Citation: Mengdan YU, Hailong WANG, Mookan NATARAJAN, Kangyu LOU, Zhiyin XIAO, Chunxin LU, Wei ZHONG, Xiaoming LIU. Influence of the pendant amine base in iron complexes on the ligand exchange reaction and electrocatalytic activity for proton reduction[J]. Chinese Journal of Inorganic Chemistry, ;2026, 42(11): 2459-2474. doi: 10.11862/CJIC.20260129 shu

Influence of the pendant amine base in iron complexes on the ligand exchange reaction and electrocatalytic activity for proton reduction

Mengdan YU ^{1, 2} ,
Hailong WANG ¹ ,
Mookan NATARAJAN ¹ ,
Kangyu LOU ¹ ,
Zhiyin XIAO ^1,, ,
Chunxin LU ¹ ,
Wei ZHONG ^1,, ,
Xiaoming LIU ¹

1.
College of Biological, Chemical Sciences and Engineering, Jiaxing University, Jiaxing, Zhejiang 314001, China
2.
College of Chemical Engineering, Zhejiang University of Technology, Hangzhou 310014, China

Corresponding author: Zhiyin XIAO, zhiyin.xiao@zjxu.edu.cn Wei ZHONG, weizhong@zjxu.edu.cn
Received Date: 14 April 2026
Revised Date: 29 July 2026

Figures(10)

A series of cyclopentadienyl iron(Ⅱ) complexes of bidentate phosphine ligands bearing pendant amine bases, R-N(CH₂P(Ph)₂)₂ [L_n: n=1 (R=n-propyl), 2 (R=benzyl), 3 (R=o-CH₂Py)], were synthesized: [CpFe(L_n)I] (1a-1c: n=1-3), [CpFe(L_n)(NCMe)]I (2a-2c: n=1-3), and [CpFe(L_n)(NCMe)]PF₆ (3a-3c: n=1-3), to mimic the structure and function of the distal iron unit in the diiron active site of [FeFe]-hydrogenases. By varying the R substituents of pendant amines, we aimed to investigate how amine basicity regulates the reactivity of these iron complexes. The iodo complexes 1a-1c underwent facile ligand substitution by MeCN, affording iodide complexes 2a-2c. The returns from 2a-2c to 1a-1c in chloroform were spectroscopically probed to demonstrate a linear correlation between rate constants and the pK_a values of the pendant amines. Nevertheless, the returns were completely inhibited in the hexafluorophosphate (PF₆^-) complexes 3a-3c. Further insights from electrochemical investigations revealed that one-electron reduction of the Fe(Ⅱ) complexes leads to the formation of 17-electron Fe(Ⅰ) species, whereby an additional chemical process should be involved to liberate the labile ligand (I^- or MeCN) from the metal centre to result in a precious vacancy. The observation was corroborated by density functional theory (DFT) calculations, which predicted the creation of a vacant site at the intermediate upon reduction. Particularly, the electrocatalytic activity of these iron complexes towards proton reduction was found to be significantly influenced by the basicity of the pendant amine, whereas low basic amines generally result in high efficiency. Our results revealed the crucial role of the substituent on the pendant amine in manipulating the chemistry of metal-based ligand exchange as well as electrocatalytic proton reduction.
- iron(Ⅱ),
- diphosphine,
- pendant amine,
- ligand exchange,
- proton reduction
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沈阳化工大学材料科学与工程学院沈阳 110142