Synthesis and Characterization of Chromium-Isothiocyanate-4-Methylpyridine Complexes
The synthesis and single crystal X-ray structure of trans-[HNC6H7][Cr(NCS)4(NC6H7)2] (1) and mer-[Cr(NCS)3(NC6H7)3] (2) are reported. Compound 1 was synthesized by refluxing chromium powder and thiourea in 4-methylpyridine. The isothiocyanate ligand is believed to be generated from the isomerization of thiourea to ammonium thiocyanate during synthesis. Compound 2 was prepared from CrCl3 and KSCN in 4-methylpyridine. The reaction conditions for both compounds yielded a mixture of [Cr(NCS)x(NC6H7)6−x]3−x isomers (x = 0–6), which were analyzed by HPLC. The thermal properties of trans-[HNC6H7][Cr(NCS)4(NC6H7)2] were analyzed by thermogravimetric analysis/differential scanning calorimetry–mass spectroscopy (TGA/DSC–MS), and the compound was found to oxidize to CrO2 in three major weight loss steps when heated to 1000 °C in dry air.
Jennifer L. Young, Jerry D. Harris, Joshua A. Benjamin, Jannah E. Fitch, Daniel F. Nogales, Joanna R. Walker, Brian J. Frost, Aaron Thurber, and Alex Punnoose. "Synthesis and Characterization of Chromium-Isothiocyanate-4-Methylpyridine Complexes" Inorganica Chimica Acta 377.1 (2011): 14-19.
Available at: http://works.bepress.com/alex_punnoose/31