Department of Chemistry, Faculty of Sciences, Tarbiat Modares University, P.O. Box 14115-4838, Tehran, Islamic Republic of Iran.
Department of Chemistry, Faculty of Science, University of Qom, P.O. Box 37185-359, Qom, Islamic Republic of Iran.
Ultrason Sonochem. 2017 Mar;35(Pt A):226-232. doi: 10.1016/j.ultsonch.2016.09.022. Epub 2016 Sep 28.
A sonochemical method by using various time and concentrations of initial reagents and power of irradiation, was used to synthesize nano-card house of a new copper(II) metal-organic coordination system, {[Cu(p-2yeinh)Cl]·(HO)} (1), where p-2yeinh=pyridin-2-yl ethylidene-isonicotinohydrazide. The compound was characterized by scanning electron microscopy (SEM), elemental analysis, IR spectroscopy, X-ray powder diffraction (XPRD), and single crystal X-ray analysis. The X-ray structure revealed that the Cu(II) atom is coordinated by one oxygen and three nitrogen atoms from two p-2yeinh ligands and one chloride anion with a CuNOCl donor set with square pyramid geometry. This arrangement produces a large quadric nuclear square ring composed of four square pyramid Cu(II) moieties linked together by two p-2yeinh units (M4L4). The adjacent frameworks connected by strong hydrogen bonding interactions of methanol molecules that interact together and with the rings and π-π interactions of adjacent aromatic rings of p-2yeinh and other weak interactions. Consequently, the labile interactions also allow the discrete structure to form a 3D metal-organic coordination network. CuO nanoparticles were obtained by thermolysis of 1 at 180°C with oleic acid as a surfactant. The average diameter of the nanoparticles was estimated by XPRD to be 38nm. The morphology and size of the prepared CuO nanoparticles were further studied using SEM.
采用不同的初始试剂浓度和辐照功率的超声化学方法，合成了一种新型的铜（II）金属有机配位体系的纳米卡片屋，[Cu(p-2yeinh)Cl]·(HO)}（1），其中 p-2yeinh=pyridin-2-yl ethylidene-isonicotinohydrazide。该化合物通过扫描电子显微镜（SEM）、元素分析、红外光谱、X 射线粉末衍射（XPRD）和单晶 X 射线分析进行了表征。X 射线结构表明，Cu(II)原子与两个 p-2yeinh 配体和一个氯离子配位，形成 CuNOCl 给体集，具有四方锥几何形状。这种排列产生了一个由四个四方锥 Cu(II)部分组成的大四元核正方形环，由两个 p-2yeinh 单元（M4L4）连接在一起。相邻的骨架通过甲醇分子的强氢键相互作用连接在一起，与 p-2yeinh 的环和相邻芳环的π-π相互作用以及其他弱相互作用相互作用。因此，不稳定的相互作用也允许离散结构形成 3D 金属有机配位网络。在 180°C 下，通过热解 1 并用油酸作为表面活性剂，可以得到 CuO 纳米粒子。通过 XPRD 估算纳米粒子的平均直径为 38nm。通过 SEM 进一步研究了制备的 CuO 纳米粒子的形态和尺寸。
