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Zur Struktur und Reaktivität von stannylierten Propylaminen und -sulfiden. Kristall- und Molekülstruktur von Bis(3-dimethylchlorostannylpropyl)sulfid S(CH2CH2CH2SnMe2Cl)2
Authors:K Jurkschat  B Schmid  M Dybiona  U Baumeister  H Hartung  A Tzschach
Abstract:Structure and Reactivity of Stannylated Propyl Amines and Propyl Sulfides. Crystal and Molecular Structure of Bis(3-chlorodimethylstannylpropyl)sulfide S(CH2CH2CH2SnMe2Cl)2 The synthesis and reactivity of stannylated propyl amines and propyl sulfides, respectively, E(CH2CH2CH2SnMe3)2 ( 1 , E ? NMe; 2 E ? S) and N(CH2CH2CH2SnMe3)3 3 are reported. 1 and 3 react with dimethyl dichlorostannane under thermal cyclisation to 1,5-dimethyl-5-chloro-1aza-5-stannabicyclo3.3.01,5]octane Me(Cl)Sn(CH2CH2CH2)2NMe 4 and 5-chloro-1-aza-5-stannatricyclo3.3.3.01,5]-undecane ClSn(CH2CH2CH2)3N 5 , respectively. The reaction of 2 with dimethyl dichlorostannane leads to the formation of bis(3-chloro-dimethylstannylpropyl)sulfide S(CH2CH2CH2SnMe2Cl)2 6 , whereas the treatment of 2 with tin tetrachloride yields the bis(3-di-chloro-methylstannylpropyl)sulfide S(CH2CH2CH2SnMeCl2)2 7 . The 1H, 13C, and 119Sn NMR data are discussed. 6 crystallizes in the ortho-rhombic space group Pna21 with the unit cell parameters a = 2275.0(1), b = 733.6(2), c = 1062.0(4) pm, V = 1.77273 nm3, Z = 4. The structure was refined to a final R value of 0.041. Both tin atoms adopt distorted trigonal bipyramidal configurations as a result of intramolecular interactions with the bridging sulphur. The sulphur and the chlorine atoms occupy the apical positions. The Sn? S distances amount to 309.7(4) and 311.8(4) pm.
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