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  • Polysulfanes  (2)
  • Strukturaufklärung  (2)
  • X-ray structural analysis  (2)
  • 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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    Paper (German National Licenses)
  • 2
    Electronic Resource
    Electronic Resource
    Große Schwefel-Stickstoff-Heterocyclen: Synthese der Schwefelimide SnNH (n = 8, 9, 11) und Strukturen von S8NH und S9NHSchwefelverbindungen, 196. Mitteilung. Diese Arbeit wurde von der Deutschen Forschungsgemeinschaft, dem Deutschen Akademischen Austauschdienst und dem Fonds der Chemischen Industrie unterstützt. 195. Mitteilung: Lit. [1]. (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für die chemische Industrie 108 (1996), S. 2641-2643 
    Details
    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
    URL: http://dx.doi.org/10.1002/ange.19961082111
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  • 3
    Electronic Resource
    Electronic Resource
    Schwefelsäure aus Schwefeltrioxid und Wasser - eine überraschend komplexe ReaktionSchwefelverbindungen, 189. Mitteilung. Für die Anfertigung der Abb. 1-4 danke ich Frau Dr. Yana Drozdova. 188. Mitteilung: M. Pridöhl, R. Steudel, J. Buschmann, P. Luger, Z. Anorg. Allg. Chem., im Druck. (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für die chemische Industrie 107 (1995), S. 1433-1435 
    Details
    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
    URL: http://dx.doi.org/10.1002/ange.19951071206
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  • 4
    Electronic Resource
    Electronic Resource
    Preparation of spiro-cyclic organic polysulfanes of type C6H10Sn and x-ray structural analysis of C6H10S11, a derivative of cyclo-dodecasulfur (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1594-1600 
    Details
    ISSN: 0044-2313
    Keywords: Organic polysulfanes ; NMR spectra ; X-ray structural analysis ; high-pressure liquid chromatography ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Darstellung spirocyclischer organischer Polysulfane des Typs C6H10Sn und Röntgenstrukturanalyse von C6H10S11Durch Reaktion von (C5H5)2Ti(μ-S2)2C6H10 3 mit S2Cl2 wurde 7,8,9,10,11,12-Hexathiaspiro[5,6]dodecan 4 hergestellt (Ausbeute 51%), das durch UV-, IR-, Raman-, Massen- und NMR-Spektren (1H, 13C) charakterisiert wurde. Die NMR-Spektren zeigen, daß der siebengliedrige CS6-Ring in Lösung Pseudorotation erleidet. Mit S7Cl2 reagiert der Komplex 3 zu 7,8,9,10,11,12,13,14,15,16,17-Undecathiaspiro-[5.11]heptadecan 5 (Ausbeute 23%). Die gelben, monoklinen Kristalle von 5 bestehen aus spirocyclischen C6H10S11-Molekülen, deren C6-Ring Sesselkonformation aufweist, während der CS11-Ring eine dem cyclo-Dodecaschwefel S12 entsprechende Konformation besitzt. Alle Glieder der homologen Reihe C6H10Sm (m = 5-14) wurden mittels HPLC charakterisiert.
    Notes: By reaction of (C5H5)2Ti(μ-S2)2C6H10 3 with S2Cl2 7,8,9,10,11,12-hexathiaspiro-[5.6]dodecane 4 is prepared (yield 51%) and characterized by UV, IR, Raman, mass, and NMR spectra (1H, 13C). The seven-membered CS6 ring undergoes pseudorotation in solution. With S7Cl2 the complex 3 yields 7,8,9,10,11,12,13,14,15,16,17-undecathiaspiro[5.11]heptadecane 5 (yield 23%). The yellow, monoclinic crystals of 5 consist of spirocyclic C6H10S11 molecules with the C6 ring in a chair-conformation while the CS11 ring is of the same conformation as cyclododecasulfur S12. UV, IR, Raman, mass and NMR-spectra of 5 are reported. A mixture of dichlorosulfanes SnCl2 (n = 1 -8) reacts with 3 to give the homologous series C6H10Sm which was characterized by reversed-phase HPLC for m = 5 - 14.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19966220924
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  • 5
    Electronic Resource
    Electronic Resource
    Sulfur Compounds. 183. A Derivative of Perthiocarbonic Acid H2CS4: X-ray structural analysis of bis(triphenylmethyl) perthiocarbonate (Ph3C)2CS4 (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1513-1516 
    Details
    ISSN: 0044-2313
    Keywords: Perthiocarbonic acid diester ; X-ray structural analysis ; perthiocarbonate ; bis(triphenylmethyl) perthiocarbonic acid diester ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ein Derivat der Perthiokohlensäure H2CS4: Röntgenstrukturanalyse von Bis(triphenylmethyl)perthiocarbonat (Ph3C)2CS4Die Molekülstruktur von Ph3CSSC(S)SCPh3 · CS2 wurde durch eine Röntgenstrukturanalyse bestimmt. Die Substanz kristallisiert im triklinen Kristallsystem [a = 884,9(2) pm, b = 1 039,5(2) pm, c = 2 064,6(3) pm, α = 75,86(1)°, γ = 79,83(2)°, γ = 77,31(5)°, Z = 2, Raumgruppe P1]. Die CS3-Gruppe ist planar; die S—S-Bindung (201,4 pm) bildet mit der CS3-Ebene einen Winkel von 5,7°. Der CSSC-Torsionswinkel beträgt 96,3°. (Ph3C)2CS4 wurde durch Umsetzung von TosNSCl2 (Tos = p-MeC6H4SO2) mit Ph3CSH in CS2 in Gegenwart von Triethylamin erhalten. Der Reaktionsmechanismus wird diskutiert.
    Notes: The molecular structure of Ph3CSSC(S)SCPh3 · CS2 has been determined by X-ray structural analysis. The substance crystallizes in the triclinic crystal system [a = 884.9(2) pm, b = 1 039.5(2) pm, c = 2 064.6(3) pm, α = 75.86(1)°, β = 79.83(2)°, γ = 77.31(5)°, Z = 2, space group P1]. The CS3 group is planar; the S—S-bond (201.4 pm) forms an angle of 5.7° with the CS3 plane. The torsional angle CSSC equals 96.3°. (Ph3C)2CS4 was obtained by reaction of TosNSCl2 (Tos = p-MeC6H4SO2) with Ph3CSH in CS2 in the presence of triethylamine. The reaction mechanism is discussed.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19956210913
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  • 6
    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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