Mono- and Bi-Iron Chalcogenofumarato Complexes: Synthesis and Characterization

ABSTRACT

New series of iron(II) chalcogenofumarato-based complexes has been successfully synthesized in good yields. The mono-iron complexes CpFe(CO)₂ESCOCH=CHCOCl (E= S (1), Se (2)) were prepared from the reaction of the corresponding iron chalcogenides (µ-E_x)[CpFe(CO)₂]₂ (E= S; x = 2–4, E= Se; x = 1) with fumaryl chloride in a 1:1 molar ratio. The corresponding 2:1 (iron:ligand) reaction produced the bi-iron complexes [CpFe(CO)₂ESCO]₂(µ-CH=CH) (E= S (3), Se (4)). The complexes CpFe(CO)₂ECOCH=CHCO₂Et (E= S (5), Se (6)) were synthesized from the reaction of complexes 1 or 2 with EtOH or from the reaction of the chalcogenides with O-ethyl chlorofumarate ClCOCH=CHCO₂Et. All complexes were characterized by UV-Vis, IR, ¹H-, ¹³C{¹H}-NMR spectroscopic techniques and the crystal structures of 1, 5 and 6 were further determined by single crystal X-ray diffraction measurements.

Graphical abstract

KEYWORDS:

• Iron
• chalcogenofumarate
• crystal structures
• synthesis
• characterization

Acknowledgments

M. El-khateeb thanks Alexander von Humboldt Foundation (Germany) for scholarship and Jordan University of Science and Technology for financial support (Grant No. 48/2015).

Disclosure statement

No potential conflict of interest was reported by the author(s).

Supporting data

Crystallographic data deposited at the Cambridge Crystallographic Data Centre under CCDC-2253893 for 1, CCDC-2253894 for 5 and CCDC-2253895 for 6 contain the supplementary crystallographic data including structure factors; these data can be obtained free of charge via www.ccdc.cam.ac.uk/conts/retrieving.html (or from the Cambridge Crystallographic Data Centre, 12, Union Road, Cambridge CB2 1EZ, UK; fax: [phone]; or [email protected]).

Supplementary material

Supplemental data for this article can be accessed online at https://doi.org/10.1080/02603594.2023.2246902.

Additional information

Funding

This work was supported by the Deanship of Scientific Research, Jordan University of Science and Technology (Grant No.48/2015).