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  • 1
    Digitale Medien
    Digitale Medien
    Synthesis and Crystal Structure of a Monomeric Tetraalkyldigallium Telluride with a Bent Ga-Te-Ga Group (1995)
    s.l. : American Chemical Society
    Organometallics 14 (1995), S. 1073-1075 
    Details
    ISSN: 1520-6041
    Quelle: ACS Legacy Archives
    Thema: Chemie und Pharmazie
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1021/om00002a065
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  • 2
    Digitale Medien
    Digitale Medien
    Aluminium Hydrazides: Reactions of tert-Butylaluminium Chlorides with Dilithium Bis(trimethylsilyl)hydrazide - Formation of Iminoalanes and their Hydrazido Adducts (1999)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 1999 (1999), S. 2021-2027 
    Details
    ISSN: 1434-1948
    Schlagwort(e): Aluminium ; Hydrazides ; Alanes ; Lithium ; Imino compounds ; Chemistry ; General Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Di(tert-butyl)aluminium chloride reacted with dilithium bis(trimethylsilyl)hydrazide with the formation of a novel Al2Li2N4 cage compound 1. Its structure consists of a dimeric iminoalane RAl(μN-SiMe3)2AlR (R = CMe3), which is bridged by a dilithiumhydrazido ligand with an intact N-N bond. A heterocubane-type molecule is formed, in which two vertices are occupied by Al atoms, two by Li atoms and four by N atoms. One face of the cube is strongly distorted due to the short N-N distance of the hydrazido group. A similar compound, 3, was formed with bis(neopentyl)aluminium chloride but it was isolated in very poor yield. The reaction of Li2N2(SiMe3)2 with (Me3C)2AlCl in the presence of THF yielded an adduct 2, in which each Li atom of the cage is additionally coordinated via Li-Cl-Al bridges to the ligand (Me3Al)2Cl·THF. The reaction of dilithium bis(trimethylsilyl)hydrazide with tert-butylaluminium dichloride gave, by complete cleavage of the hydrazido groups, a dimeric iminoalane [Me3C(THF)AlNSiMe3]2 (4), in which each aluminium atom is coordinated to one THF molecule. Its uncoordinated, solvent-free form 5 was obtained by heating solid 4 to 150 °C in vacuo for several hours. It was identified as the tetrameric iminoalane (Me3CAlNSiMe3)4, which does not adopt the expected heterocubane-type structure, but consists of three anellated four-membered Al2N2 heterocycles in a kind of ladder structure. Remarkably, the cage compound 1 could not be obtained by the reaction of an excess of lithium hydrazide with the iminoalanes 4 and 5. All compounds 1-5 were characterized by crystal structure determinations.
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
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  • 3
    Digitale Medien
    Digitale Medien
    The Reactions of R2Ga-GaR2 and R2In-InR2 [R = CH(SiMe3)2] with Protic Reagents: Substituent Exchange versus Cleavage of the Element-Element Bond (1998)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 1998 (1998), S. 355-360 
    Details
    ISSN: 1434-1948
    Schlagwort(e): Gallium ; Indium ; Low-valent compounds ; Chemistry ; General Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Tetrakis[bis(trimethylsilyl)methyl]digallane(4) (1) with a Ga-Ga single bond and the corresponding diindane(4) 2 with an In-In single bond were treated with different protic reagents: tert-Butyl alcohol did not react with 1 at all, while phenol gave a mixture of unknown products, which could not be separated. The more acidic pentafluorophenol did not react as an acid, but C-F bonds were cleaved to form almost quantitatively the dimer (R2GaF)2 5, which was characterized by a crystal-structure determination. Water and 1 yielded the dimeric dialkylgallium hydroxide 6. The Ga-Ga bond was also cleaved by the reaction of 1 with durylthiophenol (duryl = 2,3,5,6-tetramethylphenyl), which gave two main products: R2Ga(SDuryl) 7 and RGa(SDuryl)2 8. In contrast, the chelating acid dibenzoylmethane reacted by means of a substituent exchange, with the release of two equiv. of bis(trimethylsilyl)methane for each formula unit of 1, to form 9, in which the Ga-Ga bond is retained and each chelating 1,3-diphenyl-1,3-propanedionato ligand is in a terminal position bonded to only one Ga atom, in more than 80% yield. The Ga-Ga bond is shortened [244.1(1) pm] compared to that in the starting compound tetraalkyldigallane(4) 1. The In-In bond of diindane(4) 2 is, however, cleaved in a similar reaction with dibenzoylmethane, and only the fragmentation product dialkyl(1,3-diphenyl-1,3-propanedionato)indium 10 could be isolated.
    Materialart: Digitale Medien
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  • 4
    Digitale Medien
    Digitale Medien
    A Methylene-Bridged Dialuminium Compound as a Chelating Lewis Acid: Complexation of Nitrite and Nitrate Anions by R2Al-CH2-AlR2[R = CH(SiMe3)2]⋆ (1998)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 1998 (1998), S. 921-926 
    Details
    ISSN: 1434-1948
    Schlagwort(e): Aluminium ; Chelates ; Lewis acids ; Chemistry ; General Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Sodium nitrite (NaNO2) dissolves readily in THF, when the methylene-bridged dialuminium compound R2Al-CH2-AlR2 [R = CH(SiMe3)2] 1 with two coordinatively unsaturated aluminium atoms is added. Compound 1 reacts as a chelating Lewis acid, and, as shown by a crystal structure deter-mination of the [Na([18]crown-6)(Et2O)]+ derivative 5c, a compound (5) is formed, in which one oxygen atom and the nitrogen atom of the nitrite ion are each coordinated by one aluminium atom to form a five-membered Al2CNO hetero-cycle. The second oxygen atom of the nitrite anion is not affected. Similarly, lithium nitrate (LiNO3) reacts with 1 to yield a THF soluble product (6a). Single crystals were obtain-ed of the [Li(N,N′,N′′-trimethyltriazinane)2]+ derivative 6c, whose structure shows each aluminium atom to be coordinated by one oxygen atom of the nitrate ion to give a six-membered Al2CNO2 heterocycle.
    Materialart: Digitale Medien
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  • 5
    Digitale Medien
    Digitale Medien
    The Formation of Macrocyclic Compounds Containing Two Ga-Ga Bonds by the Reaction of Tetraalkyldigallane(4) R2Ga-GaR2 [R = CH(SiMe3)2] with Dicarboxylic Acids (1998)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 1998 (1998), S. 1661-1665 
    Details
    ISSN: 1434-1948
    Schlagwort(e): Gallium ; Low-valent compounds ; Macrocycles ; Chemistry ; General Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Tetrakis[bis(trimethylsilyl)methyl]digallane(4) 1 reacts with dicarboxylic acids like 1,4-benzenedi(methylcarboxylic) acid, 1,4-cyclohexanedicarboxylic acid, 1,6-hexanedicarboxylic acid, and 1,4-butanedicarboxylic acid (adipinic acid) by the release of two equivalents of bis(trimethylsilyl)methane and the retention of the Ga-Ga bond. Products are formed, in which the very short Ga-Ga bonds (237.7 pm on average) are bridged by two carboxylato groups. Two of these moieties are connected in each compound by two spacers (dimethylbenzene, cyclohexane, hexane, or butane) to form macrocyclic compounds with up to 22 atoms in the resultant heteroatomic rings. The dimeric form is also observed in solution. For comparison, the synthesis and structure of the product of the reaction of 1 with 1-adamantanecarboxylic acid is included, which also has the Ga-Ga bond (239.1 pm) bridged by two carboxylato groups.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 6
    Digitale Medien
    Digitale Medien
    The Reaction of Diazomethane Derivatives with the Dielement Compounds R2Al-AlR2 and R2Ga-GaR2 [R = CH(SiMe3)2] - Insertion versus Fragmentation (1999)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 1999 (1999), S. 201-207 
    Details
    ISSN: 1434-1948
    Schlagwort(e): Aluminium ; Gallium ; Low-valent compounds ; Insertion reactions ; Chemistry ; General Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Tetrakis[bis(trimethylsilyl)methyl]dialane(4) 1 reacted with trimethylsilyldiazomethane and bis(trimethylsilyl)diazomethane at room temperature by the insertion of the terminal nitrogen atoms into its aluminium-aluminium bond. As shown by a crystal structure determination, one of the aluminium atoms of each product enhanced its coordination number to four by the interaction with the central nitrogen atom of the C=N-N group, which results in the formation of a three-membered AlN2 heterocycle bearing an exocyclic N=C double bond. The reactions of the corresponding gallium compound (2) containing a gallium-gallium single bond needed more drastic conditions. Mixtures of many unknown products were formed, and only on treatment with trimethylsilyldiazomethane two compounds could be isolated after repeated recrystallization in yields below 10%, which were characterized by crystal structure determinations. One was identified as the trimeric dialkylgallium cyanide (8) with a nine-membered Ga3C3N3 heterocycle, and the other one (9) has a dialkylgallium fragment coordinated by both terminal nitrogen atoms of the chelating ligand NH2-N=C(SiMe3)-NH-. Due to the NMR spectroscopic characterization, 8 seems to be tetrameric in solution with an asymmetric structure containing four different gallium atoms. With this unusual structure, the IR spectrum of tetrameric dimethylgallium cyanide could now completely be interpreted, which was published more than 20 years ago.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 7
    Digitale Medien
    Digitale Medien
    Diazomethane Derivatives Bearing Dialkylaluminium or DialkylgalliumSubstituents - The Isomeric Diazomethane and Nitrile Imine Structures Realized by the Different Coordination Behavior of Aluminium and Gallium (1999)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 1999 (1999), S. 771-776 
    Details
    ISSN: 1434-1948
    Schlagwort(e): Aluminium ; Gallium ; Diazo compounds ; Dimerization ; Coordination modes ; Chemistry ; General Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Lithium trimethylsilyldiazomethanide Li(SiMe3)CN2 reacted with the dialkylaluminium or -gallium halides R2AlCl and R2GaBr [R = CH(SiMe3)2] by the elimination of lithium halide and the formation of the corresponding aluminium or gallium diazo compounds. As shown by a crystal structure determination, the gallium derivative 1 adopts the nitrile imine structure, in which the gallium atom is coordinated by the terminal nitrogen atom of the diazo group. The N-N-C-Si moiety is almost ideally linear with N-N and C-N bond lengths of 125.5 and 115.9 pm on average. In contrast, the diazomethane structure was formed with dialkylaluminium chloride, and the aluminium atom in 2 is attached to the carbon atom of diazomethane. The almost linear N-N-C group (174.1°) has N-N and N-C distances of 120.0 and 126.4 pm, respectively, inverse to that of the gallium derivative. The bonding situations can best be described by the resonance structures R-C≡N+-N--GaR2 for 1 and R2Al-(R)C=N+=N- for 2. The nitrile imine isomer of the aluminium compound could be detected by NMR spectroscopy as a by-product. Both compounds gave dimers in the solid state, a Ga2N2 four-membered heterocycle was formed of 1, while an eight-membered Al2C2N4 heterocycle resulted with 2.
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 8
    Digitale Medien
    Digitale Medien
    Aluminium Atoms at High Connectivity Sites in Polyhedral Polyborane Analogous Clusters: From Aluminaboranes to Carbaalanes (2000)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 2000 (2000), S. 1-11 
    Details
    ISSN: 1434-1948
    Schlagwort(e): Carbaalanes ; Cluster compounds ; Electron deficiency ; Aluminium ; Boron ; Chemistry ; General Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Cluster chemistry in the third main group has long been restricted to compounds of the lightest element boron. However, about 30 years ago the first compounds were synthesized and characterized in which single aluminium atoms adopted positions of high connectivity in polyhedral borane or carbaborane clusters. The next successful step in these efforts to establish a chemistry analogous to that of the polyboranes with the heavier elements of the third main-group was the synthesis of closo-dodecaaluminate [Al12iBu12]2- at the beginning of the nineties, which was the first homonuclear aluminium analogue of a polyborate anion and had a core exclusively formed by aluminium atoms. Another class of interesting new aluminium compounds was formed by the carbaalanes, which were synthesized and characterized for the first time only recently. They have clusters of aluminium and carbon atoms, and are similar to the carbaborane analogues in that their structures seem to be determined by the number of electron pairs in their molecular centers in accordance with the Wade rules.
    Zusätzliches Material: 9 Ill.
    Materialart: Digitale Medien
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  • 9
    Digitale Medien
    Digitale Medien
    Acyl- und Alkylidenphosphane. X. Synthese des Phenyl-bis(trimethylsilylsulfano)methyliden phosphans (1980)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 463 (1980), S. 144-148 
    Details
    ISSN: 0044-2313
    Schlagwort(e): Chemistry ; Inorganic Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Beschreibung / Inhaltsverzeichnis: Acyl and Alkylidene Phosphines. X. Synthesis of Phenyl-bis(trimethylsilylsulfano)- methylidene PhosphineCarbon disulfide 1 reacts with Phenylbis(trimethylsilyl)phosphine 2 to form crystalline phenyl-bis(trimethylsilylsulfano)methylidene phosphine 4. A red colour of the solution indicates the intermediate formation of the unstable 1:1 adduct 3. The NMR-data of 4 are discussed and compared with those of similar compounds.
    Notizen: Kohlenstoffdisulfid 1 reagiert mit Phenylbis(trimethylsilyl)Phosphan 2 zum kristallinen Phenyl-bis(trimethysilylsulfano)methylidenphosphan 4. Eine kurzzeitig auftretende Rotfärbung der Lösung weist auf die Bildung des instabilen 1:1 Adduktes 3 hin. Die NMR-Daten von 4 werden diskutiert und mit den Werten aus ähnlichen Verbindungen verglichen.
    Zusätzliches Material: 1 Tab.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1002/zaac.19804630120
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  • 10
    Digitale Medien
    Digitale Medien
    Acyl- und Alkylidenphosphane. XVI. (Dimethylaminomethyliden)- und (Diphenylmethyliden)phosphane (1981)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 479 (1981), S. 41-56 
    Details
    ISSN: 0044-2313
    Schlagwort(e): Chemistry ; Inorganic Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Beschreibung / Inhaltsverzeichnis: Acyl- and Alkylidenephosphines. XVI. (Dimethylaminomethylidene)- and (Diphenylmethylidene) phosphinesAlkyl- or arylbis(trimethylsilyl)phosphines 1 (R = mesityl, C9H11 a; (CH3)3C b; C6H5 c; CH3 d) react only very slowly with dimethylformamide 2 and benzophenone 4. After repeated addition of small amounts of solid sodium hydroxide, however, the reaction-time is shortened from several months to a few days. The reactions between 1 a or 1 b and 2 yield the (dimethylaminomethylidene)phosphines 3 a and 3 b; from 1 a and 4 mesityl-(diphenylmethylidene)phosphine 5 a is obtained. The formation of the thermally labile phosphines 3 d and 5 c is proved by NMR spectroscopy; these compounds dimerize very fast to give 2,4-bis(dimethylamino)-1,3-dimethyl- 10 d and 1,2,2,3,4, 4-hexaphenyl-1,3-diphosphetane 15 c. Similarly the lithium trimethylsilylphosphides 6 a, 6 c and 6 e (R = (CH3)3Si) react with 2 or 4 to form 3 a and 5 c as well as (diphenylmethylidene)-trimethyl-silylphosphine 5 e.
    Notizen: Alkyl- oder Arylbis(trimethylsilyl)phosphane 1 (R = Mesityl, C9H11 a; (CH3)3C b; C6H5 c; CH3 d) reagieren mit Dimethylformamid 2 oder Benzophenon 4 nur sehr langsam im Laufe von Monaten. Unter der Katalyse von wenig festem Natriumhydroxid sind die Umsetzungen aber nach wenigen Tagen bei +20°C beendet. Aus 1 a bzw. 1 b und 2 sind die (Dimethylaminomethyliden)phosphane 3 a und 3 b zugänglich; mit 1 a und 4 erhält man Mesityl-(diphenylmethyliden)-phosphan 5 a. Die thermisch instabilen Verbindungen 3 d und 5 c können zwar NMR-spektroskopisch nachgewiesen werden, dimerisieren aber schnell zu 2,4-Bis(dimethylamino)-1,3-dimethyl- 10 d und 1,2,2,3,4, 4-Hexaphenyl-1, 3-diphosphetan 15 c. In ähnlicher Weise reagieren die Lithium-trimethylsilylphosphide 6 a, 6 c und 6 e (R = (CH3)3Si) mit 2 oder 4 zu 3 a und 5 c sowie zum (Diphenylmethyliden)-trimethylsilylphosphan 5 e.
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1002/zaac.19814790805
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