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Iron and Silver Complexes of 4‐(Imidazol‐1‐yl)‐2,6‐di(pyrazol‐1‐yl)‐pyridine (L), Including a [Fe3(µ‐F)2F6L8]+ Assembly
European Journal of Inorganic Chemistry ( IF 2.2 ) Pub Date : 2020-09-10 , DOI: 10.1002/ejic.202000782
Izar Capel Berdiell 1 , Rafal Kulmaczewski 1 , Stuart L. Warriner 1 , Oscar Cespedes 2 , Malcolm A. Halcrow 1
Affiliation  

Treatment of 2,4,6‐trifluoropyridine with sodium imidazolate, then 2 equiv. sodium pyrazolate, in two reaction steps yields the title ligand L in 40 % overall yield. Crystalline [FeL2][BF4]2 and [FeL2][ClO4]2 are isostructural high‐spin complexes, with highly twisted six‐coordinate geometries and pendant imidazolyl groups. Conversely, [Ag(µ‐L)]BF4·0.5MeCN is a linear coordination polymer of distorted square planar silver ions linked by κ13,µ‐L ligands. Some samples of [FeL2][BF4]2 were contaminated by [FeIII3(µ‐F)2F6L8]BF4, which was prepared in pure form following reaction of Fe[BF4]2·6H2O, Na3[FeF6] and L in appropriate ratios. The linear [{trans‐FeFL4}2(µ‐F)2FeF4]+ assembly is supported by monodentate L ligands coordinated through their imidazolyl donors, and donating C–H····F interactions to the central [FeF6]3– moiety. The cluster exhibits moderate antiferromagnetic coupling between its iron(III) centres.

中文翻译:

Iron and Silver Complexes of 4‐(Imidazol‐1‐yl)‐2,6‐di(pyrazol‐1‐yl)‐pyridine (L), Including a [Fe3(µ‐F)2F6L8]+ Assembly

Treatment of 2,4,6‐trifluoropyridine with sodium imidazolate, then 2 equiv. sodium pyrazolate, in two reaction steps yields the title ligand L in 40 % overall yield. Crystalline [FeL2][BF4]2 and [FeL2][ClO4]2 are isostructural high‐spin complexes, with highly twisted six‐coordinate geometries and pendant imidazolyl groups. Conversely, [Ag(µ‐L)]BF4·0.5MeCN is a linear coordination polymer of distorted square planar silver ions linked by κ13,µ‐L ligands. Some samples of [FeL2][BF4]2 were contaminated by [FeIII3(µ‐F)2F6L8]BF4, which was prepared in pure form following reaction of Fe[BF4]2·6H2O, Na3[FeF6] and L in appropriate ratios. The linear [{trans‐FeFL4}2(µ‐F)2FeF4]+ assembly is supported by monodentate L ligands coordinated through their imidazolyl donors, and donating C–H····F interactions to the central [FeF6]3– moiety. The cluster exhibits moderate antiferromagnetic coupling between its iron(III) centres.
更新日期:2020-09-10
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