Synthesis and Characterization of Transition Metal Complex Cation Heptaborate Structures

Ahmet Genç, D. A. Köse, O. Şahin
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Abstract

Heptaborate structures with transition metal complex cations were synthesized and characterized using elemental analysis, melting point determination, FT-IR, TGA/DTA analysis, UV analysis, x-ray diffraction (XRD) analysis methods. In the infrared spectra of heptaborate salt structures, peaks of (-M-N)phen and (-M-N)pyrd stretching vibrations, which indicate the presence of transition metal complex, were observed. As the characteristic vibrations of the heptaborate structure, the -OH peaks of the B-OH bonds present in the structures and the asymmetric and symmetrical stretching vibrations, which confirm the presence of four trigonal borate molecules in the structures, appeared as sharp peaks. It was observed that the thermal analysis decomposition curves of heptaborate salt structures with transition metal complex cations were similar. Depending on the similar degradation characteristics of the molecules, it is seen that the hydrate waters settled outside the coordination sphere in all structures move away from the structures in a single step. As the second degradation step of heptaborate salt structures, the removal of water in amounts that can be attributed to the removal of -OH groups in the borate rings in the form of water vapor in all structures was detected. It was seen that this degradation step took place in a single step in all structures and the related experimental theoretical mass losses were compatible with each other. Combustion degradation of organic ligands was observed as the final degradation step of heptaborate salt structures with metal cation complexes. While peaks belonging to heptaborate rings were observed from the recorded powder x-ray diffraction patterns, electronic transition data also supported that the metal cation complex was in octahedral geometry.
过渡金属络合阳离子七硼酸盐结构的合成与表征
采用元素分析、熔点测定、傅立叶变换红外光谱、TGA/DTA 分析、紫外分析和 X 射线衍射 (XRD) 分析方法合成了带有过渡金属配合物阳离子的七硼酸盐结构,并对其进行了表征。在庚硼酸盐结构的红外光谱中,观察到 (-M-N)phen 和 (-M-N)pyrd 伸缩振动峰,这表明过渡金属络合物的存在。作为七硼酸盐结构的特征振动,结构中存在的 B-OH 键的 -OH 峰以及不对称和对称伸缩振动出现了尖锐的峰值,这证实了结构中存在四个三叉硼酸盐分子。据观察,带有过渡金属复合阳离子的庚硼酸盐结构的热分析分解曲线相似。根据分子相似的降解特征,可以看出在所有结构中沉淀在配位层外的水合物水会一步步地远离结构。在七硼酸盐结构的第二个降解步骤中,检测到所有结构中的水都以水蒸气的形式从硼酸盐环中的-OH基团中移除,移除的水量可归因于硼酸盐环中的-OH基团。可以看出,在所有结构中,这一降解步骤都是一步完成的,而且相关的实验理论质量损失相互吻合。有机配体的燃烧降解是含有金属阳离子络合物的庚硼酸盐结构的最终降解步骤。从记录的粉末 X 射线衍射图样中可以观察到属于七硼酸盐环的峰值,电子转变数据也证明金属阳离子复合物呈八面体几何形状。
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