Preparation of a dicationic, p-cymene ruthenium(II) dimer, [(p-cymene)Ru(µ-Cl)(P{OCH2}3CEt)]2 2+: structure, characterization and reactivity

Autor: Bazemore, Joseph G., Padgett, Clifford W., Quillian, Brandon
Rok vydání: 2021
DOI: 10.6084/m9.figshare.13705219.v1
Popis: Reaction of (p-cymene)RuCl2(P{OCH2}3CEt) (P{OCH2}3CEt = 4-ethyl-2,6,7-trioxa-1-phosphabicyclo[2.2.2]octane) with silver tetrakis[(3,5-trifluoromethyl)phenyl]borate (Ag[BArF′]) in the presence of acetonitrile produces the monomeric, cationic, acetonitrile ruthenium(II) compound, [(p-cymene)RuCl(P{OCH2}3CEt)(NCMe)][BArF′] (1), in near quantitative yields (97%). Chloroform solutions of 1 cause precipitation of the binuclear, dicationic ruthenium(II) dimer complex, [(p-cymene)Ru(µ-Cl(P{OCH2}3CEt)]2[BArF′]2 (2), with bridging chloride ligands (73%). Complex 2 can be readily converted back to 1 by treatment with acetonitrile. Complexes 1 and 2 were characterized by 1H, 13C{1H}, 31P{1H}, 19F{1H} nuclear magnetic resonance spectroscopy and infrared spectroscopy. Complex 2 was also characterized by single crystal X-ray crystallography, which revealed a rhomboid Ru2Cl2 core. The two ruthenium ions in 2 are displaced at 3.668 Å, which precludes Ru–Ru bonding. To our knowledge, this is the first cymene ruthenium(II) dimeric complex with bridging halide ligands supported by a monodentate phosphite ligand.
Databáze: OpenAIRE