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首页> 外文期刊>Structural Chemistry >Chlorodiphenyltin(IV) and triphenyltin(IV) complexes of N-alkylated 2-amino-1-cyclopentene-1-carbodithioic acids: synthesis, spectroscopic characterization and X-ray studies
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Chlorodiphenyltin(IV) and triphenyltin(IV) complexes of N-alkylated 2-amino-1-cyclopentene-1-carbodithioic acids: synthesis, spectroscopic characterization and X-ray studies

机译:N-烷基化的2-氨基-1-环戊烯-1-碳二硫代酸的氯二苯基锡(IV)和三苯基锡(IV)配合物:合成,光谱表征和X射线研究

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摘要

Four new complexes, [Ph3Sn(isopropylACDA)] (1), [Ph2SnCl(isopropylACDA)] (2), [Ph3Sn(secbutylACDA)] (3), and [Ph2SnCl(secbutylACDA)] (4), have been prepared from reaction between N-alkylated 2-amino-1-cyclopentene-1-carbodithioic acids (ACDA) with Ph2SnCl2 and Ph3SnCl in 1:1 ratio. All complexes are characterized by FTIR, multinuclear NMR (H-1, C-13, and Sn-119) and mass spectrometry. In all complexes, the S-H proton has been removed and coordination takes place through the carbodithioate moiety. The Sn-119 NMR data are consistent with five coordination of tin atom in solution. Complexes 2, 3, and 4 have also been confirmed by single X-ray crystallography. All three crystals are triclinic with space group P - 1. In complexes 2 and 4, the geometry around tin atom is distorted trigonal bipyramidal while in 3 the geometry is in between distorted tetrahedral and trigonal bipyramid. In all three structures, ligands are asymmetrically coordinated to tin atom. In addition, crystal structures are further stabilized by N-H center dot center dot center dot S hydrogen bonding.
机译:从反应中制备了四个新的配合物[Ph3Sn(isopropylACDA)](1),[Ph2SnCl(isopropylACDA)](2),[Ph3Sn(secbutylACDA)](3)和[Ph2SnCl(secbutylACDA)](4)。 N-烷基化的2-氨基-1-环戊烯-1-碳二硫代酸(ACDA)与Ph2SnCl2和Ph3SnCl的比例为1:1。所有复合物均通过FTIR,多核NMR(H-1,C-13和Sn-119)和质谱进行表征。在所有络合物中,S-H质子均已去除,配位通过碳二硫代酸酯部分发生。 Sn-119 NMR数据与溶液中锡原子的五配位相一致。配合物2、3和4也已经通过单X射线晶体学证实。所有三个晶体都是三斜晶系的,其空间群为P-1。在配合物2和4中,锡原子周围的几何形状是扭曲的三角双锥体,而在3中,几何形状介于扭曲的四面体和三角双锥体之间。在所有三个结构中,配体与锡原子不对称配位。另外,通过N-H中心点中心点中心点S氢键使晶体结构进一步稳定。

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