ALBERT — All Library Books, journals and Electronic Records Telegrafenberg

Hits per page

hits 1 - 7 | 7 hits

Sorting

Electronic Resource

Preparation of Organic Polysulfanes R2Sn (n = 5, 7, 8, 9) from Sulfenyl Chlorides, RSCl, and Transition Metal Polysulfido Complexes (2000)

Steudel, Ralf ; Hassenberg, Karin ; Münchow, Vera ; [et al.]

Weinheim : Wiley-Blackwell

Berichte der deutschen chemischen Gesellschaft 2000 (2000), S. 921-928

add to mindlist on the mindlist

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

Permalink

	Location	Call Number	Expected	Availability

Others were also interested in ...

Paper (German National Licenses)

Electronic Resource

Sulfur Compounds. 183. A Derivative of Perthiocarbonic Acid H2CS4: X-ray structural analysis of bis(triphenylmethyl) perthiocarbonate (Ph3C)2CS4 (1995)

Münchow, Vera ; Steudel, Ralf ; Buschmann, Jürgen ; [et al.]

Weinheim : Wiley-Blackwell

Zeitschrift für anorganische Chemie 621 (1995), S. 1513-1516

add to mindlist on the mindlist

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

Permalink

	Location	Call Number	Expected	Availability

Others were also interested in ...

Paper (German National Licenses)

Fulltext

Electronic Resource

The Decomposition of Aqueous Dithionite and its reactions with polythionates SnO2-6 (n = 3-5) studied by ion-pair chromatography (1994)

Münchow, Vera ; Steudel, Ralf

Weinheim : Wiley-Blackwell

Zeitschrift für anorganische Chemie 620 (1994), S. 121-126

add to mindlist on the mindlist

Details

ISSN: 0044-2313

Keywords: Dithionite decomposition ; polythionate reduction ; thiosulfate decomposition ; ion-pair chromatography ; Chemistry ; Inorganic Chemistry

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Description / Table of Contents: Die Zersetzung von Dithionit in Wasser und seine Reaktionen mit Polythionaten SnO2-6 (n = 3-5) - eine Untersuchung mittels IonenpaarchromatographieDithionit hydrolysiert in Wasser bei 20°C und pH-Werten nicht weit von 7,0 zu Thiosulfat und Sulfit, aus denen dann Trithionat entstehen kann. Zugabe von Thiosulfat beschleunigt die Hydrolysereaktion nur bei pH 〈 6. Diese pH-Abhängigkeit wird durch die Bildung des Ions HS2O3- erklärt, das durch Dithionit zu Sulfid und Sulfit reduziert wird. Sulfidionen zerstören Dithionit durch nucleophile Spaltung, wobei wahrscheinlich primär Sulfoxylat und Thiosulfit entstehen. Die Polythionate SnO62- (n = 3-5) werden von Dithionit bei 20°C und pH = 7,0 reduziert (Gleichung siehe Abstract), wobei die Reaktionsgeschwindigkeit mit der Kettenlänge n rasch ansteigt. In Sekundärreaktionen baut Sulfit die Polythionationen unter Bildung von Thiosulfat ab.

Notes: Aqueous dithionite decomposes at 20°C and pH values not far from 7.0 to give thiosulfate and sulfite from which trithionate may form. Addition of thiosulfate accelerates this reaction only at pH 〈 6. The pH dependence is explained by formation of HS2O3- ions which are reduced by dithionite to HS- and SO2-3. Sulfide destroys dithionite by nucleophilic cleavage, probably with formation of sulfoxylate and thiosulfite ions. The polythionates SnO2-6 (n = 3-5) are reduced by dithionite at pH = 7.0 and 20°C according to SnO2-6 + S2O2-4 + 2 H2O→S2O32- + Sn-3SO32- + 4H1 + 2SO32- The reaction rate rapidly increases with the number n of sulfur atoms. In secondary reactions sulfite attacks SnO62- ions with thiosulfate formation.

Additional Material: 7 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/zaac.19946200120

Permalink

	Location	Call Number	Expected	Availability

Others were also interested in ...

Paper (German National Licenses)

Fulltext

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)

Steudel, Ralf ; Kustos, Monika ; Münchow, Vera ; [et al.]

Weinheim : Wiley-Blackwell

Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 757-764

add to mindlist on the mindlist

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

Permalink

	Location	Call Number	Expected	Availability

Others were also interested in ...

Paper (German National Licenses)

Fulltext

Electronic Resource

Preparation of spiro-cyclic organic polysulfanes of type C6H10Sn and x-ray structural analysis of C6H10S11, a derivative of cyclo-dodecasulfur (1996)

Steudel, Ralf ; Münchow, Vera ; Pickardt, Joachim

Weinheim : Wiley-Blackwell

Zeitschrift für anorganische Chemie 622 (1996), S. 1594-1600

add to mindlist on the mindlist

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

Permalink