-methylsilyl)silyl]mesityl(trimethylsiloxy)methane (11). The unforeseen formation of 13 is discussed as proceeding via the silene-lithium bromide adduct (Me3Si)2Si(Br)CH(Li)Mes (12). In the absence of LiBr 1 was converted by MeLi in THF at -78°C to 11 and the trisilane (Me3Si)2Si(Me)CH2Mes (4b). Probable pathways of the formation of all new compounds are discussed. For 6 and 13 the results of the X-ray structural analyses are given.
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    Metallkomplexe mit biologisch wichtigen Lisganden, LXXXLXXIX. Mitteilung: Lit.. (η3:η3-C10H16)Ru(IV)-Komplexe mit α-Aminocarboxylaten, α-Aminosäureestern und Peptidestern als Liganden (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1117-1125 
    Details
    ISSN: 0009-2940
    Keywords: 1,7-Dimethylocta-2,6-diene-1,8-diyl ; Ruthenium complexes ; α-Amino carboxylates ; α-Amino acid esters ; Peptide esters ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Metal Complexes Containing Biologically Important Ligands, LXXXLXXIX. Mitteilung: Lit. .  -  (η3:η3-C10H16)Ru(IV) Complexes with α-Amino Carboxylates, α-Amino Acid Esters, and Peptide Esters as LigandsReactions of the chloro-bridged bis(allyl) complex [(η3:η3-C10H16)Ru(Cl)(μ-Cl)]2 with α-amino carboxylates and α-amino acid esters afford the complexes (η3:η3-C10H16)(Cl)RuNH2CHRCO2 (2) and (η3:η3-C10H16)(Cl)2-RuNH2CHRCO2R′ (3). Abstraction of chloride from 3 by Ag+ gives the N,O-chelates [(η3:η3-C10H16)(Cl)RuNH2CHRCO2R′]+BF4 (4). Cysteine methyl ester forms the N,S-chelate complex (η3:η3-C10H16)(Cl)RuNH2CH(CO2CH3)CH2S (5), and with histidine methyl ester a dinuclear complex 6 with N,N-histidine bridge is obtained. Compound 3d with L-PheOEt as ligand was characterized by X-ray diffraction.
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    [MeO(CH2CH2O)3(CH2)3C5Me4]FeCl: A Halfsandwich Iron (II) Chloride Complex of Remarkable Stability (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1135-1136 
    Details
    ISSN: 0009-2940
    Keywords: Hemilabile ligands ; Cyclopentadienyl ligands, functionalised ; Iron compounds ; Halfsandwich complex ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reaction of iron(II) chloride with one equivalent of [MeO-(CH2CH2O)3(CH2)3C5Me4]Li in THF yields the title halfsand-wich complex 1, which is stable in solution up to room temperature. Compound 1 reacts with C5H5Li and CO to give [MeO(CH2CH2O)3(CH2)3C5Me4]Fe(C5H5) (2) and [MeO-(CH2CH2O)3(CH2)3C5Me4]Fe(CO)2CI (3), respectively, in high yields.
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    [Cp4Fe4(E2)2] Clusters with Triangulated Dodecahedral Fe4E4 Skeletons (E = P, As)Dedicated to Professor Herbert Schumann on the occasion of his 60th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1145-1148 
    Details
    ISSN: 0009-2940
    Keywords: P2, As2, P2S2, and P2Se2 ligands ; Iron complexes ; Triangulated dodecahedra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The thermolysis of [CpFe(CO)2]2 (1) and P4 or As4 affords the iron clusters [Cp4Fe4(E2)2], E = As (2a), P (2b), the Fe4E4 skeleton of which consists of a triangulated dodecahedron. S8 and gray Se oxidize the P2 ligands of 2b with formation of [Cp4Fe4(P2X2)2], X = S (3a), Se (3b), complexes with the hitherto unknown P2X2 ligands, 2a, b and 3a, b have been characterized by X-ray crystallography.
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    Functionalized Diorganozinc Compounds: Key Reagents for the Synthesis of Enantiomerically Pure 2,5-Disubstituted cis- and trans-Tetrahydrofurans (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1021-1028 
    Details
    ISSN: 0009-2940
    Keywords: Synthesis, stereoselective ; Catalysis ; Tetrahydrofurans ; Dialkylzinc reagents ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 1,4-Diol derivatives 4a-i were synthesized stereoselectively by either reagent- or catalyst-controlled routes using the addition of functionalized diorganozinc reagents to aldehydes. The stereoselectivities along the reagent-controlled synthetic path were in the range between 80:20 and 95:5. The stereoselectivities along the catalyst route exceeded 95:5. The 1,4-diol derivatives 4 thus obtained were transformed into enantiomerically pure cis- and trans-2,5-disubstituted tetrahydrofurans (16-20) by means of an intramolecular Williamson reaction.
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    Contributions to the Chemistry of Boron, 231Part 230: Ref.. Synthesis and Structures of Borylated HydrazinesDedicated to Professor H. P. Fritz on the occasion of his 65th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1187-1194 
    Details
    ISSN: 0009-2940
    Keywords: Hydrazines ; N,N'-bis(diphenylboryl)-N,N'-dimethyl- ; N,N'-bis(diphenylboryl)-N',N'-dimethyl- ; N,N'-bis(dimethylphenylsilyl)- ; N,N'-bis(chloromesitylboryl)-N'-phenyl-N'-(trimethylsilyl)- ; 1,2,4,5,3,6-Tetrazadiborinane, 1,2,4,5-tetrakis(tert-butyldimethylsilyl)-3,6-difluoro- ; Triazadiborolidine, dihydro-, derivative ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The diboration of the diazene PhN = NSiMe3 (15) by diborane(4) derivatives provides a new synthetic route to N,N'-diborylated hydrazines. The product formed depends on the type of the diborane(4) compound. Thus, addition of dimesityldiboron dichloride to 15 in a 1:1 ratio afforded (mesCIB)PhN-N(SiMe3)(BClmes) (16) while bis(dimethyl-amino)diboron dichloride was found to react in a 1:2 ratio to give a triazadiborolidine derivative 17. In addition, it was demonstrated that in the solid state Me2N-N(BPh2)2 (8) is a derivative of a three-membered dihydroazadiboriridine C while its isomer, (Ph2B)MeN-NMe(BPh2) (7), forms no BN coordinative bond. The new 3,6-difluoro-1,2,4,5-tetraza-3,6-diborine 13 shows a twist conformation. The molecular structures of all these compounds were determined by X-ray crystal structure analysis, and the influence of the B substituent on the conformation is discussed.
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    Metal Complexes of Functional Isocyanides, XXV. Amino(hydrazino)carbene Complexes (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1061-1068 
    Details
    ISSN: 0009-2940
    Keywords: N-Isocyanides ; N-Isocyanodialkylamine complexes ; Carbene complexes ; Imaging-Plate data collection ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The N-isocyanodialkylamine metal complexes [M(CO)5CN-NR2] (M = Cr, W), trans-[MI2(CNNR2)2] (M = Pd, Pt), trans-[Pt(Cl)(CNNR2)(PPh3)2]BF4, and cis-[PtCl2(CNNR2)(PPh3)] [R = Et, iPr; 2 R = -{CHMe(CH2)3CHMe}-] react with primary amines to give the amino(hydrazino)carbene metal complexes [M(CO)5(C(NHR′)NHNR2}] (R′ = Me, nPr, Cy) (1-9), trans-[PtI2{C(NHMe)NHNR2}2] (10-12) and trans, and the amine adducts cis-[PtCl2{C(NHMe)NHNC(H)(Me) (CH2)3CHMe}(PPh3)] H2NMe (14), and trans-[PdI2{C (NHMe)NHNC(H)(Me)(CH2)3CHMe}2] 2 H2NMe (15). With secondary amines the amino(hydrazino)carbene metal complexes trans (18) and trans-[PtCl{C(NEt2)NHNEt2} (PPh3)2]BF4 (19) Were isolated. The complexes trans-[PtI2{C(NHCy)NHNiPr2}CNNiPr 2] (20) and trans-[PdI2 (NH2Cy){C(NHCy)NHNiPr2}] (21) were obtained by reaction of trans-[MI2(CNNiPr2)2] (M = Pd, Pt) with cyclohexylamine. The structures were assigned on the basis of IR, NMR- (1H, 13C, 31P), and mass spectroscopy as well as an X-ray structural analysis of 21.
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    Metallocenophanes, VIIPart VI: Ref.. Preparation and Characterisation of the Disilver(I) Complexes of Conjugated Polyenes with [2.2.2]Paracyclophanyl End Groups (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1079-1082 
    Details
    ISSN: 0009-2940
    Keywords: [2.2.2]Paracyclophanes ; Polyenes ; Silver complexes ; X-Ray structural analysis ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The preparation of the disilver(I) complexes 3 and 4, polyene metal complexes that are terminally substituted with [2.2.2]paracyclophanyl units, is described. NMR spectro-scopic studies on the disilver perchlorate complex 3b showed that (a) the sites of complexation are the cyclophane groups and (b) the olefinic spacers do not overly perturb the overall complexation properties of the individual [2.2.2]paracyclo-phanyl groups. The crystal structures of the disilver hexafluo-roantimonate complexes 4a-b were determined. The use of the hexafluoroantimonate counterion and solvent mixtures containing toluene both proved crucial in obtaining single crystals; toluene is incorportated into the crystal lattices.
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    Highly Substituted Tris(pyrazolyl)methane Ligands and Some Zinc Complexes Thereof (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1095-1103 
    Details
    ISSN: 0009-2940
    Keywords: Zinc complexes ; Tridentate ligands ; Tris(pyrazolyl)methane ; Reactivity ; Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Tris(pyrazolyl)methane ligands in which two or three of the pyrazole carbon atoms bear organic substituents (L1-L7) were synthesized from chloroform and the corresponding pyrazole under phase transfer conditions. Their behavior towards zinc salts was found to span the range from no reaction at all to hydrolytic destruction. One hydrolysis product isolated and structurally characterized was the perchlorate complex [(HPz5)3Zn-OClO3]ClO4 (1), other ones were the 2:1 complexes (HPz3)2ZnBr2 (2) and (HPz6)2Zn(NO3)2 (3, HPzn = substituted pyrazole). Zinc perchlorate and tris(trimethylpy-razolyl)methane (L2) formed the octahedral binary complex [L22Zn](ClO4)2 (4) as evidenced by a structure determination. Zinc halides produced the 1:1 complexes L1 · ZnBr2 (5), L4 · ZnCl2 (6), and L4 · ZnBr2 (7), which according to the structure determinations of 6 and 7 contain tetrahedral ZnN2Hal2 units with only bidentate tris(pyrazolyl)methane ligands. In contrast, the zinc nitrate complex L4 · Zn(NO3)2 (8) was found to have an octahedral structure with mono- and bidentate nitrate and tridentate L4. The bromide complex 7 was converted by silver perchlorate hydrate into the labile compound [L4 · ZnBr]ClO4 (9) and then into the unstable product [L4 · Zn-OH2](ClO4)2 (10), both presumed to contain zinc in a tetrahedral ZnN3Br or ZnN3O environment, respectively. The ease of hydrolytic self-destruction prevented the exploitation of the reactivity of 9 and 10 in analogy to that of the corresponding tris(pyrazolyl)borate zinc complexes.
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    Unusual Complexation Behavior of Metallomacrocycles Based on Isothiosemicarbazides with Respect to Alkali and Alkaline Earth Metal Ions: Novel 2:1 Associates (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1089-1093 
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    ISSN: 0009-2940
    Keywords: Metallomacrocycles ; Nickel complexes ; Complexation reactions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reactions between alkali and alkaline earth metal ions and nickel(II) macrocycles based on S-alkylated isothiosemi-carbazides with different crown ether cavity size were studied in propylene carbonate by spectrophotometric and calorimetric titrations. Metallomacrocycles 1 and 2 exhibit normal behavior on 1:1 complexation with alkali- and alkaline earth metal ions and resemble in this respect 15C5 and 18C6, respectively. The most stable complexes are formed by these “ligands” when the diameter of the cation and the crown ether hole have approximately the same size. The most striking feature of the complexation processes studied is the formation of 1:2 metal-ligand associates even in the case of the smallest cations. These associates are very different from “normal” crown ether sandwich complexes. In reality, the particle formed is an associate between a 1:1 complex, in which the corresponding metal ion is well accommdated inside the ligand cavity, and a second metallomacrocyclic ligand. Their formation is disfavored by enthalpic contributions. A special kind of “switch” from these associates to normal sandwich complexes takes place in the case of 1, when the cation diameter compared to hole size increases. The macrocycle 2 forms this kind of associates with all akali and alkaline earth ions.
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    Synthesis and Reactivity of Silicon Transition Metal Complexes, 3433. Mitteilung: Lit.. Pentachlordisilanyl- und Disilanyl-Komplexe von Molybdän und Wolfram: Darstellung, Struktur und spektroskopische CharakterisierungHerrn Professor Hubert Schmidbaur zum 60. Geburtstag gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1109-1115 
    Details
    ISSN: 0009-2940
    Keywords: Silicon transition metal complexes ; Metallodisilanes ; Nucleophilic metallation ; Cl/H exchange at silicon ; Raman spectroscopy ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis and Reactivity of Silicon Transition Metal Complexes, 34[*].  -  Pentachlorodisilanyl and Disilanyl Complexes of Molybdenum and Tungsten: Synthesis, Structure, and Spectroscopic CharacterizationReaction of the lithium metallates Li[M(PMe3)(CO)2C5R5] [M = Mo, W; R = H (1a, b), Me (1c, d)] with Si2Cl6 (2) leads to the formation of the pentachloro(metallo)disilanes 5R5(OC)2(Me3P)M - SiCl2 - SiCl3 (3a - d), which are transformed into the metallo disilanes C5R5(OC)2(Me3P)M - SiH2 - SiH3 (4a - d) on treatment with LiAlH4. The disilanes 4a - d are reconverted into 3a - d in the presence of tetrachloromethane. Extensive spectroscopic investigations (NMR, Raman, and IR spectroscopy) were performed to establish the transition-metal effect especially with respect to the H5Si2 ligand. The molecular structure of C5Me5(OC)2(Me3P)W - SiCl2 - SiCl3 (3d) was determined by single-crystal X-ray diffraction.
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    Octacarbonylbis {μ-(tris(trimethylsilyl)methyl]indany l} dimanganese with Two Monoalkyl Indium Groups Bridging the Mn-Mn Bond (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1137-1139 
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    ISSN: 0009-2940
    Keywords: Tetraindane(4) ; Indium(I) ; Mn-Mn bond ; Indium alkyl bridge ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Tetrahedra-tetrakis[tris(trimethylsilyl)methyl]tetraindane(4) (1) reacts with decacarbonyldimanganese(0) to yield the bright red crystalline title compound 2, in which two carbonyl ligands are replaced by two InR fragments. The crystal structure determination of 2 shows two Mn(CO)4 groups (Mn-Mn 313.7 pm) bridged by two monoalkylindium units and a planar Mn2In2 molecular center.
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    Thioselonocarboxylic Ester, Selenetane, and Dihydrodiselenine Complexes Prepared from Pentacarbonyl(selenobenzaldehyde)tungsten with π-Donor-Substituted Alkynes (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1149-1156 
    Details
    ISSN: 0009-2940
    Keywords: Selenoaldehyde complex ; Thioselonocarboxylic ester complexes ; Selenetane complex ; Dihydrodiselenine complex ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Pentacarbonyltungsten-coordinated selenobenzaldehyde, [(CO)5W{Se=C(Ph)H}] (1), reacts with tBu-C≡C-SMe (2) by insertion of the C≡C into the Se=C bond to form in a highly regio- and stereoselective manner the α,β-unsaturated thioselonocarboxylic ester complex (Z)(C=C)-[(CO)5W{≡1-Se=C(SMe)C(tBu)=C(Ph)H}] (3). The thioselonocarboxylic ester ligand is cleaved intact from the metal by treatment of 3 with [NEt4]Br. Three complexes are formed in the reaction of 1 with Me-C≡C-SMe (5): the thioselonocarboxylic ester complex [(CO)5W{≡1-Se=C(SMe)C(Me)=C(Ph)H}] (6) as a mixture of the (E) and (Z)(C=C) isomers, a selenetane complex (7) and a dihydrodiselenine complex (8). The product distribution depends on the ratio 1:5 and on the solvent. The reaction of 1 with the bis(organylthio)alkynes RS-C≡C-SR (9) [R = Me (a), iPr (b), 2,6-C6H3Me2 (c)] yields mixtures of the (E) and (Z)(C=C) isomers of the α,β-unsaturated α-organylthio thioselonocarboxylic ester complexes [(CO)5W{≡1-Se=C(SR)C(SR)=C(Ph)H)] (10a-c). In contrast, the reaction of 1 with tert-butoxyethyne, H-C≡C-OtBu (11), affords a bis(pentacarbonyltungsten) 5,6-dihydro-1,2-diselenine complex (12). Compound 12 is probably formed by consecutive reaction of 1 with 11 to give the selonocarboxylic ester complex [(CO)5W{≡1-Se=C(OtBu)C(H)=C(Ph)H}] which then further reacts as a heterodiene by highly regioselective [4 + 2] cycloaddition with the Se=C bond of a second molecule of 1 to give 12. In the reaction of 1 with 5 and 9a the isomer with a trans arrangement of C(=Se)SMe and Ph is the kinetically controlled reaction product [(E)-6 and (Z)-10a, respectively]. The formation of (E)-6 and (Z)-10a is followed by isomerization until an (E)/(Z) equilibrium is reached. Complexes 3 and 7 were characterized by X-ray structural analyses.
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    Tin for Organic Synthesis, 13Part 12: Ref.. A New and Regioselective Method for the Synthesis of Aromatic, Heteroaromatic, and Olefinic Sulfonamides by Electrophilic Destannylation (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1195-1198 
    Details
    ISSN: 0009-2940
    Keywords: Electrophilic aromatic substitution ; Electrophilic vinylic substitution ; Trialkylstannanes, application of ; Sulfonamides, synthesis of ; Sulfodestannylation, application of ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A mild and effective method for the preparation of aromatic and olefinic sulfonamides is described. The reaction of trialkylaryl- (4a-f), heteroaryl- (4g), and vinylic stannanes (4h) with sulfuryl chloride and secondary amines provides the corresponding sulfonamides in an ipso-specific manner.
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    Ylidylphosphorsulfide, -selenide, -disulfide, -sulfidselenide und -diselenide (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1207-1219 
    Details
    ISSN: 0009-2940
    Keywords: Ylide-substituted phosphorus ; Phosphorus sulfides ; Phosphorus selenides ; Thioxophosphanes ; Selenoxo-phosphanes ; Dithioxophosphoranes ; Diselenoxophosphoranes ; Alkylation reactions ; Selenadiphosphirane ; 2,5,7-Triselena-1,3,4,6-tetraphosphanorbornane ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Ylidylphosphorus Sulfides, Selenides, Disulfides, Sulfide Selenides, and DiselenidesWe report on the first stable monomeric phosphorus mono-chalcogenides 2, 8 and the first stable dichalcogenides 4, 10 without bulky or intramolecularly coordinating substituents. They are stabilized by a high contribution of the zwitterionic resonance formula, which follows both from the NMR spectra and from an X-ray structure determination. Their preparation starts from triphenylphosphoniumylidyl-dichlorophosphanes 1. For the monochalcogenides they are treated with sodium sulfide or selenide or better with bis(trimethylsilyl) sulfide or selenide. In case of the C-phenyl and C-meta-tolyl representatives and also of the C-trimethylsilyl compound a number of secondary, partly novel products are obtained. - The dichalcogenides result from the reaction with sodium disulfide and diselenide, respectively, or from the oxidation of the monochalcogenides. - Alkylation of the monochalcogenides results in ylidylalkylchalcogenophosphenium salts 13, 15. In solution they are in equilibrium with more or less of the covalent form 14, 16, depending on the anion and on the solvent. Alkylation is often accompanied by secondary reactions. A diselenide loses selenium on alkylation.
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    Synthesis and Reactivity of Silicon Transition Metal Complexes, 3332. Mitteilung: Lit.. Metallo Silanols and Metallo Siloxanes, 87. Mitteilung: Lit.. Metallo-silanole vom Typ C5R5(OC)2(Me3P)M - SiPh2OH (M = Cr, Mo, W): Darstellung nach der Dimethyldioxiran-Methode und Überführung in funktionalisierte Metallo-disiloxaneHerrn Professor Max Schmidt zum 70. Geburtstag gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1251-1255 
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    ISSN: 0009-2940
    Keywords: Oxofunctionalization ; Dimethyldioxirane ; Metallo silanes ; Metallo silanols ; Metallo siloxanes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis and Reactivity of Silicon Transition Metal Complexes, 3332. Mitteilung: Lit. .  -  Metallo Silanols and Metallo Siloxanes, 8 7. Mitteilung: Lit. .  -  Metallo Silanols of the Type C5R5(OC)2(Me3P)M-SiPh2OH (M = Cr, Mo, W): Preparation According to the Dimethyldioxirane Route and Conversion into Metallo Disiloxanes Herrn Professor Max Schmidt zum 70. Geburtstag gewidmet.The metallo silanes C5R5(OC)2(Me3P)M-SiPh2H (4a-c), are converted into the corresponding metallo silanols C5R5(OC)2-(Me3P)M-SiPh2OH [R = H, M = Cr (6a); R = Me, M = Mo (6b); M = W (6c)] by oxofunctionalization with dimethyldioxirane (5). Treatment of 6b, c with the chlorosilanes Me2Si(R)Cl [R = H (3b), [R = Cl (3c)] in the presence of triethylamine gives access to the metallo disiloxanes C5Me5(OC)2(Me3P)M-SiPh2OSiMe2R (M = Mo, R = H (7a); M = W, R = Cl (7b)]. The structure of tungsten silanol 6c is determined by X-ray diffraction analysis.
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    Synthesis and Characterization of β-Phosphaenones An Investigation on the Conjugative Properties of the P=C Bond (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 465-476 
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    ISSN: 0009-2940
    Keywords: Phosphaalkenes, C-halo, C-metal ; Phosphaacrylic acid ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Thermally and air-stable β-phosphaenones were synthesized by functionalization of Mes*P=CCl2 (1; Mes* = supermesityl = 2,4,6-tri-tert-butylphenyl). At low temperature, 1 was lithiated by halogen-metal exchange with n-butyllithium to give the phosphanylidene carbenoid (Z)-Mes*P=C(Cl)Li [(Z)-2] which reacted with acid chlorides to furnish the C-carbonyl-substituted phosphaalkenes (Z)-Mes*P=C(Cl)R (3: P = COtBu; 4: R = COPh; 5: R = COOEt). The reaction of (Z)-2 with carbon dioxide furnished the carboxylate 6, which was converted by treatment with pivaloyl chloride or trimethylsilyl chloride into the phosphaalkenes 7 and 8 functionalized at the carbon atom by an anhydride or a trimethylsilyl ester function, respectively. Acidification of 6 or hydrolysis of 8 with water in chloroform solution afforded the novel carboxylic acid (Z)-Mes*P=C(Cl)COOH (9). Spectroscopic investigations (NMR, UV, IR) of 3-9 and the X-ray structures of 3 and 4 are presented. Based on these properties and on theoretical calculations, the occurrence of conjugation in the β-phosphaenone system is discussed and compared with the well-known conjugation in normal enones.
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    Reactions of Phosphaalkenes with HexafluoroacetoneDedicated to Professor H. M. R. Hoffmann on the occasion of his 60th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 499-502 
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    ISSN: 0009-2940
    Keywords: Phosphaalkenes ; Cycloadditions ; Insertion reactions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The dimethylamino-substituted phosphaalkene 1 reacts with hexafluoroacetone (HFA) with addition at the P=C bond to form the 1,5,2-dioxaphosphorinane 2. The structure of 2 was confirmed by an X-ray crystal structure analysis. The six-membered ring displays an envelope conformation with the phosphorus atom out of the plane, but the phosphorus is disordered over two sites. Reaction of P-trimethylsilyl-substituted phosphaalkenes with HFA proceeds with retention of the P=C double bond and insertion of HFA into the P—Si bond. Two isomeric products are obtained and are characterized by 1H-, 13C-, 19F-, and 31P-NMR spectroscopy, IR spectroscopy, mass spectrometry, and elemental analysis.
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    Monomere (Acetylacetonato)kupfer(I)-Komplexe von Alkinen und 1,4-Diinen (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 525-529 
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    ISSN: 0009-2940
    Keywords: Copper complexes ; Acetylacetonate ; Alkynes ; 1,4-Diynes ; Titanocenes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Monomeric (Acetylacetonato)copper(I) Complexes of Alkynes and 1,4-DiynesMonomeric (η2-Me3SiC≡CSiMe3)Cu(acac) (3) is formed by the reaction of dimeric [(η2-Me3SiC≡CSiMe3)CuBr]2 (1) with two equivalents of Na(acac) (2). In a similar manner Me2-Si(C≡CSiMe3)2 (4) reacts with CuCl (5) and 2 to afford Me2Si[(η2-C≡CSiMe3)Cu(acac)]2 (6). In compounds 3 and 6 an alkyne unit is η2-coordinated to a monomeric Cu(acac) moiety with a copper atom in a planar environment. With the organometallic 1,4-diyne (η5-C5H4SiMe3)2Ti(C≡CSiMe3)2 (7), compound [(η5-C5H4SiMe3)2Ti(C≡CSiMe3)2]Cu(acac) (8) is formed. In 8 both Me3SiC≡C ligands of the 3-titanapenta-1,4-diyne fragment are η2-coordinated to a monomeric Cu-(acac) building block. The copper atom in 8 possesses a pseudo-tetrahedral environment (shown by X-ray analysis), built by the two Me3SiC≡C ligands of the (η5-C5H4SiMe3)2-Ti(C≡CSiMe3)2 moiety and the two oxygen atoms of the acetylacetonato ligand. 8 is additionally formed by the reaction of 3 or 6 with 7, or by treatment of [(η5-C5H4SiMe3)2Ti(C≡C-SiMe3)2]CuCl (9) with Na(acac) (2). The application of 3, 6, and 8 as precursors for the preparation of copper films in the CVD process of copper(I) is discussed.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951280515
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  • 92
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    Chiral Organometallic Reagents, XIIIPart XII: Ref.. Structural Aspects of Differentially Solvated Benzyllithium Contact Ion Pairs (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 551-556 
    Details
    ISSN: 0009-2940
    Keywords: Benzyllithium compounds ; Ion pairs ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The solvation and ion pair nature of α-(phenylthio)benzyllithium (2d) in THF solution were investigated by NMR-spectroscopic methods. The effect of additives such as diethylene-glycol dimethyl ether or of 12-crown-4 was studied. The results were compared to those of benzyllithium compounds 4 and 6, containing a pentaoxapentadecane ansa chain. These compounds exist as contact ion pairs in which lithium is held at the anionic carbon. This is reflected in the 6Li,13C coupling and 1H,6Li-HOESY contacts in the NMR spectra.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280604
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  • 93
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    Sulfur Compounds, Part 186Part 185: K. Bergemann, M. Kustos, P. Krüger, R. Steudel, Angew. Chem., in print.. The Synthesis of Cyclic Organosulfur Compounds from (C5H5)4Ti2C2S4 by Ligand Transfer Reactions (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 561-564 
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    ISSN: 0009-2940
    Keywords: Titanocene complexes ; Organosulfur ligands ; Ligand transfer ; Organosulfur heterocycles ; Sulfur-sulfur bonds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The tetrathiaoxalate complex Cp4Ti2C2S4 (1) reacts with an equimolar amount of COCl2 to give the blue-green mononuclear complex Cp2TiC2S4CO (4). This reaction is analogous to the known reactions of 1 with SCl2 or S2Cl2. However, when 1 was treated with equimolar amounts of the bifunctional sulfenyl chlorides 1,2-C2H4(SCl)2 (5), 1,3-C3H6(SCl)2 (6) or 1,2-C6H4(SCl)2 (7), the bi- or monocyclic tetrakisdisulfanes C6H8S8 (9b), C8H12S8 (10), and C14H8S8 (11), respectively, were obtained. The X-ray crystal structure analysis of 11 · CS2 showed that 11 possesses Ci symmetry with a central exocyclic CC double bond similar to tetrathiafulvalenes: C6H4(μ-S2)2C=C(μ-S2)2C6H4.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951280606
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  • 94
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    Norbornadiene(bipyridyl)molybdenum(II) Complexes: Synthesis, Structure and Reactivity of [Mo(CO)(C7H8)(C10H6R2N2)X2] (X = I, Br)Dedicated to Professor Dr. Helmut Werner on the occasion of his birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1007-1013 
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    ISSN: 0009-2940
    Keywords: Tetracarbonyl(norbornadiene)molybdenum(0) ; Oxidative addition of I2 ; Dihalogeno(bipyridyl)molybdenum(II) complexes ; 7-Coordinated complexes ; Neutral and cationic molybdenum(II) complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of [Mo(CO)4(C7H8)] (1) with I2 gave the norbornadienemolybdenum(II) complex [Mo(CO)2(C7H8)I2]n≥1 (2), which existed in an equilibrium of two isomeric forms. In acetonitrile, 2 reversibly formed the adduct [Mo(CO)2-(C7H8)(NCCH3)I2] (3), whereas on treatment with 2,2′-bipyridine or 4,4′-di-2,2′-tBu-bipyridine, it gave stable 7-coordinated molybdenum(II) complexes, [Mo(CO)(C7H8)-(C10H8N2)I2] (4) and [Mo(CO)(C7H8)(C10H6tBu2N2)I2] (5), in good yield. In similar reactions, the related dibromomolybdenum compounds [Mo(CO)(C7H8)(C10H8N2)Br2] (6) and [Mo-(CO)(C7H8)(C10H6tBu2N2)Br2] (7) were prepared by oxidation of 1 with two equivalents of CuBr2. The X-ray structural analysis of 6 reveals that the geometry around the molybdenum atom is nearly perfectly pentagonal bipyramidal, with the CO and one of the bipyridyl rings perpendicular to the plane formed by the other ligands. The compounds 5 and 6 react with AgSbF6 by halogen abstraction to give cationic complexes, {[Mo(CO)(C7H8)(C10H8N2)Br]SbF6}n≥1 (8) and {[Mo(CO)(C7H8)(C10H6tBu2N2)I]SbF6}n≥1 (9): In acetone, 8 and 9 reversibly formed the adducts [Mo(CO)(C7H8)(C10H8N2)(acetone)Br]SbF6 (8′) and [Mo(CO)(C7H8)(C10H6tBu2N2)(acetone)I]SbF6 (9′); while on treatment with PMe3, the stable monomeric complexes, [Mo(CO)(C7H8)(C10H8N2)(PMe3)Br]SbF6 (10) and [Mo(CO)(C7H8)(C10H6tBu2N2)(PMe3)I]SbF6 (11), were isolated in almost quantitative yield. In the presence of KBr, compound 8′ reverted to the dibromo complex 6, whereas 9′ reacted to produce a 1:1:2 mixture of 5, 7 and the bromo(iodo) complex [Mo(CO)(C7H8)(C10H6tBu2N2)BrI] (12). The same mixture is available from the reaction of 5 with one equivalent of 7.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951281008
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    Graphical Abstract (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. A149 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951281018
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  • 96
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    Amino Substituted Tricarbonyl(cyclobutadiene)iron Complexes: Pd-Catalyzed Coupling of Iodocyclobutadiene Complexes with Amines (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1055-1058 
    Details
    ISSN: 0009-2940
    Keywords: Aminations ; Palladium catalysis ; Organometallic amines ; Coupling reactions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The coupling of the iodides 1 with amines under palladium catalysis affords the novel aminated cyclobutadiene derivatives 2 in preparative useful yields.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951281016
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  • 97
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    Masthead (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995) 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951281101
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  • 98
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    Chiral Carbanions, 1. Configurational Stability and Reactions of α-Acyloxy-Substituted α-Methylbenzyllithium Compounds (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1069-1077 
    Details
    ISSN: 0009-2940
    Keywords: Esters, 1-phenylethyl ; Carbanions, α-methyl-α-oxybenzyl, Configurational stability ; Ester - hydroxy ketone rearrangement ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Racemic and optically active 1-phenylethyl esters of pivalic, ( - )-camphanic and 2,4,6-triisopropylbenzoic acid were prepared. The esters 7a of pivalic acid were deprotonated with lithium 2,2,6,6-tetramethylpiperidide (Li-TMP) to form α-oxy-α-methylbenzyllithium compounds which are partly con-figurationally stable prior to acylation with starting material. Camphanic ester (-)-7b cannot be deprotonated by Li-TMP and tBuLi is added to the ester function to afford ketone (-)-12a. 1-Phenylethyl 2,4,6-triisopropylbenzoates 16 were transformed within minutes to carbanions 19 by using sBuLi/TMEDA in THF, hexane, toluene and sBuLi without TMEDA in toluene/20% diethyl ether at -78°C. The carbanions are configurationally stable only in toluene/20% diethyl ether and racemise partly in the other solvents. They react with a variety of electrophiles with either retention [MeOD, AcOD, (MeO)2CO, CICO2Me] or inversion (Me3SnCl) of configuration. Carbanions 19 rearrange on warming to -20°C to hydroxy ketone 24 with racemisation.
    Additional Material: 1 Tab.
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    URL: http://dx.doi.org/10.1002/cber.19951281103
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  • 99
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    Metal Complexes with Tetrapyrrole Ligands, LXIX. Facile Synthesis and 13C-NMR Spectrum of Dichloro(octaethylporphyrinato)zirconium(IV) (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1131-1133 
    Details
    ISSN: 0009-2940
    Keywords: Zirconium(IV) octaethylporphyrin complex ; Dichlorozirconium(IV) porphyrin complex ; Precursor of organometallic compounds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The synthesis of dichloro(2,3,7,8,12,13,17,18-octaethylpor-phyrinato)zirconium(IV), Zr(oep)Cl2, from zirconium tetrachloride and octaethylporphyrin, H2(oep), is described. The reported synthesis is a new and simple route to this precursor of organometallic compounds. Zr(oep)Cl2 was characterized by elemental analyses, 1H- and 13C-NMR, UV/Vis, and mass spectra. Hydrolysis yielded a mixture of mono- and binuclear hydroxy zirconium(IV) porphyrins.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951281112
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  • 100
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    Synthese und Bestimmung der absoluten Konfiguration des proximalen (S, S)-1,1′-Dimethyl-2,2′-spirobiindans (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 1902-1910 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Determination of the Absolute Configuration of the Proximal (S,S)-1,1′-Dimethyl-2,2′-spirobiindaneThe proximal (S,S)-1,1′-dimethyl-2,2′-spirobiindane (1a) is synthesized as the racemic mixture and with more then 98.5% optical purity. Its absolute configuration is determined by the path of synthesis. Key-steps are the trans-alkylation of 3 yielding 4a and the hydrogenolysis of the mixture of 10a and 10b yielding practically exclusively 1a. This is one of three possible diastereoisomers 1a-c which are needed to test the theory of hyperchirality.
    Notes: Das proximale (S,S)-1,1′-Dimethyl-2,2′-spirobiindan (1a) wird racemisch und zu mehr als 98.5% enantiomerenrein dargestellt. Seine absolute Konfiguration ist durch den Syntheseweg eindeutig bestimmt. Schlüsselschritte der Synthese sind die trans-Alkylierung von 3 zu 4a und die praktisch einheitlich verlaufende Hydrogenolyse des Gemisches von 10a und 10b zu 1a. Dieses ist eines von drei möglichen Diastereomeren 1a-c, die zum Test der Theorie der Hyperchiralität dienen sollen.
    Additional Material: 2 Tab.
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    URL: http://dx.doi.org/10.1002/cber.19821150520
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