Correction to: Neutral and Cationic Hydridoruthenium Tetrakiscarbene Complexes (Eur. J. Inorg. Chem. (2010), 2010, 6, (918–925), 10.1002/ejic.200900708)

Wolf R., Plois M., Hepp A.

Abstract

Incorrect 1H NMR data were reported for [RuCl2(IMe)4] (1) in the original manuscript. The correct values are as follows: 1H NMR (400 MHz, C6D6, 300 K): δ = 1.80 (s, 24 H, CCH3), 3.72 (s, 24 H, NCH3). We thank Prof. Deryn E. Fogg (University of Ottawa, Canada) for making us aware of this mistake. We further wish to comment on the NMR assignment reported for [RuH(IMe)4][BEt4] (3BEt4). As described in the original manuscript, this compound was isolated as a mixture with two minor products, which we tentatively identified as the putative THF adduct [RuH(IMe)4(thf)][BEt4] (3thf) and an unknown hydroborane species. We have now come to different conclusions regarding the nature of these minor products. A reassessment of the original data and reports by Whittlesey and co-workers, suggest that the minor components likely are the dihydride [RuH2(IMe)4] (2),, and the dihydrogen complex [Ru(H)(η2-H2)(IMe)4][BEt4] (4BEt4).[3]The assignment of the 1H NMR data should be corrected accordingly, the corrected assignment is given below. 1H NMR integration indicates that 2/3BEt4/4BEt4 are present in a 4:89:7 ratio at 220 K. Broadening of the hydride signals at δ = ‒40.0 and ‒9.00 ppm was observed at temperatures >220 K. This might be caused by intermolecular exchange between 3BEt4 and 4BEt4. 1H NMR Data for [RuH(IMe)4][BEt4] (3BEt4) and Minor Products: 1H NMR (400 MHz, [D8]THF, 300 K): δ = ‒39.9 (br., νFWHM = 400 Hz, 0.86 H, HRu of 3BEt4), ‒8.15 (s, νFWHM = 6.0 Hz, 0.06 H, H2Ru of 2), ‒4.04 (s, νFWHM = 11.0 Hz, 0.26 H, Ru–η2-H2 of 4BEt4), ‒0.17 (m, 8 H, JH-11B = 4.0 Hz, JH-10B = 1.3 Hz, JH-H = 7.8 Hz, BCH2CH3 of [BEt4]‒), 0.60 (m, 12 H, JH-11B = 2.9 Hz, JH-10B = 1.0 Hz, JH-H = 7.8 Hz, BCH2CH3 of [BEt4]‒), 1.96 (s, 0.7 H, CCH3 of 2; this signal partiallyoverlaps with the signal at δ = 2.04 ppm), 2.04 (s, 26 H, overlapping CCH3 signals of 3BEt4 and 4BEt3), 3.13 (s, 26 H, overlapping NCH3 signals of 3BEt4 and 4BEt3), 3.33 (s, 0.7 H, NCH3 of 2). 1H NMR (400 MHz, [D8]THF, 220 K): δ = ‒40.0 (br. s, νFWHM = 40 Hz, 0.86 H, HRu of 3BEt4), ‒8.99 (s, νFWHM = 9 Hz, 0.14 H, RuH of 4BEt3), ‒8.33 (s, νFWHM = 8 Hz, 0.05 H, H2Ru of 2), ‒4.20 (s, νFWHM = 31.1 Hz, 0.28 H, Ru–η2-H2 of 4BEt4), ‒0.23 (br., νFWHM = 21 Hz, 8 H, BCH2CH3), 0.56 (br., νFWHM = 18 Hz, 12 H, BCH2CH3), 1.96 (s, 0.6 H, CCH3 of 2), 2.04 (s, 26 H; overlapping CCH3 signals of 3BEt4 and 4BEt3), 3.03 (s, 2 H, NCH3 of 4BEt3), 3.13 (s, 24 H, NCH3 of 3BEt3), 3.30 (s, 0.6 H, NCH3 of 2).