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  • 1
    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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  • 2
    ISSN: 0044-2313
    Keywords: Seleniumsulfides ; thermal polymerization ; DSC ; HPLC ; Raman spectroscopy ; X-ray diffraction ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Schwefelverbindungen. 164. Thermische Polymerisation des cyclischen Selensulfids 1,2-Se2S5 - eine Untersuchung mittels DSC, HPLC, Ramanspektroskopie und RöntgenbeugungKristallines 1,2-Se2S5 polymerisiert bei 47°C endotherm zu einem kettenförmigen Polymer, das nach Streckung und Extraktion aus helicalen Molekülen ähnlich denen im polymeren Schwefel besteht. Beim Erhitzen zersetzt sich das Polymer bei 84°C exotherm zu einer Mischung aus sieben cyclischen SenS8-n-Molekülen; diese Mischung schmilzt bei 111°C. Wenn das polymere Se2S5 mit CS2 gekocht wird, enstehen primär 1,2-Se2S5, SeS5 und 1,2,3-Se3S5, aber zusätzlich werden SeS7 und 1,2-Se2S6 beobachtet.Diese Ergebnisse sprechen für die Atomfolge -Se—S5—Se- in dem Polymer, dessen Pulverdiagramm, Gitterkonstanten und Ramanspektrum mitgeteilt werden.
    Notes: Solid 1,2-Se2S5 polymerizes endothermically at 47°C to give a linear polymer which after stretching and extraction consists of helical molecules similar to those of polymeric sulfur. Heating of the polymer results in slow exothermic depolymerization at 84°C to give a mixture of seven cyclic SenS8-n molecules which melts at 111°C. When the polymeric Se2S5 is refluxed with CS2 the initial depolymerization Products are 1,2-Se2S5, SeS5 and 1,2,3-Se3S5 but in addition SeS7 and 1,2-Se2S6 are formed. These results indicate the atomic sequence -Se—S5—Se- in the polymer. The powder x-ray diffraction pattern and Raman spectrum of the polymer as well as its lattice parameters are reported and the Probable mechanism of its depolymerization is discussed.
    Additional Material: 7 Ill.
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 725-728 
    ISSN: 0009-2940
    Keywords: Organic polysulfanes ; Titanocene compounds ; Sulfur ligand transfer ; Chain length equilibration ; Sulfur helix ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: CCl3SCl reacts with (C5H5)2TiS5 to give the heptasulfane (CCl3)2S7 which forms colorless crystals of m.p. 38°C. An X-ray structural analysis revealed that the C-S7-C chain is helical but the CCl3 groups are slightly tilted. In the triclinic crystals the molecules are arranged parallel to each other. Decomposition of (CCl3)2S7 provides other members of the homologous series with 4-12 sulfur atoms as shown by HPLC analysis. The reaction of CCl3SCl with (C5H4-CH3)4Ti2S4 yields colorless crystals of (CCl3)2S4, demonstrating the usefulness also of dinuclear titanocene polysulfide complexes for the synthesis of organic polysulfanes. Infrared, Raman, and 13C-NMR spectra of (CCl3)2S7 and (CCl3)S7 are reported.
    Additional Material: 2 Ill.
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