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第12族金属单硒代羧酸盐:合成、表征、结构及其向金属硒化物(MSe;M = Zn、Cd、Hg)纳米颗粒的转化

Group 12 metal monoselenocarboxylates: synthesis, characterization, structure and their transformation to metal selenide (MSe; M = Zn, Cd, Hg) nanoparticles.

作者信息

Kedarnath Gotluru, Kumbhare Liladhar B, Jain Vimal K, Phadnis Prasad P, Nethaji Munirathinam

机构信息

Chemistry Division, Bhabha Atomic Research Centre, Mumbai, 400085, India.

出版信息

Dalton Trans. 2006 Jun 14(22):2714-8. doi: 10.1039/b517224a. Epub 2006 Mar 13.

DOI:10.1039/b517224a
PMID:16804584
Abstract

Reactions of [MCl2(tmeda)] with potassium salts of monoselenocarboxylic acids gave complexes of the general formula [M(SeCOR)2(tmeda)] (M = Zn, Cd; R = Ph, Tol; Tol = C6H4-p-CH3; tmeda = Me2NCH2CH2NMe2). The analogous mercury complexes were unstable at room temperature and afforded HgSe nanoparticles during the course of reaction. All the complexes were characterized by elemental analysis, IR, UV-vis, NMR (1H, 13C, 77Se, 113Cd) data. The X-ray structural analysis of [Cd(SeCOPh)2(tmeda)] revealed that the complex is a discrete monomer having an approximate tetrahedral coordination environment around the central metal atom with monodentate (Se-bonded) selenocarboxylates. Thermal behavior of these complexes was studied by TG analysis. Pyrolysis in a furnace or in HDA (hexadecylamine) gave MSe nanoparticles, which were characterized by XRD, EDAX, SEM and absorption spectroscopy.

摘要

[MCl2(tmeda)]与单硒代羧酸的钾盐反应生成通式为[M(SeCOR)2(tmeda)]的配合物(M = Zn、Cd;R = Ph、Tol;Tol = C6H4-p-CH3;tmeda = Me2NCH2CH2NMe2)。类似的汞配合物在室温下不稳定,在反应过程中生成HgSe纳米颗粒。所有配合物均通过元素分析、红外光谱、紫外可见光谱、核磁共振(1H、13C、77Se、113Cd)数据进行表征。[Cd(SeCOPh)2(tmeda)]的X射线结构分析表明,该配合物是一种离散单体,中心金属原子周围具有近似四面体配位环境,含单齿(硒键合)硒代羧酸盐。通过热重分析研究了这些配合物的热行为。在炉中或在十六胺(HDA)中热解得到MSe纳米颗粒,通过X射线衍射、能量散射X射线光谱、扫描电子显微镜和吸收光谱对其进行了表征。

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