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  • 1
    Electronic Resource
    Electronic Resource
    Cascade reactions with chiral michael acceptors; synthesis of enantiomerically pure tricyclo[3.2.1.02,7]- and bicyclo[3.2.1]octanesDedicated to Professor Dr. Wolfgang Lüttke, Georg-August-Universität Göttingen, on the occasion of his 75th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 1995 (1995), S. 2165-2169 
    Details
    ISSN: 0947-3440
    Keywords: Peterson olefination ; Horner Emmons olefination ; Diastereoselective aprotic Michael cascade reaction ; Tricyclo[3.2.1.02,7]octanes ; Bicyclo[3.2.1]octanes ; Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Starting from the easily accesible chiral aldehyde 2, we obtained enantiomerically pure (Z)- and (E)-α,-chloro-α,β-unsaturated esters 4c in good yields by olefination reactions. (Z)-and (E)-4c were allowed to react with the kinetically controlled generated lithium dienolate Li-7 to give the enantiomerically pure tricyclo[3.2.1.02,7]octanes 8 and 9, respectively. The „push-pull“ substituted cyclopropane moiety of 8 was opened to give solely bicyclo[3.2.1]octane 10.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jlac.1995199512302
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  • 2
    Electronic Resource
    Electronic Resource
    Phase Relationships in the N2O3/N2O4 System and Crystal Structures of N2O3 (1995)
    Weinheim : Wiley-Blackwell
    Chemistry - A European Journal 1 (1995), S. 389-393 
    Details
    ISSN: 0947-6539
    Keywords: crystal structure ; differential thermal analysis ; nitrogen oxides ; phase transitions ; twinning ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Mixtures of N2O3 and N2O4 have been prepared from measured volumes of NO and O2. Phase relationships in the system N2O3/N2O4, which depend on the composition of the samples and on the temperature, were studied by the Guinier technique and differential thermal analysis. Single crystals of phases A and B of N2O3 were grown in situ on a diffractometer and studied at temperatures between -107 and -170°C by X-ray diffraction. The structure analysis of A-N2O3 (tetragonal, space group I41/a, T = -170°C, a = 1625.57 (16), c = 880.49(13) pm, Z = 32, R1 = 0.051 for 1030 unique reflections) is hampered by twinning and additional disorder of one of two crystallographically independent molecules. B-N2O3 is nicely ordered with one molecule in the asymmetric unit (orthorhombic, space group P212121, T = -160°C, a = 506.86(4), b = 647.96(5), c = 863.26(6) pm, Z = 4, R1 = 0.023 for 1352 unique reflections). The most interesting features of the N2O3 molecule are its planarity and the extraordinarily long N—N bond (189.0(1) pm).
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/chem.19950010610
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  • 3
    Electronic Resource
    Electronic Resource
    Thermal Conversion of closo-1,2-(SiMe3)2-1,2-C2B4H4 to closo-1,6-(SiMe3)2-1,6-C2B4H4: Structure Determination by Ab Initio Calculations, Gas-Phase Electron Diffraction, and Low-Temperature X-Ray Diffraction (1997)
    Weinheim : Wiley-Blackwell
    Chemistry - A European Journal 3 (1997), S. 1059-1063 
    Details
    ISSN: 0947-6539
    Keywords: ab initio calculations ; carboranes ; electron diffraction ; rearrangements ; structure elucidation ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: closo-1,2-(SiMe3)2-1,2-C2B4H4 undergoes thermal conversion to 1,6-(SiMe3)2-1,6-C2B4H4. The reaction pathway was monitored by 11B NMR spectroscopy. The structures of the 1,2- and 1,6-isomers were optimized at the HF/6-31 G* ab initio level. Gas-phase electron diffraction studies for both isomers are reported, as well as low-temperature X-ray crystal structure determinations. Comparison of calculated structural data with the data obtained experimentally shows good agreement between theory and experiment.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/chem.19970030712
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  • 4
    Electronic Resource
    Electronic Resource
    On the Polymorphism of White PhosphorusDedicated to Professor Gottfried Huttner on the occasion of his 60th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1235-1240 
    Details
    ISSN: 0009-2940
    Keywords: Phosphorus ; Phase transitions ; Molecular crystal ; Crystal growth ; Low-temperature crystal structure ; Librational motion ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: White phosphorus occurs in three modifications. The α form, which exists at roomtemperature, transforms reversibly to the β form at -77°C. The α · β transformation may be strongly delayed. Quenching the α form to -185°C followed by slow warming results in an exothermic reactions with formation of the γ form which transforms into the β form at -120°C in an endothermic reaction. A transition β · γ is not observed. The γ form is characterized by its powder diagram. The structure of the β form is redetermined from a single crystal at -185°C (P., α = 547.88(5), b = 1078.62(11), c = 1096.16(11)pm, α= 94.285(8), β = 99.695(7), γ = 100.680(7)., V = 623.79(10) · 106 pm3, Z = 6 formula units per cell). The P4 molecules exhibit pronounced librational motion in spite of the low temperature of investigation. The arrangement of the centers of the tetrahedra corresponds to the atom positions in the γ-plutonium structure, which is discussed in relation to the bcc structure.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971300911
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  • 5
    Electronic Resource
    Electronic Resource
    Dimethyl(methansulfinyl)sulfoniumhexafluorometallate (CH3)2SS(O)CH3+MF6- (M = As, Sb) und Kristallstruktur von Methansulfinylchlorid [1]Professor Herbert Jacobs zum 60. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 889-894 
    Details
    ISSN: 0044-2313
    Keywords: Dimethyl(methanesulfinyl)sulfonium-Hexafluorometallates ; Vibrational-, NMR-, Mass-Spectra ; Crystal Structure of CH3S(O)Cl ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Dimethyl(methanesulfinyl)sulfonium Hexafluorometallates (CH3)2SS(O)CH3+MF6- (M = As, Sb) and the Crystal Structure of Methanesulfinylchloride CH3S(O)Cl [1]The preparation of dimethyl(methanesulfinyl)sulfoniumhexafluorometallates (CH3)2SS(O)CH3+MF6- (M = As, Sb) and the spectroscopic characterization of the new thiosulfonium salts are described. Alternatively they can be obtained from methylmethanethiosulfinate by methylation. In addition the crystal structure of methanesulfinylchloride CH3S(O)Cl at 113 K is reported. The compound crystallizes in the monoclinic space group P21/n with a = 528.2(1), b = 829.2(2), c = 880.9(2) pm, β = 90.48(2)° and Z = 4.
    Notes: Die Darstellung von Dimethyl(methansulfinyl)sulfoniumhexafluorometallaten (CH3)2SS(O)CH3+MF6- (M = As, Sb) aus Methansulfinylchlorid CH3S(O)Cl und Dimethylsulfoniumhexafluorometallaten (CH3)2SH+MF6- sowie die spektroskopische Charakterisierung der neuen Thiosulfoniumsalze wird beschrieben. Alternativ können diese auch durch Methylierung von Methylmethanthiosulfinat CH3SS(O)CH3 erhalten werden. Die Ergebnisse einer Einkristallröntgenstruktur-analyse von CH3S(O)Cl bei 113 K werden mitgeteilt. Das Sulfinylchlorid kristallisiert in der monoklinen Raumgruppe P21/n mit a = 528,2(1), b = 829,2(2), c = 880,9(2) pm, β = 90,48(2)°, Z = 4.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19966220524
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  • 6
    Electronic Resource
    Electronic Resource
    Synthese und Charakterisierung eines neuen gemischten Titan-Aluminium-Alkoxids (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1163-1167 
    Details
    ISSN: 0044-2313
    Keywords: Titanium-Aluminium Alkoxide ; Aluminium Titanate (Tialite) ; Ceramics Precursor ; X-Ray Structure Determination ; 1H/13C-NMR (2 D) ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structural Characterization of a Novel Titanium-Aluminium AlkoxideThe novel Ti-Al-Alkoxide TiAl2(OiPr)10, was synthesized from aluminium turnings and titanium tetraisopropoxide in 2-propanol and isolated by subsequent fractionating distillation. Colourless prismatic crystals precipitated after 24 h at 20°C from the main fraction. They proved very moisture sensitive. The compound crystallizes in the monoclinc space group C2/c (no. 15) with a = 2303.1(4), b = 1097.2(3), c = 1685.0(3) pm, β = 104.32(1)° and Z = 4. The molecular structure exhibits a bent Al-Ti-Al′ unit, in which Al shows tetrahedral, but Ti octahedral1 coordination. The polyhedra are connected via cis-edges of the octahedron. The structure of the compound in solution was determined by NMR spectroscopy (1H, 13C, COSY) and proved to be identical to the structure in the solid state.
    Notes: Das neue Ti-Al-Alkoxid TiAl2(OiPr)10 wurde durch Umsetzung von Al-Spänen mit Titantetraisopropoxid in Isopropanol und anschließender fraktionierender Destillation dargestellt. Die nach 24 h bei 20°C aus der Hauptfraktion gebildeten farblosen, prismatischen Kristalle sind sehr hydrolyseempfindlich. Die Kristallstruktur konnte bei -83°C bestimmt werden: monokline Raumgruppe C2/c (Nr. 15) mit a = 2303,1(4), b = 1097,2(3), c = 1685,0(3) pm, β = 104,32(1)° und Z = 4. Die Molekülstruktur besteht aus einer gewinkelten Al-Ti-Al′-Einheit, in der Al tetraedrisch und Ti oktaedrisch koordiniert sind. Die verknüpfenden Kanten am Ti-Oktaeder sind cis angeordnet. Die Struktur der Verbindung in Lösung wurde NMR-spektroskopisch (1H, 13C, COSY) ermittelt und stimmt mit der Struktur im Einkristall überein.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976230726
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