Kumar Rajiv, Singh R P, Singh R P
Department of Chemistry, University of Delhi, New Delhi 110007, India.
Spectrochim Acta A Mol Biomol Spectrosc. 2008 Nov 15;71(2):305-11. doi: 10.1016/j.saa.2007.12.013. Epub 2007 Dec 28.
In this study, we synthesized 1,2-di(o-aminophenoxy)ethane, as the starting material, used in the preparation of a novel hexadentate OONNOO-donor macrocyclic ligand-1,4,11,14-tetraoxo-7,8-diaza-5,6:9,10;15,16:19,20-terabezocyclododeca-8,17-iene. It has twenty membered organic framework (OF), which has been designed, synthesized and characterized. Our main findings of this paper are related to the organic framework of ligand, its capacity to digest the metal ions and the stability of metal organic framework (MOFs) with cobalt(II), nickel(II) and manganese(II). The authenticity of the used organic framework and its metal complexes have been detected and observed in solid state as well as in aqueous solutions. The main observations were made on the basis of physiochemical measurements viz.: elemental analyses, molar conductance measurements, magnetic susceptibility measurements, IR, 1H NMR, 13C NMR, mass spectroscopy, electronic, ESR spectroscopy. In addition, the magnetic susceptibility and electrochemistry measurements have been made. The 1H NMR spectra suggest stereochemistry and proton movement interaction. Considering the used organic framework there are a lot of carbon atoms in the molecule reflected by the 13C NMR spectrum. All these observations gave a clear view to confirming the encapsulation; arrive at the composition, structure and geometry of encapsulated complexes. In simple words, it confirms the host/guest coordination and its stability. Electrochemical properties of the complexes have been investigated to confirm the various changes in oxidation state of metals with change in potentials with respect to current at different scan rate.
在本研究中,我们合成了1,2-二(邻氨基苯氧基)乙烷作为起始原料,用于制备一种新型六齿OONNOO供体大环配体——1,4,11,14-四氧代-7,8-二氮杂-5,6:9,10;15,16:19,20-四环十二碳-8,17-二烯。它具有二十元有机骨架(OF),该骨架已被设计、合成和表征。本文的主要研究结果涉及配体的有机骨架、其消化金属离子的能力以及钴(II)、镍(II)和锰(II)金属有机骨架(MOF)的稳定性。所使用的有机骨架及其金属配合物的真实性已在固态以及水溶液中进行了检测和观察。主要观察结果是基于物理化学测量得出的,即:元素分析、摩尔电导率测量、磁化率测量、红外光谱、1H核磁共振、13C核磁共振、质谱、电子光谱、电子顺磁共振光谱。此外,还进行了磁化率和电化学测量。1H核磁共振谱表明了立体化学和质子移动相互作用。考虑到所使用的有机骨架,13C核磁共振谱反映出分子中有许多碳原子。所有这些观察结果为确认包封情况、确定包封配合物的组成、结构和几何形状提供了清晰的视角。简而言之,它证实了主体/客体配位及其稳定性。已对配合物的电化学性质进行了研究,以确认在不同扫描速率下,随着电位相对于电流的变化,金属氧化态的各种变化。