| 有机锡氧簇合物[(μ-O)(μ-OH)Sn2(n-Bu)4]2(C5H4NCO2)2的合成、结构和量子化学研究 | |
| Synthesis, Crystal Structure and Quantum Chemistry of the Organooxotin Cluster [(μ-O)(μ-OH)Sn2(n-Bu)4]2(C5H4NCO2)2 | |
| 摘要: 吡啶-4-甲酸与(n-Bu)2SnO反应合成二(μ-氧)二(μ-羟基氧)桥联四[二(正丁基)锡]二(吡啶-4-甲酸酯)，经元素分析、1H NMR、IR和X-射线衍射表征分子结构,该配合物晶体属单斜晶系,空间群P21/n,晶胞参数：a=1.306 5(3) nm,b=1.314 5(2) nm，c=1.660 8(3) nm，β=96.180(5)°，V=2.835 7(9) nm3，Z=4，Dc=1.454 g·cm-3，μ(Mo Kα)=1.784 mm-1，F(000)=1 248，R1=0.044 9，wR2=0.124 1(I>2σ(I))和R1=0.088 7，wR2=0.175 6(对所有的衍射)。共收集15 802个衍射点，其中独立衍射点4 885个，可观察衍射(I>2σ(I))点2 733个用于结构精修。中心Sn原子形成五配位畸变三角双锥构型，分子间通过N…H-O氢键作用形成二维网络结构。利用量子化学G98W软件，在Lanl2dz基组对配合物的稳定性、前沿分子轨道组成及能量进行研究。 | |
| 关键词: 有机锡氧化合物 合成 晶体结构 量子化学 | |
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| Abstract: A novel organooxotin complex of di-μ-oxygen and di-μ-hydroxyl bridged tetra(bisbutyltin) bis(pyridine-4-carboxylate) has been synthesized by the reaction of n-Bu2SnO with pyridine-4-carboxylic acid and characterized by IR, 1H NMR spectra and elemental analysis. The crystal structure has been determined by X-ray diffraction. It crystallizes in the monoclinic, space group P21/n with a=1.306 5(3) nm, b=1.314 5(2) nm, c=1.660 8(3) nm, β=96.180(5)°, V=2.835 7(9) nm3, Z=4, Dc=1.454 g·cm-3, μ(Mo Kα)=1.784 mm-1, F(000)=1 248, R1=0.044 9, wR2=0.124 1 (I>2σ(I) observed reflections) and R1=0.088 7, wR2=0.175 6 (all reflections). A total of 4 885 (Rint=0.032 1) unique reflections were collected, of which 2 733 with I>2σ(I) were observed. The crystal structure shows that the central Sn atom is five-coordinated to assume a distorted trigonal bipyramidal configuration. The complex belongs to centrosymmetric dimer structure with four-membered central endo-cyclic Sn2O2 units in which the bridging oxygen atoms are di- and tri-coordinated, respectively. In crystal, the molecules are packed in the unit cell in two-dimensional network structure through the hydrogen bond (N…H-O) interaction between the O4-H atom and one of the nitrogen of an adjacent molecule. CCDC: 715879. | |
| Keywords: organooxotin compound synthesis crystal structure quantum chemistry | |
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| 邝代治,冯泳兰,张复兴,王剑秋.有机锡氧簇合物[(μ-O)(μ-OH)Sn2(n-Bu)4]2(C5H4NCO2)2的合成、结构和量子化学研究[J].无机化学学报,2010,26(12):2160-2164. | |
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