Synthesis, solution behaviour and X-ray structures of [2-(Me2NCH2)C6H4]SnCl3 and [2-(Me2NCH2)C6H4]SnCl3-DMSO

被引:34
作者
Varga, RA
Silvestru, C [1 ]
Deleanu, C
机构
[1] Univ Babes Bolyai, Fac Chem & Chem Engn, RO-400028 Cluj Napoca, Romania
[2] Roumanian Acad, Natl NMR Lab, Inst Organ Chem, RO-71141 Bucharest, Romania
关键词
hipervalent organotin (IV); solution NMR; X-ray structure; hydrogen bonding; supramolecular association;
D O I
10.1002/aoc.817
中图分类号
O69 [应用化学];
学科分类号
081704 ;
摘要
[2-(Me2NCH2)C6H4]SnCl3 (1) was prepared via (i) salt elimination reaction between RLi and SnCl4 (1:1 molar ratio), in toluene solution, and (ii) redistribution reaction between [2-(Me2NCH2)C6H4](4)Sn and SnCl4 (1:3 molar ratio), in the absence of a solvent. Recrystallization from DMSO afforded the isolation of the DMSO adduct [2-(Me2NCH2)C6H4](SnCl3DMSO)-D-. (1a). The compounds were characterized by multinuclear NMR (H-1, C-13, Sn-119) in solution. The molecular structures of 1 and la were determined by single-crystal X-ray diffraction. The crystal structure of compounds 1 and la consists of discrete monomeric molecular units separated by normal van der Waals distances between heavy atoms. The N atom of the pendant CH2NMe2 arm is strongly coordinated to the tin atom, thus resulting in distorted trigonal bipyramidal (CN)SnCl3 and octahedral (C,N)SnCl3O cores for 1 and 1a, respectively. For both compounds hydrogen bonding generates supramolecular associations in crystal. Copyright (C) 2004 John Wiley Sons, Ltd.
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页码:153 / 160
页数:8
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