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  • Polysulfanes  (2)
  • Strukturaufklärung  (2)
  • X-ray crystallography  (2)
  • 1
    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
    ISSN: 0044-8249
    Keywords: Schwefelverbindungen ; Stickstoffverbindungen ; Strukturaufklärung ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 3
    ISSN: 0044-8249
    Keywords: Atmosphärenchemie ; Schwefelsäure ; Schwefelverbindungen ; Strukturaufklärung ; Wasserstoffbrücken ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 117-120 
    ISSN: 0044-2313
    Keywords: X-ray crystallography ; sulfur-sulfur bonds ; tetra-sulfides ; dicyanosulfanes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Kristall- und Molekülstruktur von Dicyanotetrasulfan S4(CN)2S4(CN)2 kristallisiert in der monoklinen Raumgruppe P21/c mit den im Abstract angegebenen Parametern. Die Moleküle besetzen allgemeine Lagen, sind aber ungefähr von C2-Symmetrie. Die Konformation ist all-trans mit den Torsionswinkeln CSSS = 74,6° und 81,7° sowie SSSS = 84,8°. Die mittlere SS-Bindung (201,7 pm) ist viel kürzer als die äußeren (Mittelwert 206,8 pm). Die intermolekularen Wechselwirkungen sind vom van-der-Waals-Typ.
    Notes: S4(CN)2 crystallizes in the monoclinic space group P21/c with a = 885.7 pm, b = 794.2 pm, c = 1032.6 pm, β = 109.0° (at 173 K). The molecules occupy general sites but are of approximate C2 symmetry. The conformation of the molecules is all-trans with torsional angles CSSS = 74.6° and 81.7° and SSSS = 84.8°. The central SS bond (201.7 pm) is much shorter than the terminal SS bonds (av. 206.8 pm). There are no stronger than van-der-Waals type intermolecular interactions.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1672-1676 
    ISSN: 0044-2313
    Keywords: X-ray crystallography ; dithiosulfite ; vibrational spectra ; sulfane oxide ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Darstellung und Röntgenstrukturanalyse des bemerkenswert stabilen Bis(triphenylmethyl)trisulfan-2-oxids R2S3O [1]Triphenylmethylthiol reagiert in Gegenwart von Aminen mit Thionylchlorid zu [(C6H5)3CS]2SO, das als Solvat mit 1 Mol CS2 kristallisiert: triklin, Raumgruppe P1 mit a = 1 193,4(4), b = 1 266,8(5), c = 1 421,6(7) pm, α = 63,79(2)°, β = 65,25(2)°, γ = 63,18(2)α, ρ = 1,354 g cm-3 bei -80°C. Das Trisulfanoxidmolekül R2S3O ist von C1-Symmetrie und weist ein fast planares Gerüst CSSSC auf mit den im Abstract angegebenen geometrischen Parametern.
    Notes: Triphenylmethylthiol reacts with thionylchloride in the presence of amines to give [(C6H5)3CS]2SO which crystallizes with one mole of CS2 in the triclinic space group P1 with a = 1 193.4(4), b = 1 266.8(5), c = 1 421.6(7) pm, α = 63.79(2)°, β = 65.25(2)°, γ = 63.18(2)°, π = 1.354 g cm-3 at -80°C. The R2S3O molecules are of C1 symmetry containing an almost planar CSSSC backbone with dss = 212.7(1) and 211.4(1) pm, dcs = 188.0(2) and 188.2(2) pm, dso = 146.9(1) pm, αSSS = 83.8°, αSSO = 112.0° and 112.2°, τCSSS = 160.7° and -172.3°.
    Additional Material: 1 Ill.
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1021-1024 
    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
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