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  • 1
    ISSN: 0009-2940
    Keywords: cis-Stannyl-boryl-alkenes ; Sulfur diimide anions ; Multinuclear NMR ; 1,2,5-Azastannaboratoles ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis of 1,2,5-Azastannaborole Derivatives from Sulfur Diimide Anions and cis-Stannyl-boryl-alkenes - X-ray Crystallographic Study of Two 2,5-Dihydro-1-(imino-λ4-sulfanylidene)-1,2,5-azastannaboratoles(E)-3-(Diethylboryl)-2-(chlorodimethylstannyl)-2-pentene (1) reacts with the sulfur diimide anions 3 [R - NSN-K+, R=tBu (a), Me3Si (b), tBu2P (c)] in a 1:1 ratio, and with 4 (K+;-NSN-K+) in a 2:1 ratio, to give various heterocycles. The first products of the reaction between 1 and 3 [2,5-dihydro-1-(imino-λ4-sulfanylidene)-1,2,5-azastannaboratoles 5a, b, c] are isolated at -30°C and characterized by X-ray crystallography. The compounds 5a,b rearrange into the borole derivates 6a,b (with an additional N—Sn coordination) by transfer of an ethyl group from the boron to the sulfur atom. Ethylene is eliminated from compound 6a (not 6b) to give the diaminosulfane derivative 7a. The 2:1 reaction between 1 and 4 affords an unstable intermediate 8 with a fluxional structure, leading to 9 in which an EtS moiety bridges a borole ring (analogous to 6 but without the additional N - Sn coordination) and a boratole ring (analogous to 5). All compounds are characterized by 1H-, 11B-, 13C-, 15N- (in part), 29Si- and 119Sn-NMR spectra.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 0044-2313
    Keywords: Dimethyl(methanesulfinyl)sulfonium-Hexafluorometallates ; Vibrational-, NMR-, Mass-Spectra ; Crystal Structure of CH3S(O)Cl ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Dimethyl(methanesulfinyl)sulfonium Hexafluorometallates (CH3)2SS(O)CH3+MF6- (M = As, Sb) and the Crystal Structure of Methanesulfinylchloride CH3S(O)Cl [1]The preparation of dimethyl(methanesulfinyl)sulfoniumhexafluorometallates (CH3)2SS(O)CH3+MF6- (M = As, Sb) and the spectroscopic characterization of the new thiosulfonium salts are described. Alternatively they can be obtained from methylmethanethiosulfinate by methylation. In addition the crystal structure of methanesulfinylchloride CH3S(O)Cl at 113 K is reported. The compound crystallizes in the monoclinic space group P21/n with a = 528.2(1), b = 829.2(2), c = 880.9(2) pm, β = 90.48(2)° and Z = 4.
    Notes: Die Darstellung von Dimethyl(methansulfinyl)sulfoniumhexafluorometallaten (CH3)2SS(O)CH3+MF6- (M = As, Sb) aus Methansulfinylchlorid CH3S(O)Cl und Dimethylsulfoniumhexafluorometallaten (CH3)2SH+MF6- sowie die spektroskopische Charakterisierung der neuen Thiosulfoniumsalze wird beschrieben. Alternativ können diese auch durch Methylierung von Methylmethanthiosulfinat CH3SS(O)CH3 erhalten werden. Die Ergebnisse einer Einkristallröntgenstruktur-analyse von CH3S(O)Cl bei 113 K werden mitgeteilt. Das Sulfinylchlorid kristallisiert in der monoklinen Raumgruppe P21/n mit a = 528,2(1), b = 829,2(2), c = 880,9(2) pm, β = 90,48(2)°, Z = 4.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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