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Synthesis and Structural Characterisation of an N-Phosphanyl Ferrocene Carboxamide and its Ruthenium, Rhodium and Palladium Complexes.
ChemPlusChem ( IF 3.4 ) Pub Date : 2020-06-02 , DOI: 10.1002/cplu.202000303
Michal Navrátil 1 , Ivana Císařová 1 , Adam Alemayehu 1 , Karel Škoch 1 , Petr Štěpnička 1
Affiliation  

[((Diphenylphosphanyl)amino)carbonyl]ferrocene (1 ) has been synthesized and coordinated to light platinum metals, ruthenium, rhodium and palladium, in diverse coordination modes. Specifically, compound 1 was used to prepare the following phosphane complexes, [(η6‐mes)RuCl2(1 ‐κP )], [(η5‐C5Me5)RhCl2(1 ‐κP )], trans ‐[PdCl2(1 ‐κP )2], and [(LNC)PdCl(1 ‐κP )] (mes=mesitylene, LNC=[2‐(dimethylamino‐κN )methyl]phenyl‐κC 1). They were subsequently converted into cationic O,P‐chelate complexes by halide abstraction with AgClO4 and into neutral O,P‐chelate complexes by deprotonation with potassium tert ‐butoxide. All coordination compounds and phosphane chalcogenides 1E (P‐bound chalcogen atom E=O, S and Se), which were also synthesised, were structurally characterised using spectroscopic methods (IR, multinuclear NMR and ESI MS) and single‐crystal X‐ray diffraction analysis. The electrochemical behaviour of the prepared compounds was studied by cyclic voltammetry, and the (LNC)Pd‐1 complexes were further studied by Mössbauer spectroscopy.

中文翻译:

N-膦酰基二茂铁羧酰胺及其钌,铑和钯配合物的合成和结构表征。

[((二苯基膦烷基)氨基)羰基]二茂铁(1)已经合成并以多种配位方式配位用于轻铂金属,钌,铑和钯。具体而言,化合物1被用于制备下列膦络合物,[(η 6 -Mes)的RuCl 21P)],[(η 5 -C 55)的RhCl 21P)],反式- [的PdCl 21个P2 ]和[(L NC)的PdCl(1P)](MES =均三甲苯,L NC = [2-(二甲基氨基- κ Ñ)甲基]苯基-κ Ç 1)。随后通过与AgClO 4的卤化物萃取将它们转化为阳离子O,P-螯合物,并通过丁醇钾去质子化为中性O,P-螯合物。所有的配位化合物和膦硫属元素化物1E(P结合的硫属元素原子E = O,S和Se)也已合成,使用光谱法(红外光谱,多核NMR和ESI MS)和单晶X射线衍射进行结构表征分析。所制备的化合物的电化学行为通过循环伏安法研究,和(L NC)Pd- 1络合物通过Mössbauer光谱进一步研究。
更新日期:2020-06-23
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