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  • 1
    Electronic Resource
    Electronic Resource
    Sulfur Compounds, 199Part 198: R. Steudel, Y Drozdova, K. Miaskiewicz, R. H. Hertwig, W. Koch, J Am. Chem. Soc. 1997, 119, 1990.. Novel Titanocene Thiolato Complexes and Their Application in Preparing New Sulfur-Containing Heterocycles (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 757-764 
    Details
    ISSN: 0009-2940
    Keywords: Titanocene complexes ; S ligands ; Organic polysulfanes ; Ligand transfer reactions ; Sulfur heterocycles ; Chalcogens ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Treatment of Cp2Ti(CO)2 (3) with the di- and polysulfanes 1,2,4-(CH2)2S3, C4S6 (9), C,7H10S3 (11), 1,2,4,6-(CH2)3S4 (16), C6H10S6(19), and S6 affords the titanocene chelate complexes Cp2TiS3(CH2)2 (8), (Cp2Ti)2C4S6 (10), Cp2TiS3C7H10 (13), Cp2TiS2C7H10 (14), Cp2TiS4(CH2)3 (17), Cp,2TiS6C6H6H10 (20), and Cp2TiS8 (23). 14 is also obtained from Cp2TiCl2 (1) and the geminal dithiol of norbornene. The analogous reaction with the dithiol of dicyclopentadiene yields Cp2TiS2C10H12 (15). In ligand transfer reactions, 8 reacts with SCl2 to give 1,2,3,5-tetrathiane (25), 10 provides 9 on reaction with Cl2, 13 when treated with S2Cl2 affords C7H10S5 (12), 15 reacts with S2Cl2Cl2 to give C10H12S4. 17 and SCl2 yield 1,2,3,5,7-pentathiepane (18), 20 is converted to C6H10S7 (22) on reaction with SCl2, and 23 yields S10 and 1,2,-C6H4(SCl)2, respectively. With phosgene, thiophosgene, and thionyl chloride, compound 15 yields the corresponding dithiocarbonate 26, the trithiocarbonate 27 and the trisulfane 2-oxide 28. The structure of 27 was determined by X-ray crystallography.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971300614
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  • 2
    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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  • 3
    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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