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Published April 20, 2009 | Supplemental Material
Journal Article Open

Synthesis and Characterization of Iron Derivatives Having a Pyridine-Linked Bis(anilide) Pincer Ligand


A pyridine-linked bis(aniline) pincer ligand, [2]H_2 ([2]H_2 = (2,6-NC_5H_3(2-(2,4,6-Me_3C_6H_2)-NHC6H4)2), has been synthesized in two steps. Deprotonation with Me_3SiCH_2Li followed by metalation with FeCl_2 yielded a LiCl adduct of [2]Fe. The complex is freed of LiCl with excess TlPF_6 or by crystallization from toluene/petroleum ether, giving [2]Fe(THF). [2]Fe(THF) reacts with I_2 and O_2 to generate [2]FeI and ([2]Fe)_2O, respectively. The complexes have been characterized by ^1H NMR spectroscopy, elemental analysis, X-ray crystallography, and UV−vis spectroscopy. [2]Fe(THF) has been examined using cyclic voltammetry.

Additional Information

© 2009 American Chemical Society. Received January 15, 2009. Publication Date (Web): March 20, 2009. We thank Larry Henling and Dr. Mike Day for their assistance with crystallographic characterization. The Bruker KAPPA APEXII X-ray diffractometer was purchased via an NSF CRIF:MU award to the California Institute of Technology, CHE-0639094. We also thank Dr. Aaron Wilson for his help with electrochemical methods. We are grateful to the USDOE Office of Basic Energy Sciences (Grant DE-FG03-85ER13431) and the Moore Foundation for financial support. Supporting Information Available: UV-vis spectra, diffraction data, and voltammograms. Crystallographic data in CIF file format. This material is available free of charge via the Internet at http://pubs.acs.org.

Attached Files

Supplemental Material - Weintrob2009p2408Inorg_Chem_supp.pdf

Supplemental Material - ic900083s_si_002.cif


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August 20, 2023
October 19, 2023