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Imidazolidine ligands and their coordination behaviour towards the fac-[Re(CO)3]+ core: Unusual synthetic route, spectroscopic and X-Ray crystallographic characterization
Journal of Organometallic Chemistry ( IF 2.1 ) Pub Date : 2019-11-20 , DOI: 10.1016/j.jorganchem.2019.121033
G. Habarurema , J. Mukiza , T.I.A. Gerber , T. Mukabagorora , E.C. Hosten , R. Betz

Rhenium(I) complexes with benzimidazolidines, imidazolidines and their derivatives are reported. This study highlights the unusual synthetic route that led to a series of the unexpected ring-containing benzimidazolidines and imidazolidines, obtained from the reaction of ketone and diamino-containing compounds. The reaction of the bridging pyridyl; 2,2′-dipyridylketone (dpk) with 1,2-diaminobenzene and 1,2-diaminoethane in methanol led to the isolation of 2,3-dihydro-2,2-di(pyridin-2-yl)-1H-benzo[d]imidazole (H2dpb) and 2-(2-(pyridine-2-yl)imidazolidin-2-yl)pyridine (H2pip) respectively. The compounds fac-[Re(CO)3(H2dmb)Cl] (1) and fac-[Re(CO)3(H2pip)]Cl.H2O (2) were isolated in good yield by reacting [Re(CO)5Cl] with 2,3-dihydro-2,2-di(pyridin-2-yl)-1H-benzo[d]imidazole (H2dpb) and 2-(2-(pyridine-2-yl)imidazolidin-2-yl)pyridine (H2pip) in toluene respectively. A surprising aspect of fac-[Re(CO)3(H2dmb)Cl] (1) is the benzimidazolidine ring opening in H2dpb, which resulted in the formation of the neutrally coordinated Schiff-base ligand, N1-(di(pyridine-2-yl)methylene)benzene-1,2-diamine (H2dmb), which acts as a bidentate N,N-donor chelate. On other hand, the H2pip ligand did not undergo any modification. Therefore, it acted as a tridentate N3,O-donor ligand towards the cationic cluster compound with a fac-[Re(CO)3]+ core. The crystal structure of H2dpb, 1 and 2 were determined by X-ray single crystal diffraction, in addition to IR, 1H NMR and electronic analysis.



中文翻译:

咪唑烷配体及其对fac- [Re(CO)3 ] +核的配位行为:异常的合成路线,光谱学和X射线晶体学表征

with与苯并咪唑烷,咪唑烷及其衍生物的配合物。这项研究突显了一种异常的合成路线,该路线导致了一系列从酮和含二氨基化合物的反应中获得的出乎意料的含环苯并咪唑烷和咪唑烷。桥联吡啶的反应;2,2'- dipyridylketone(DPK)与1,2-二氨基苯和1,2-二氨基乙烷在甲醇导致2,3-二氢-2,2-二(吡啶-2-基)-1-的隔离ħ -苯并[ d ]咪唑(H 2 dpb)和2-(2-(吡啶-2-基)咪唑啉丁-2-基)吡啶(H 2 pip)。化合物fac- [Re(CO)3(H 2 dmb)Cl](1)和通过[Re(CO)5 Cl]与2,3-二氢-2,2-di()的反应以高收率分离出fac- [Re(CO)3(H 2 pip)] Cl.H 2 O(2)。吡啶-2-吡啶基)-1 H-苯并[ d ]咪唑(H 2 dpb)和2-(2-(吡啶-2-基)咪唑烷基-2-基)吡啶(H 2 pip)。fac- [Re(CO)3(H 2 dmb)Cl](1)的一个令人惊讶的方面是H 2 dpb中的苯并咪唑烷开环,导致形成了中性配位的席夫碱配体N 1-(二(吡啶-2-基)亚甲基)苯-1,2-二胺(H 2 dmb),其作为双齿N,N-给体螯合物。另一方面,H 2 pip配体没有进行任何修饰。因此,它充当具有fac- [Re(CO)3 ] +核心的阳离子簇化合物的三齿N 3,O供体配体。除了IR,1 H NMR和电子分析以外,还通过X射线单晶衍射测定了H 2 dpb,12的晶体结构。

更新日期:2019-11-20
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