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  • General Chemistry  (2)
  • 1H/13C-NMR (2 D)  (1)
  • Diaminosulfanes / Disilanes / Sulfur diimides
  • 1995-1999  (3)
  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Chemistry - A European Journal 1 (1995), S. 389-393 
    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.
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  • 2
    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.
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1163-1167 
    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.
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