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首页> 外文期刊>Dalton transactions: An international journal of inorganic chemistry >Tin(II) ketoacidoximates: synthesis, X-ray structures and processing to tin(II) oxide
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Tin(II) ketoacidoximates: synthesis, X-ray structures and processing to tin(II) oxide

机译：酮酸肟酸锡（II）：合成，X射线结构和氧化锡工艺

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摘要

Tin(II) ketoacidoximates of the type [HON=CRCOO](2)Sn (R = Me 1, CH2Ph 2) and (MeON=CMeCOO)(3)Sn](-) NH4+center dot 2H(2)O 3 were synthesized by reacting pyruvate-and hydroxyl- or methoxylamine RONH2 (R = H, Me) with tin(II) chloride dihydrate SnCl2 center dot 2H(2)O. The single crystal X-ray structure reveals that the geometry at the Sn atom is trigonal bipyramidal in 1, 2 and trigonal pyramidal in 3. Inter- or intramolecular hydrogen bonding is observed in 1-3. Thermogravimetric (TG) analysis shows that the decomposition of 1-3 to SnO occurs at ca. 160 degrees C. The evolved gas analysis during TG indicates complete loss of the oximato ligand in one step for 1 whereas a small organic residue is additionally removed at temperatures >400 degrees C for 2. Above 140 degrees C, [HON=C(Me)COO](2)Sn (1) decomposes in air to spherical SnO particles of size 10-500 nm. Spin coating of 1 on Si or a glass substrate followed by heating at 200 degrees C results in a uniform film of SnO. The band gap of the produced SnO film and nanomaterial was determined by diffuse reflectance spectroscopy to be in the range of 3.0-3.3 eV. X-ray photoelectron spectroscopy indicates surface oxidation of the SnO film to SnO2 in ambient atmosphere.
机译：[HON = CRCOO]（2）Sn（R = Me 1，CH2Ph 2）和（MeON = CMeCOO）（3）Sn]（-）NH4 +中心点2H（2）O 3的锡（II）酮酸肟酸酯通过使丙酮酸和羟基或甲氧基胺RONH2（R = H，Me）与二水合氯化锡（II）SnCl2中心点2H（2）O反应合成。 X射线单晶结构表明，Sn原子的几何形状在1、2中为三角双锥体，在3中为三角锥体。在1-3中观察到分子间或分子内氢键。热重分析（TG）表明，大约1-3分解为SnO。 160℃。TG中析出的气体分析表明，一步反应1中的肟基配体完全丧失，而在> 400℃的温度下2去除了少量有机残留物。高于140℃，[HON = C（Me ）（COO]（2）Sn（1）在空气中分解成大小为10-500 nm的球形SnO颗粒。在Si或玻璃基板上旋涂1，然后在200摄氏度下加热，得到均匀的SnO膜。通过漫反射光谱法确定所制备的SnO膜和纳米材料的带隙在3.0-3.3eV的范围内。 X射线光电子能谱表明在环境大气中SnO膜表面氧化成SnO2。

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