Compound Ru5

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Compound data: NMR

Compound data: CIF

Synthetic procedure: See article for the definitive version of this procedure and for full experimental details.

All liquid reagents and solvents were dried over 4 Å molecular sieves and degassed with 3 freeze-pump-thaw cycles prior to use. An oven dried crimp-cap microwave vial equipped with a stirring bar was transferred to a glove box, then Ru3 (65.7 mg, 0.1 mmol, 1 equiv), K₂CO₃ (41.5 mg, 0.3 mmol, 3 equiv), KOAc (4.9 mg, 0.05 mmol, 0.5 equiv), benzene (1.9 mL) and NMP (0.1 mL) were added. The vial was placed in a heating block at 80 °C and stirred for 18 h. Upon completion, the reaction crude was diluted with benzene and filtered through a short plug of Celite^®. The solution was concentrated under reduced pressure and the resulting residue was redissolved in a minimum amount of benzene. Ru5 was precipitated after the addition pentane as a deep red solid (48.7 mg, 72%). Ru5 must be kept in a glove box as it quickly decomposes if exposed to air. Suitable crystals of Ru5 for X-ray crystallography were grown by slow crystallization from benzene/Et₂O/pentane (see crystallographic section). ¹H-NMR (500 MHz, C₆D₆) δ 0.59 (s, 6 H), 1.84 (s, 6 H), 2.01 (s, 6H), 2.06 (s, 6 H), 2.10 (s, 6 H), 8.56 (s, 2 H), 9.30 (s, 2 H) ppm; ¹³C-NMR (125 MHz, C₆D₆) δ 10.9 (dd, J = 7.1 Hz), 11.8-11.9 (m), 16.7, 19.4, 114.1 (dd, J = 20.4, 3.4 Hz), 122.4 (dd, J = 26.6, 4.8 Hz), 123.4 (d, J = 22.3 Hz), 127.4, 133.3 (dd, J = 21.6, 4.9 Hz), 142.0, 149.5 (d, J = 41.3 Hz), 151.2, 156.6 (d, J = 246.1 Hz), 165.1 (d, J = 7.6 Hz), 167.6 (d, J = 222.8 Hz), 170.3 (d, J = 54.4 Hz) ppm (Me group of the MeCN ligand is missing due to an upfield shift); ¹⁹F-NMR (376 MHz, C₆D₆) δ −124.2 (d, J = 23.3 Hz), −123.6 (d, J = 23.3 Hz) ppm.