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  • Inorganic Chemistry  (3)
  • Aluminium  (2)
  • (Arene)chromium complexes  (1)
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  • 1
    Electronic Resource
    Electronic Resource
    Benzil Derivatives as Trapping Reagents for the Monomeric Alkylindium(i) Compound in-c(SiMe3)3 (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1269-1272 
    Details
    ISSN: 0009-2940
    Keywords: Indium ; Clusters ; Low-valent compounds ; Trapping reactions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The tetrahedral cluster compound tetrakis[[Tris(trimethylsilyl)methyl]indium(I)] 91) reacts in boiling n-hexane with benzil derivatives (p-X-C6H4)C(O)(p-X-C6H4) (X = H, OMe, Br), to yield the 1,4-cycloadditon products of the monomeric alkylindium(I), In-C(SiMe3)3, in which the In atoms are coordinated by a chelating enediolato ligand, to form a five-membered InO2C2 heterocycle. As shown by two crystal structure determinations (X = H, OMe), the products are dimeric in the solid state, with a four-membered In2O2 heterocycle in the molecular center and both C(SiMe3)3 groups, as well as both enediolato substitutents in a cis arrangement.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971300915
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  • 2
    Electronic Resource
    Electronic Resource
    Synthesis and reactions of novel tricyclo[4.3.1.12,5]undec-3-en-10-ones (1990)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 123 (1990), S. 2131-2139 
    Details
    ISSN: 0009-2940
    Keywords: Stereoselective synthesis ; Rings, bridged seven-membered ; Ketones, α,α'-dibromo, monoterpenoid ; Oxyallyl cations ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Sodium iodide/copper mediated intermolecular cyclodehalo-genation of 2,6-dibromocyclohexanones in the presence of furan and cyclopentadiene afforded a variety of alkylated tricyclo[4.3.1.12,5]undec-3-en-10-ones. An alkyl group (methyl or isopropyl) adjacent to the carbonyl carbon atom in the starting 2,6-dibromocyclohexanone derivative was important for the success of the cycloaddition procedure. Even tricylic ketone 11, containing two quaternary carbon atoms adjacent to the carbonyl carbon atom, was prepared. The α,α'-dibromoketones derived from either enantiomer of menthone and cyclopentadiene reacted enantioselectively, yielding tricycles (7R)-7 and (7S)-7. Since a number of tricyclic ketones 3-11 were sensitive, they were reduced to secondary alcohols 19-25, having an axial, α-configurated OH group and were also converted into tertiary methylcarbinols 26 and 27 using methyllithium activated with tBuOK. Secondary α-configurated alcohols 19-25 had an earthy-mouldy odour, and tertiary carbinols 26 and 27 even more so. Unsaturated alcohols 26 and 27 showed a 4 J coupling of 2 Hz between the rigidly held OH proton and the nearest methyl protons. On hydrogenation of the olefinic double bond (4 → 33, → 34) this long-range coupling disappeared.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19901231108
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  • 3
    Electronic Resource
    Electronic Resource
    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
    Keywords: Aluminium ; Chelates ; Lewis acids ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 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.
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    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
    Keywords: Aluminium ; Gallium ; Diazo compounds ; Dimerization ; Coordination modes ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 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.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 5
    Electronic Resource
    Electronic Resource
    Diastereoselective Ring Expansion Rearrangements of (Benzocyclobutenone)-and (Benzocyclobutenedione)chromium Complexes: Syntheses of Substituted 1-Indanone and 1,3-Indandione Complexes (1999)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 1999 (1999), S. 823-835 
    Details
    ISSN: 1434-193X
    Keywords: (Arene)chromium complexes ; α-Ketol rearrangement ; Vinylcyclobutene-cyclohexadiene rearrangement ; Benzocyclobutenes ; Indanone derivatives ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: -Organolithium and Grignard reagents add to the oxo group of (benzocyclobutenone)tricarbonylchromium(0) (1) diastereoselectively from the exo face of the organic ligand. If acyl anion equivalents are used as nucleophiles, deprotection of the carbonyl functions of the adducts causes ring expansion reactions to occur. Among these a rare example of an anion-accelerated 1-vinylcyclobutenol-cyclohexadienol rearrangement is reported which results, after isomerization, in a naphthol complex. Other ring expansion reactions gave coordinated substituted indanone derivatives. The facial differentiation by the tricarbonylchromium moiety allows for the first time the determination of the distereoselectivity of these reactions. The 1-oxoindan-2-ol derivatives obtained can undergo an α-ketol rearrangement with formation of the corresponding 2-oxoindan-1-ol complexes. Some of these reactions were performed with nonracemic starting material in order to determine how far chirality transfer from the planar chiral starting material to C-2 in the indanone system was possible. The ring expansion was also feasible with the benzocyclobutenedione complex as a starting compound, the reaction giving substituted 1,3-indandione complexes. Crystal structure analyses of three of the complexes prepared are reported.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 6
    Electronic Resource
    Electronic Resource
    Kalium-Lanthanoid-Carbonate, KM(CO3)2 (M = Nd, Gd, Dy, Ho, Yb)Professor Rudolf Hoppe zum 75. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1753-1758 
    Details
    ISSN: 0044-2313
    Keywords: Carbonates ; Lanthanoids ; Synthesis ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Potassium Lanthanoid Carbonates, KM(CO3)2 (M = Nd, Gd, Dy, Ho, Yb)The ternary potassium lanthanoid carbonates KM(CO3)2 (M = Nd, Gd, Dy, Ho, Yb) are obtained as single crystals by high-pressure synthesis in steel autoclaves with carbon dioxide (starting pressure approximately 50 bar at ambient temperature) in the presence of water from a mixture of K2CO3 and MCl3 · x H2O (x = 7 and 6, respectively) at 450°C within 4 weeks. In KNd(CO3)2 (orthorhombic, Pmn21, Z = 4, a = 973.1(2), b = 645.69(8), c = 855.58(14) pm, R1 = 0.0763 for all data) [Nd-μ1-(CO3)3-μ2-(CO3)3] polyhedra are connected three-dimensionally to [Nd(CO3)] layers as similarly in UO2(CO3); these layers are connected via the second half of the carbonate ligands and K+ ions. In KDy(CO3)2 (monoclinic, C2/c, Z = 4, a = 853.8(2), b = 949.1(1), c = 694.5(1) pm, β = 111.1(2)°, R1 = 0.0266 for all data) and in the isotypic carbonates KM(CO3)2 (M = Gd, Ho, Yb) the polyhedra [Dy-μ1-(CO3)4-μ2-(CO3)2] and [K-μ1-(CO3)6] are connected to “syndiotactic” zig-zag chains and by further O-ligator atoms of the carbonate ligands such that each zig-zag chain is surrounded by four unlike chains and vice versa.
    Notes: Die ternären Kalium-Lanthanoid-Carbonate KM(CO3)2 (M = Nd, Gd, Dy, Ho, Yb) erhält man in Form von Einkristallen durch Hochdrucksynthese im Stahlautoklaven mit Kohlendioxid (Anfangsdruck etwa 50 bar bei Raumtemperatur) in Anwesenheit von Wasser aus Gemengen von K2CO3 und MCl3 · x H2O (x = 7 bzw. 6) bei 450°C innerhalb von 4 Wochen. In KNd(CO3)2 (orthorhombisch, Pmn21, Z = 4; a = 973,1(2); b = 645,69(8); c = 855,58(14) pm; R1 = 0,0763 für alle Daten) werden Polyeder [Nd-μ1-(CO3)3-μ2-(CO3)3] ähnlich wie in UO2(CO3) zu Schichten [Nd(CO3)] verknüpft; die Schichten werden über die zweite Hälfte von CO32--Liganden sowie durch K+ dreidimensional verknüpft. In KDy(CO3)2 (monoklin, C2/c, Z = 4; a = 853,8(2); b = 949,1(1); c = 694,5(1) pm; β = 111,1(2)°; R1 = 0,0266 für alle Daten) und in den isotypen Carbonaten KM(CO3)2 (M = Gd, Ho, Yb) sind die Polyeder [Dy-μ1-(CO3)4-μ2-(CO3)2] und [K-μ1-(CO3)6] jeweils zu „syndiotaktischen“ Zick-Zack-Ketten und weiter über gemeinsame O-Ligatoratome der Carbonat-Liganden so verknüpft, daß die Zick-Zack-Ketten jeweils von vier Ketten der anderen Sorte umgeben sind.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976231115
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