Synthesis, Characterization, and Crystal Structure of a Diorganotin(IV) Complex with 2-Oxo-2-Phenylacetic Acid 4-Hydroxybenzohydrazone.

ISRN Organic Chemistry Pub Date : 2011-04-11 eCollection Date: 2011-01-01 DOI:10.5402/2011/708162
Jing Li, Handong Yin, Min Hong
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引用次数: 2

Abstract

The complex dibutyltin 2-oxo-2-phenylacetic acid 4-hydroxybenzohydrazone has been synthesized and characterized by elemental analysis, IR, (1)H and (13)C NMR, and X-ray single-crystal diffraction studies. The crystal structure belongs to triclinic, space group P-1 with a = 9.3220 (10) Å, b = 9.8779 (11) Å, c = 15.9401 (17) Å, β = 97.0930 (10)°, Z = 2, V = 1427.6(3) Å(3), Dc = 1.413 mg/cm(3), μ = 0.936 mm(-1), F(000) = 628, R = 0.1158, and wR = 0.2522. X-ray analysis indicates that O(2), N(2), O(4), and O(4)#1 from the ligand and O(5) from ethanol molecule are in the equatorial positions; the axial positions are occupied by two n-butyl groups. It shows a distorted pentagonal bipyramid configuration with seven-coordination for central tin atom. Fascinatingly, the supramolecular infrastructures are observed, which exist as two-dimensional sheets assembled from the organometallic subunits through intermolecular and intramolecular O-H⋯X or C-H⋯X (X = O or N) hydrogen bonds.

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二有机锡-2-氧-2-苯乙酸- 4-羟基苯并腙配合物的合成、表征和晶体结构
合成了配合物二丁基锡2-氧-2-苯乙酸4-羟基苯腙,并通过元素分析、IR、(1)H和(13)C NMR和x射线单晶衍射对其进行了表征。晶体结构为三斜型,空间群P-1, a = 9.3220 (10) Å, b = 9.8779 (11) Å, c = 15.9401 (17) Å, β = 97.0930(10)°,Z = 2, V = 1427.6(3) Å(3), Dc = 1.413 mg/cm(3), μ = 0.936 mm(-1), F(000) = 628, R = 0.1158, wR = 0.2522。x射线分析表明,配体上的O(2)、N(2)、O(4)、O(4)#1和乙醇分子上的O(5)位于赤道位;轴向位置由两个正丁基占据。中心锡原子呈七配位畸变五边形双棱锥构型。令人着迷的是,超分子基础结构被观察到,它们存在于由有机金属亚基通过分子间和分子内O- h⋯X或C-H⋯X (X = O或N)氢键组装的二维薄片中。
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