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  • 1
    ISSN: 0044-2313
    Keywords: Di(organosulfonyl)amines ; addition compounds with dimethyl sulfoxide ; addition compounds with triphenylphosphine oxide ; preparation ; crystal and molecular structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Polysulfonyl Amines. XLVI. Molecular Adducts of Di(organosulfonyl)amines with Dimethyl Sulfoxide and Triphenylphosphine Oxide. X-Ray Structure Determination of Di(4-fluorobenzenesulfonyl)amine-Dimethyl Sulfoxide(2/1)From equimolar solutions of the respective components in CH2Cl2/petroleum ether, the following crystalline addition compounds were obtained: (X—C6H4SO2)2NH … OS(CH3)2, where X = H, 4—CH3, 4—Cl, 4—Br, 4—I, 4—NO2 or 3—NO2; [(4—F—C6H4SO2)2NH]2 · (OS(CH)3)2 (8); (4—I—C6H4SO2)2NH · OP(C6H5)3. A (2/1) complex of (4—F—C6H4SO2)2NH with OP(C6H5)3 could not be isolated. The solid-state structure of the (2/1) compound 8 is compared with the known structure of the (1/1) complex (CH3SO2)2NH · OS(CH3)2. The crystallographic data for 8 at -95°C are: monoclinic, space group C2/c, a = 2 369.9(13), b = 1 006.8(4), c = 2 772.6(13) pm, β = 110.71(4)°, U = 6.187 nm3, Z = 8. Two N—H … O hydrogen bonds with N … O 275 and 280 pm connect the disulfonylamine molecules with the dimethyl sulfoxide molecule. The O atom of the latter has a trigonal-planar environment consisting of the S atom and the two hydrogen bond H atoms.
    Notes: Aus äquimolaren Lösungen der jeweiligen Komponenten in CH2Cl2/Petrolether wurden die folgenden kristallinen Addukte erhalten: (X—C6H4SO2)2NH · OS(CH3)2 mit X = H, 4—CH3, 4—Cl, 4—Br, 4—I, 4—NO2 und 3—NO2; [(4—F—C6H4SO2)2NH]2 · (OS(CH)3)2 (8); (4—I—C6H4SO2)2NH · OP(C6H5)3. Ein (2/1)-Komplex aus (4-F—C6H4SO2)2NH und OP(C6H5)3 ließ sich nicht isolieren. Die Festkörperstruktur des (2/1)-Addukts 8 wird mit der bekannten Struktur des (1/1)-Komplexes (CH3SO2)2NH · OS(CH3)2 verglichen. Kristallographische Daten von 8 bei -95°C: monoklin, Raumgruppe C2/c, a = 2 369,9(13), b = 1 006,8(4), c = 2 772,6(13) pm, β = 110,71(4)°, U = 6,187 nm3, Z = 8. Zwei Wasserstoffbrücken N—H … O mit N … O 275 bzw. 280 pm verknüpfen die Disulfonylamin-Moleküle mit dem Dimethylsulfoxid-Molekül. Das O-Atom des letzteren ist trigonal-planar vom S-Atom und den zwei Brücken-H-Atomen umgeben.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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