at room temperature under argon using standard Schlenk, high vacuum,
and glovebox techniques using dry and degassed solvents. C6D6, C6D5CD3, and THF-d8 were vacuum transferred from potassium. NMR
spectra were recorded at 298 K (unless otherwise stated) on Bruker
Avance 400 and 500 MHz NMR spectrometers and referenced as follows:
C6D6 (1H, δ 7.16; 13C, δ 128.0), C6D5CD3 (1H, δ 2.09), THF-d8 (1H, δ 3.58; 13C, δ 25.3). 31P{1H} spectra were referenced externally to 85% H3PO4 and 119Sn to SnMe4. IR
spectra were recorded on a Nicolet Nexus spectrometer and UV–vis
spectra on a PerkinElmer Lambda 35 spectrometer. Elemental analyses
were performed by Elemental Microanalysis Ltd., Okehampton, Devon,
U.K. [Ru(PPh3)3HCl]·toluene,43 (link) [Ru(PPh3)(C6H4PPh2)2H][Li(THF)2] (
prepared according to literature methods. Prior to use, [Ru(PPh3)3HCl]·toluene was dried under high vacuum
and ground to a fine powder affording a material with ca. 1 molecule
of toluene per Ru (based on 1H NMR analysis). IMe4 was purified by sublimation. LiCH2TMS was used as a colorless
solid obtained upon cooling a commercial 1.0 M solution in pentane
at −32 °C, separating the resulting colorless crystals
by decantation in a glovebox and drying under vacuum. AlMe2Cl (1.0 M solution in hexane, Merck) and SnMe3Cl (Merck)
were used as received.