Synthesis, X-ray crystal structures, and electrochemistry of two diiron ethane-1,2-dithiolate complexes containing tris(4-trifluoromethylphenyl)phosphine or triethyl phosphite

Abstract

Two diiron ethane-1,2-dithiolate complexes were prepared and structurally characterized. Reactions of the parent complex [Fe₂(CO)₆(μ-SCH₂CH₂S)] (1) with tris(4-trifluoromethylphenyl)phosphine or triethyl phosphite and Me₃NO·2H₂O as the oxidative reagent resulted in the formation of the phosphine-substituted analog [Fe₂(CO)₅{P(4-C₆H₄CF₃)₃}(μ-SCH₂CH₂S)] (2) and phosphite-substituted analogue [Fe₂(CO)₅{P(OCH₂CH₃)₃}(μ-SCH₂CH₂S)] (3) in 84% and 78% yields, respectively. The new complexes 2 and 3 were characterized by elemental analysis, IR, NMR spectroscopy, and single crystal X-ray diffraction analysis. Moreover, the electrochemical properties of both complexes were studied by cyclic voltammetry.

Keywords:

• Diiron ethane-1,2-dithiolate
• [FeFe]-hydrogenases
• carbonyl substitution
• X-ray crystallography
• electrochemistry

Supplementary material

CCDC 2014367 and 2014368 contain the supplementary crystallographic data for this paper. These data can be obtained free of charge from The Cambridge Crystallographic Data Center via http://www.ccdc.cam.ac.uk/conts/retrieving.html, or from the Cambridge Crystallographic Data Center, 12 Union Road, Cambridge CB2 1EZ, UK; fax: [phone]; or e-mail: [email protected].

Additional information

Funding

This research was supported by Zhejiang Provincial Natural Science Foundation of China under Grant LY19B020002, National Natural Science Foundation of China under Grant 21501124, Science & Technology Department of Sichuan Province under Grant 2018JY0235, Education Department of Sichuan Province under Grant 18ZA0337, and Sichuan University of Science & Engineering under Grant S201910622022.