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。