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Periodic trends in charge distribution for transition-metal complexes containing catecholate and semiquinone ligands. Synthetic, physical, and stereodynamic properties of the tris(3,5-di-tert-butylquinone) complexes of ruthenium and osmium

Journal Article · · Journal of the American Chemical Society; (USA)
DOI:https://doi.org/10.1021/ja00159a031· OSTI ID:7123371

Tris(3,5-di-tert-butylbenzoquinone) complexes of Ru and Os have been synthesized in the interest of investigating periodic trends in charge distribution for tris(quinone) complexes of second- and third-row transition metals. Infrared spectra of the two complexes are similar but differ from spectra obtained on related semiquinone (Fe(DBSQ){sub 3}) and catecholate (Re(DBCat){sub 3}) complexes. Both complexes undergo two oxidation and two reduction reactions at similar potentials. Crystallographic characterization on the cis and trans isomers of Ru(DBQ){sub 3} and on trans-Os(DBQ){sub 3} at {minus}60{degree}C shows short M-O bond lengths, typical of complexes containing high oxidation state forms of Ru and Os. Ligand C-O bond lengths are found to be intermediate between semiquinone and catecholate values, with lengths that are more semiquinone-like for Ru(DBQ){sub 3} and more catecholate-like for Os(DBQ){sub 3}. This subtle difference in charge distribution between the second- and third-row metals appears to contribute to marked differences in the stereodynamic properties of the two complexes. Both are diamagnetic and show sharp NMR spectra at room temperature. Eight tert-butyl and eight ring proton resonances are observed for Ru(DBQ){sub 3} at room temperature, indicating the presence of stereochemically rigid cis and trans isomers. Two tert-butyl and two ring proton resonances are observed for Os(DBQ){sub 3} at room temperature. At {minus}85{degree}C eight tert-butyl and eight ring proton resonances appear as molecular rearrangement rates decrease on the NMR time scale. Analysis of the temperature dependence of the spectrum of Os(DBQ){sub 3} has indicated racemization by a trigonal twist mechanism at lower temperatures, with structural isomerization and racemization by a rhombic twist mechanism at higher temperatures.

OSTI ID:
7123371
Journal Information:
Journal of the American Chemical Society; (USA), Journal Name: Journal of the American Chemical Society; (USA) Vol. 112:3; ISSN 0002-7863; ISSN JACSA
Country of Publication:
United States
Language:
English