Sascha A. Schäfer, Rose Jordan, Katharina M. Klupsch, Felix Carl-Heinz Herwede, Axel Klein
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引用次数: 0
摘要
在合成多用途前体 (NMe4)[Ni(CF3)3(MeCN)] 时,我们最近遇到了一个问题:在所选反应条件下,大量的 C2F5 取代 CF3 加入,形成了混合配体镍酸盐 [Ni(CF3)x(C2F5)y(MeCN)]- (x + y = 3)。我们利用 19F 核磁共振 (NMR) 光谱和单晶 X 射线衍射研究了 y = 0、1 或 2 的三种产物。通过修改实验条件,我们追溯到了反应机理并解决了问题。
Synthesis of Tris(trifluoromethyl)nickelates(II)—Coping with “The C2F5 Problem”
When synthesizing the versatile precursors (NMe4)[Ni(CF3)3(MeCN)] we recently encountered the problem that marked amounts of C2F5 were incorporated instead of CF3 under the chosen reaction conditions forming mixed-ligand nickelates [Ni(CF3)x(C2F5)y(MeCN)]− (x + y = 3). We studied the three products with y = 0, 1, or 2, using 19F nuclear magnetic resonance (NMR) spectroscopy and single-crystal X-ray diffraction. We were able to trace the reaction mechanism and solve the problem by modifying the experimental conditions.
期刊介绍:
Inorganics is an open access journal that covers all aspects of inorganic chemistry research. Topics include but are not limited to: synthesis and characterization of inorganic compounds, complexes and materials structure and bonding in inorganic molecular and solid state compounds spectroscopic, magnetic, physical and chemical properties of inorganic compounds chemical reactivity, physical properties and applications of inorganic compounds and materials mechanisms of inorganic reactions organometallic compounds inorganic cluster chemistry heterogenous and homogeneous catalytic reactions promoted by inorganic compounds thermodynamics and kinetics of significant new and known inorganic compounds supramolecular systems and coordination polymers bio-inorganic chemistry and applications of inorganic compounds in biological systems and medicine environmental and sustainable energy applications of inorganic compounds and materials MD