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  • 1
    Electronic Resource
    Electronic Resource
    Preparation of Organic Polysulfanes R2Sn (n = 5, 7, 8, 9) from Sulfenyl Chlorides, RSCl, and Transition Metal Polysulfido Complexes (2000)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 2000 (2000), S. 921-928 
    Details
    ISSN: 1434-1948
    Keywords: Sulfur ; Titanium ; Zinc ; Polysulfido complexes ; Sulfur heterocycles ; Polysulfides ; Polysulfanes ; Sulfenyl chlorides ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The preparation of seven novel organic polysulfanes is reported. Bis(n-octyl)heptasulfane R2S7 1 is formed upon reaction of RSCl with [Cp2TiS5], while the corresponding nonasulfane R2S9 2 is obtained by reaction of RSSCl with [Cp2TiS5]. The bis(n-octyl)pentasulfane R2S5 3 is obtained from RSCl and [(Cp′2TiCl)2S3] by transfer of the S3 ligand at 20 °C. The new alkyl polysulfanes 1-3 have been obtained in quantitative yields. They are liquids at 20 °C, having freezing points below -50 °C, but do not form mesogenic phases. Reactions of [Cp2TiS5] with 2-naphthyl- and 4-chlorophenyl sulfenyl chloride furnish the corresponding heptasulfanes 4 and 5, respectively, which are solids at 20 °C. 1,2-Benzodisulfenyl chloride C6H4(SCl)2 reacts with [(Cp′2TiCl)2S3] to give the known 1,2,3,4,5-benzopentathiepin C6H4S5 6, with [Cp2TiS5] to give the novel 1,2,3,4,5,6,7-benzoheptathionin C6H4S7 7, and with [(TMEDA)ZnS6] to give the novel 1,2,3,4,5,6,7,8-benzooctathiecin C6H4S8 8. The cyclic polysulfanes 6-8 are solids at 20 °C and have been recovered in yields of 60-83%. The orthorhombic structure of 1,2-C6H4S7 has been investigated by single-crystal X-ray diffraction analysis. The molecules are found to be located at sites of Cs symmetry and the motif of the C2S7 heterocycle is +-+-+-+-, with the torsion angle of zero at the carbon-carbon bond. The three internuclear SS distances measure 205.0(1), 203.7(1), and 205.7(1) pm.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    Crystal and Molecular Structures as well as Spectra of Two Organic Tetrasulfanes R2S4 (R = 2-benzothiazolyl and 4-chlorophenyl) (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1021-1024 
    Details
    ISSN: 0044-2313
    Keywords: Polysulfanes ; structure ; spectra ; preparation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Kristall- und Molekülstrukturen sowie Spektren zweier organischer Tetrasulfane R2S4 (R = 2-Benzothiazolyl und 4-Chlorphenyl)Bis(2-benzothiazolyl)tetrasulfan, hergestellt aus dem Mercaptan und S2Cl2, kristallisiert in der monoklinen Raumgruppe C2/c mit den im Abstract angegebenen Zelldimensionen. Die Moleküle haben C2-Symmetrie; das S4-Gerüst ist von all-trans-Konformation mit den Parametern dss = 202,7 (terminal) und 207,3 pm (zentral), αsss = 106,4° und τssss = 78,5°. Bis(4-chlorphenyl)tetrasulfan kristallisiert in der monoklinen Raumgruppe P21/a (s. Abstract). Die Moleküle befinden sich in allgemeinen Lagen, sind aber näherungsweise von C2-Symmetrie und ebenfalls von all-trans-Konformation mit dss = 203,6 (terminal), 206,7 (zentral) und 202,3 pm (terminal), αsss = 107,4° und 108,4° sowie τssss = 75,5°. Die intermolekularen Wechselwirkungen sind vom van der Waals-Typ. Infrarot-, Raman-, Massen- und NMR-Spektren (1H, 13C) der Verbindungen werden mitgeteilt.
    Notes: Bis(2-benzothiazolyl)tetrasulfane prepared from the mercaptane and S2Cl2 crystallizes in the monoclinic space group C2/c with a = 3513 pm, b = 577.28 pm, c = 800.0 pm, β = 98.74°, ρ = 1.64 g cm-3 (at 298 K). The molecules are of C2 symmetry with the geometrical parameters of the S4 backbone: dss = 202.7 (terminal) and 207.3 pm (central), αsss = 106.4°, τssss = 78.5°. The overall conformation is all-trans.Bis(4-chlorophenyl)tetrasulfane prepared from the mercaptane and diisopropoxydisulfane crystallizes in the monoclinic space group P21/a with a = 1237.7 pm, b = 748.4 pm, c = 1623.9 pm, β = 105.58°, ρ = 1.61 g cm-3 (at 298 K). The molecules occupy general positions but are approximately of C2 symmetry with dss = 203.6 (terminal), 206.7 (central) and 202.3 pm (terminal), αsss = 107.4° and 108.4°, τssss = 75.5° (all-trans conformation). The intermolecular interactions are of van der Waals type. Infrared, Raman, mass and NMR spectra (1H, 13C) are reported.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19956210621
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