Synthesis and Structural Studies of (h3-allyl)carbonylnitrosyl Triphenylphosphine Iron Complexes

Misbah Tabassam,Zaid Mehmood,Liviu Mitu,Muhammad Imran,Syeda Robina Gillani,Amna Farooq,Asad Gulzar

doi:10.37358/rc.70.19.11.7666

Abstract

In this paper we report the preparation of two (h3-allyl)carbonylnitrosyltriphenylphosphine iron complexes i.e.(p-allyl)carbonylnitrosyltriphenylphosphine iron (1) and (2-methyl-p-allyl) carbonylnit rosyltriphenylphosphine iron (2). These complexes (1) and (2) were prepared by reacting (p-allyl)dicarbonylnitrosyl iron and (2-methyl-p-allyl)dicarbonylnitrosyl iron with triphenylphosphine under inert atmospheric conditions. Both the resulting complexes were sufficiently and well characterized by IR, 1H NMR, 13C NMR, ESI/MS, HRMS and single crystal XRD. Triphenylphosphine ligand was found to be strong sigma donor and replaced carbonyl ligand readily. XRD revealed that the geometry of iron in both complexes is distorted octahedral.

Highlights

In this paper we report the preparation of two (η3-allyl)carbonylnitrosyltriphenylphosphine iron complexes i.e.(π-allyl)carbonylnitrosyltriphenylphosphine iron (1) and (2-methyl-π-allyl) carbonylnit rosyltriphenylphosphine iron (2)
The allyl ligand is of great interest and has been widely used in several synthesis and transition metal mediated reactions [1]
Catalysis based on such metal complexes has been recognized as powerful synthetic tool in organic synthesis

Summary

Experimental part Material and methods

All the reactions and necessary manipulations which are sensitive to air and moisture were performed with rigorous exclusion of air and moisture under an atmosphere of dry nitrogen by using high vacuum Schlenk techniques. Low resolution mass spectrometry (LRMS) and High resolution mass spectrometry (HRMS) of the allyl iron complexes was done using BRUCKER Type microTOF-Q (ESI). The synthesized complexes (1) and (2) were purified by suitable techniques and characterized by infrared, nuclear magnetic resonance spectroscopy, low resolution mass and high resolution mass spectrometry. Both the complexes (1) and (2) are colored solids (red, 1; orange, 2) and sensitive towards air and moisture, all work up was carried out in an inert atmosphere. The IR spectra of carbonylnitrosyl(η3-allyl)triphenylphosphine iron complexes (1), (2) show absorption bands in the range of 1917 cm-1 to 1902 cm×1 and 1655 cm-1 to 1686 cm×1 which can be assigned to carbonyl stretching and nitrosyl stretching respectively [10]

NMR studies and Mass spectrometry

Conclusions