Stroek Wowa, Rowlinson Nathalie A V, Hudson Luke A, Albrecht Martin
Department of Chemistry, Biochemistry and pharmaceutical sciences, University of Bern, Bern CH-3012, Switzerland.
Inorg Chem. 2024 Sep 16;63(37):17134-17140. doi: 10.1021/acs.inorgchem.4c02827. Epub 2024 Sep 3.
N-Heterocyclic carbenes have proven to be excellent ligands for transition metals, with numerous applications in catalysis and beyond. However, they have also displayed lability with first row transition metals, largely due to the hard-soft mismatch of the metal-carbon bond. Chelation is often considered a suitable methodology for supporting the labile M-C bond through the introduction of a strongly coordinating donor site such as hard phenolates. Herein, we demonstrate that chelating phenolate-carbene ligands are kinetically labile in iron(II) complexes. Specifically, heteroleptic iron complexes [Fe(C^O)(N^N)] were synthesized composed of a phenolate-functionalized triazolylidene (CO) ligand and ,bidentate coordinating bisoxazoline ligand (N^N). Stability studies by H NMR spectroscopy showed that the heteroleptic complexes preferentially convert to their corresponding homoleptic complexes [Fe(C^O)] and [Fe(N^N)], indicating reversible decoordination of the carbene phenolate chelate from the iron center. The rate of this rearrangement is dependent on the substituents on the ligands and increases for triazolylidene wingtip groups mesityl (Mes) < di(isopropyl)aryl (DIPP) < adamantyl (Ad), with significant ligand redistribution for DIPP and Ad systems observed even at room temperature. The most stable heteroleptic complex featured mesityl wingtips on the triazole and phenyl groups as oxazoline substituents and displayed signs of ligand exchange only after 16 h at room temperature. This substitutional lability of carbene ligands even when supported by a phenolate chelating group has direct consequences when designing iron complexes for catalytic applications.
N-杂环卡宾已被证明是过渡金属的优良配体,在催化及其他领域有众多应用。然而,它们与第一行过渡金属形成的配合物也表现出不稳定性,这主要归因于金属-碳键的硬软不匹配。螯合作用通常被认为是一种合适的方法,通过引入强配位供体位点(如硬酚盐)来稳定不稳定的M-C键。在此,我们证明了螯合酚盐-卡宾配体在铁(II)配合物中动力学上是不稳定的。具体而言,合成了由酚盐官能化的三唑亚基(CO)配体和双齿配位双恶唑啉配体(N^N)组成的杂配铁配合物[Fe(C^O)(N^N)]。通过核磁共振氢谱进行的稳定性研究表明,杂配配合物优先转化为其相应的均配配合物[Fe(C^O)]和[Fe(N^N)],这表明卡宾酚盐螯合物从铁中心发生了可逆的去配位。这种重排的速率取决于配体上的取代基,对于三唑亚基翼尖基团,重排速率按如下顺序增加:均三甲苯基(Mes)<二(异丙基)芳基(DIPP)<金刚烷基(Ad),即使在室温下,DIPP和Ad体系也观察到了显著的配体重新分布。最稳定的杂配配合物在三唑上具有均三甲苯基翼尖,恶唑啉取代基为苯基,仅在室温下放置16小时后才显示出配体交换的迹象。当设计用于催化应用的铁配合物时,即使有酚盐螯合基团的支持,卡宾配体的这种取代不稳定性也会产生直接影响。