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  • 1
    Electronic Resource
    Electronic Resource
    Komplexchemie reaktiver organischer Verbindungen, XIV. Das Reaktionsverhalten aliphatischer Diazoverbindungen gegenüber Tricarbonyl(cyclopentadienyl)hydridomolybdän und -wolfram (1977)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 110 (1977), S. 896-915 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Complex Chemistry of Reactive Organic Compounds, XIV. The Reactions of Aliphatic Diazo Compounds with the Tricarbonyl(cyclopentadienyl) Hydrides of Molybdenum and TungstenDepending on their constitution, aliphatic diazo compounds 3 behave differently in their reactions with tricarbonyl(cyclopentadienyl)hydridomolybdenum (1) and -tungsten (2). Diazomethane (3a), diazoethane (3b), and 2-diazopropane (3c) are stabilized as alkane diazo ligands in complexes of the type C5H5M(CO)2[N2CHR1R2] (M = Mo: 6; M = W: 7). Phenyl-, (4-nitrophenyl)-, (4-methoxyphenyl)diazomethane (3d, e, f), and 9-diazofluorene (3g) form in clean reactions the carbene insertion products C5H5M(CO)3CHR1R2 (M = Mo: 4; M = W: 5), whereas ω-diazoacetophenone (3h) and diazodimedone (3i) yield the binuclear diazo complexes C5H5M(CO)3-M(CO)2C5H5[N2 = CR1R2] (M = Mo: 9; M = W: 10). Diethyl diazomalonate (3h) is coordinated as an imino-amido ligand in the coordination compound 14 which arises from a 1,1-insertion of 3k into the polar tungsten-hydrogen bond of 2.
    Notes: In ihrer Reaktivität gegenüber Tricarbonyl(cyclopentadienyl)hydridomolybdän (1) und -wolfram (2) weisen Diazoalkane 3 starke konstitutionsbedingte Unterschiede auf: Diazomethan (3a), Diazoethan (3b) und 2-Diazopropan (3c) werden als Alkandiazo-Liganden in Komplexen vom Typ C5H5M(CO)2[N2CHR1R2] (M = Mo: 6; M = W: 7) stabilisiert; Phenyl-, (4-Nitrophenyl)-, (4-Methoxyphenyl)diazomethan (3d, e, f) sowie 9-Diazofluoren (3g) bilden in glatten Reaktionen die Carben-Insertionsprodukte C5H5M(CO)3CHR1R2 (M = Mo: 4; M = W: 5), während ω-Diazoacetophenon (3h) wie auch Diazodimedon (3i) die zweikernigen Diazoketon-Komplexe C5H5M(CO)3-M(CO)2C5H5[N2 = CR1R2] (M = Mo: 9; M = W: 10) ergeben. Diazomalonsäure-diethylester (3k) wird im Zuge einer zur Koordinationsverbindung 14 führenden 1,1-Insertion in die polare Wolfram-Wasserstoff-Bindung von 2 als Imino-amido-Ligand komplexiert.
    Additional Material: 8 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19771100310
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  • 2
    Electronic Resource
    Electronic Resource
    Syntheses of Metal Carbonyls, XVI1). Metal-Metal Multiple Bonds: Synthesis, Crystal and Molecular Structure of Tri-μ-carbonyl-bis[(η5-pentamethylcyclopentadienyl)manganese](Mn ≡ Mn) - The First Manganese-Manganese Triple Bond (1984)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 117 (1984), S. 434-444 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Metallcarbonyl-Synthesen, XVI1). Metall-Metall-Mehrfachbindungen: Synthese, Molekül- und Kristallstruktur von Tri-μ-carbonylbis([η5-pentamethylcyclopentadienyl)mangan](Mn ≡ Mn) - die erste Mangan-Mangan-DreifachbindungPhotolyse des Halbsandwich-Mangan-Komplexes (η5-C5Me5)Mn(CO)3 (1) in Tetrahydrofuran (THF) führt ohne Nebenreaktionen zum Solvenskomplex (η5-C5Me5)Mn(CO)2(THF) (2). Dieser ist im festen Zustand im deutlich unter 0°C liegenden Temperaturbereich haltbar, erleidet aber spontane CO-Eliminierung bei Raumtemperatur; dabei bildet sich der neue Zweikernkomplex (η5-C5Me5)2Mn2(μ-CO)3 (3). Während Elementaranalyse, Infrarot- und Massenspektren sowie die 1H- und 13C-NMR-Spektren dieser Verbindung eine hochsymmetrische dreifach Carbonylverbrückte Struktur zuweisen, stützt eine Einkristall-Röntgenstrukturanalyse das Vorliegen der ersten bisher bekannten Mangan-Mangan-Dreifachbindung (dMn - Mn 217.0(1) pm). Eine verbesserte Darstellung von Tricarbonyl(η5-pentamethylcyclopentadienyl)mangan (1) wird beschrieben.
    Notes: Photolysis of the manganese half-sandwich complex (η5-C5Me5)Mn(CO)3 (1) in tetrahydrofuran (thf) cleanly yields the solvent complex (η5-C5Me5)Mn(CO)2(thf) (2). Compound 2 is stable as solid at temperatures well below 0°C but undergoes spontaneous elimination of carbon monoxide at ambient temperature with concomitant formation of the novel dinuclear complex (η5-C5Me5)2-Mn2(μ-CO)3 (3). While elemental analysis, infrared and mass spectroscopy as well as the 1H NMR and 13C NMR spectra unequivocally demonstrate this compound to adopt a highly symmetrical triply carbonyl-bridged structure, a single-crystal X-ray diffraction study supports the presence of the first triple bond between manganese atoms (dMn - Mn 217.0(1) pm). An improved synthesis of tricarbonyl(η5-pentamethylclopentadienyl)manganese (1) is also described.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19841170203
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  • 3
    Electronic Resource
    Electronic Resource
    Übergangsmetall-Methylen-Komplexe, XLIII. Drei- und viergliedrige Dimetallacyclen mit Schwefeldioxid, Selen, Chlorogold und einem Silberdiazoalkan als Molekülbausteinen (1984)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 117 (1984), S. 1271-1286 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Transition Metal Methylene Complexes, XLIII. Three- and Four-membered Dimetallacycles Having Sulfur Dioxide, Selenium, Chlorogold, and a Silver Diazoalkane as Molecular Building BlocksAs a very good π-ligand, sulfur dioxide adds under mild conditions (-80… +25°C) in fast and clean reactions to metal-metal double bonds with formation of stable 1:1 adducts that exhibit bridging sulfur dioxide ligands. Starting from the doubly bridged metal-metal double bonds of the dinuclear organorhodium- and -cobalt complexes 1a, b, 3, and 5, the novel μ-SO2 complexes 2a, b, 4, and 6, respectively, are formed. In some of these reactions, the coordination mode of the former bridging ligands changes to terminal. The first known μ-(thioformaldehyde S,S-dioxide-C,S) complexes 8a, b are achieved by means of clean electrophilic ring expansion reactions when sulfur dioxide inserts into the μ-methylene complexes 7a and 7b, respectively. Elemental selenium (9a), carbonyl(chloro)gold (9b), and the silver diazoalkane 9c form the three-membered metallacycles 10a - c upon treatment with 1a.
    Notes: Schwefeldioxid addiert sich als vorzüglicher π-Ligand unter schonenden Reaktionsbedingungen (-80… +25°C) rasch und übersichtlich an Metall-Metall-Doppelbindungen unter Bildung beständiger 1:1-Addukte, in denen stets SO2-Brücken vorliegen. Ausgehend von den zweifach verbrückten Metall-Metall-Doppelbindungen der zweikernigen Organorhodium- und cobalt-Komplexe 1a, b, 3 und 5 entstehen unter teilweiser Konstitutionsisomerisierung der Brückenliganden die neuen μ-SO2-Komplexe 2a, b, 4 bzw. 6. Durch glatt verlaufende elektrophile Ringerweiterungsreaktionen der μ-Methylen-Komplexe 7a, b sind die ersten μ-(Thioformaldehyd-S,S-dioxid-C,S)-Komplexe 8a, b zugänglich. Mit elementarem Selen (9a), Carbonyl(chloro)gold (9b) und dem Silberdiazoalkan 9c bildet 1a die dreigliedrigen Ringsysteme 10a - c.
    Additional Material: 3 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19841170403
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  • 4
    Electronic Resource
    Electronic Resource
    Notiz zur Darstellung von Tricarbonyl(cyclopentadienyl)-(p-toluolsulfonamido)wolfram (1976)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 109 (1976), S. 3489-3491 
    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.19761091029
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  • 5
    Electronic Resource
    Electronic Resource
    Übergangsmetall-Methylen-Komplexe, IV: Neue Methylen-Cobalt-Komplexe (1978)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 111 (1978), S. 1077-1082 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Transition Metal Methylene Complexes, IV: Novel Methylene Cobalt ComplexesDicarbonyl(η-cyclopentadienyl)cobalt (2) reacts with ethyl diazoacetate (3a), tert-butyl diazoacetate (3b), dimethyl diazomalonate (3c), and diethyl diazomalonate (3d) in boiling benzene to yield the dinuclear diamagnetic complexes [η-C5H5Co(CO)]2-μ-[C(R)(CO2R′)] (R = H, R′ = C2H5; 4a; R = H, R′ = tert-C4H9: 4b: R = CO2CH3, R′ = CH3: 5a: R = CO2C2H5, R′ = C2H5: 5b) in which the carbenes corresponding to 3a-d are stabilized as bridging ligands.
    Notes: Dicarbonyl(η-cyclopentadienyl)cobalt (2) reagiert mit Diazoessigsäure-ethylester (3a). Diazoessigsäure-tert-butylester (3b). Diazomalonsäure-dimethylester (3c) bzw. Diazomalonsäurediethylester (3d) in siedendem Benzol unter Bildung der zweikernigen diamagnetischen Komplexe [η-C5H5Co(CO)]2-μ-[C(R)(CO2R′)] (R = H, R′ = C2H5; 4a; R = H, R′ = tert-C4H9: 4b: R = CO2CH3, R′ = CH3: 5a: R = CO2C2H5, R′ = C2H5: 5b), in denen die 3a-d entsprechenden Carbene als Brückenliganden stabilisiert sind.
    Additional Material: 3 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19781110326
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  • 6
    Electronic Resource
    Electronic Resource
    Komplexchemie reaktiver organischer Verbindungen, XXII1) Metallorganische Cyclopentadienylierungen mit Diazocyclopentadienen. Synthesen von (η-Halogencyclopentadienyl)eisen-Komplexen (1978)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 111 (1978), S. 3124-3135 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Complex Chemistry of Reactive Organic Compounds, XXII: Organometallic Cyclopentadienylations with Diazocyclopentadienes. Syntheses of (η-Halocyclopentadienyl)iron ComplexesThe tetracarbonyliron halides (CO)4Fe(σ-C3F7)I (2) and (CO)4FeX2 [X = Br: 4; X = I: 5] react with diazocyclopentadiene (1a) and its derivatives 1b-e to yield (η-monohalocyclopentadienyl)iron complexes (η-C5R4X)Fe(CO)2L (3a-d, 6a, b, 8) [R = H, Cl, Br, C6H5; X = Br, I; L = C3F7, Br, I] and 1,1′-dibromoferrocene (7a). In addition to the analytical and spectroscopic characterization, the constitution of (η-C5H4I)Fe(CO)2I (6b) has been proved chemically.
    Notes: Die Tetracarbonyleisen-halogenide (CO)4Fe(σ-C3F7)I (2) und (CO)4FeX2 [X = Br: 4; X = 1: 5] reagieren mit Diazocyclopentadien (1a) und seinen Derivaten 1b-e unter Bildung der (η-Monohalogencyclopentadienyl)eisen-Komplexe (η-C5R4X)Fe(CO)2L (3a-d, 6a, b, 8) [R = H, Cl, Br, C6H5;X = Br, I;L = C3F7, Br, I] und von 1,1′-Dibromeferrocen (7a). Über die analytische und spektroskopische Charakterisierung der Produkte hinaus ist die Konstitution von (η-C5H4I)Fe(CO)2I (6b) auch chemisch bewiesen.
    Additional Material: 2 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19781110913
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  • 7
    Electronic Resource
    Electronic Resource
    Metallcarbonyl-Synthesen, III. Eine ergiebige Hochdrucksynthese von Tetracarbonyl(η5-cyclopentadienyl)niob, (η5-C5H5)Nb(CO)4 (1979)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 112 (1979), S. 3942-3945 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Syntheses of Metalcarbonyls, III. A Productive High-Pressure Synthesis of Tetracarbonyl(η5-cyclopentadienyl)niobium, (η5-C5H5)Nb(CO)4Tetracarbonyl(η5-cyclopentadienyl)niobium (1), which could hitherto be prepared only in small amounts, can be synthesized with reproducible yields by reductive high-pressure carbonylation of (η5-C5H5)2NbCl2 (2) on a 5 - 20 g scale.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19791121219
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  • 8
    Electronic Resource
    Electronic Resource
    Metallcarbonyl-Synthesen, XII. Tetracarbonyl(η5-pentamethylcyclopentadienyl)vanadium (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 3886-3889 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Metalcarbonyl Syntheses, XII. Tetracarbonyl(η5-pentamethylcyclopentadienyl)vanadiumThe hitherto unknown halfsandwich complex tetracarbonyl(η5-pentamethylcyclopentadienyl)vanadium (3) is easily accessible in 45% yield upon reaction of hexacarbonylvanadium (1) with pentamethylcyclopentadiene (2). Photolysis of 3 as well as reduction and subsequent protonation yield the dinuclear derivative 4 of composition (η5-C5Me5)2V2(CO)5.
    Additional Material: 1 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19821151220
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  • 9
    Electronic Resource
    Electronic Resource
    Übergangsmetall-Methylen-Komplexe, XLII. Formylmethylen-Brücken in Eisen-, Cobalt- und Rhodium-Komplexen (1984)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 117 (1984), S. 69-78 
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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 Methylene Complexes, XLII. Formylmethylene Bridges in Iron, Cobalt, and Rhodium ComplexesThe formyl-substituted dimetallacyclopropanes 3a - c are cleanly formed upon reaction of formyldiazomethane (α-diazoacetaldehyde; 1) with the metal-metal double bonded dinuclear iron, cobalt, and rhodium complexes 2a - c. The molecular structure of these compounds was elucidated in case of the rhodium derivative 3c by X-ray diffraction.
    Notes: Formyldiazomethan (α-Diazoacetaldehyd; 1) reagiert mit den zweikernigen, Metall-Metall-Doppelbindungen aufweisenden Eisen-, Cobalt- und Rhodium-Komplexen 2a - c) ohne Nebenreaktionen unter N2-Eliminierung zu den formylsubstituierten Dimetallacyclopropanen 3a - c), deren Geometrie für das Rhodium-Derivat 3c durch Kristallstrukturanalyse ermittelt wurde.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19841170106
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  • 10
    Electronic Resource
    Electronic Resource
    Metallcarbonyl-Synthesen, XIV. Neuartige Vanadium-, Niob- und Tantal-Komplexe mit Wasserstoff-Brücken (1984)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 117 (1984), S. 79-94 
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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: Syntheses of Metal Carbonyls, XIV. Novel Vanadium, Niobium, and Tantalum Complexes Having Hydrido BridgesThe novel homo- and heterodinuclear organometallic μ-hydrido compounds 3a - c of vanadium, niobium, and tantalum have been synthesized by light-induced reactions of the hydridoniobium complex (η5-C5H5)2NbH3 (1) with the half-sandwich complexes (η5-C5H5)M(CO)4 (2a: M = V; 2b: M = Nb; 2c: M = Ta). These compounds have the general composition LxM - H - Nb(CO)(η5-C5H5)2. The formation of the M - H - Nb moieties is a dark-reaction preceded by two photoreactions that are independent from each other elimination of CO from 2a - c and elimination of H2 from 1, with the extruded carbon monoxide being transfered to the (η5-C5H5)2NbH fragment; subsequent fixation of the species (η5-C5H5)2Nb(CO)H thus generated to the photogragments (η5-C5H5)M(CO)3 results in donor stabilization of these latter groups. The structural architecture of the derivatives 3a und b was established by X-Ray diffraction. The hydrogen bridges are to be considered as three-center two-electron functions that are responsible for a serious lengthening of the otherwise by at least 40 pm shorter metal-to-metal distances amounting to 371.3 pm in 3a and 373.3 pm in 3b (mean values).
    Notes: Die neuartigen, dem Verbindungstyp LxM - H - Nb(CO)(η5-C5H5)2 zugehörigen homo- und heterodinuclearen Hydrid-verbrückten Organometall-Verbindungen 3a - c der Metalle Vanadium, Niob und Tantal wurden lichtinduziert aus dem Hydridoniob-Komplex (η5-C5H5)2NbH3 (1) und den Halbsandwich-Komplexen (η5-C5H5)M(CO)4 (2a: M = V; 2b: M = Nb; 2c: M = Ta) synthetisiert. Dem als Dunkelreaktion ablaufenden Aufbau der M - H - Nb-Systeme gehen zwei voneinander unabhängige Photoreaktionen voraus: CO-Eliminierung aus 2a - c sowie H2-Eliminierung aus 1, wobei das freigesetzte Kohlenmonoxid auf das (η5-C5H5)2NbH-Fragment übertragen wird; durch die nachfolgende Fixierung der so erzeugten Spezies (η5-C5H5)2Nb(CO)H an die Photofragmente (η5-C5H5)M(CO)3 kommt es zu deren Donor-Stabilisierung. Die Geometrie der beiden Derivate 3a und b wurde durch Röntgenstrukturanalysen ermittelt. Die Wasserstoff-Brücken sind als 3z,2e-Funktionen aufzufassen, die eine starke Aufweitung der sonst um mindestens 40 pm kürzeren Metall-Metall-Abstände auf durchschnittlich 371.3 pm (3a) bzw. 373.3 pm (3b) verursachen.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19841170107
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