Experiments forming 1 were conducted in CD3CN solution in J-Young NMR tubes. In a typical experiment, [Pd(triphos)(PPh3)](BF4)2 (6.0 mg, 5.6 µmol) was dissolved in 0.55 mL of CD3CN, transferred to the NMR tube, and a stoichiometric amount of the base was added. The solution turned from a beige color to bright yellow. H2 was added, and the NMR spectra were collected for several days, over which time no further changes were observed. Crystals of 1 were then grown from a CD3CN solution of 1 and t BuTMG that had been layered with diethyl ether. In the structure of 1, two acetonitrile solvates were removed from the refinement using PLATON/SQUEEZE as described above. Experiments forming 2 were conducted in a Vigor glovebox under an N2 atmosphere. A solution of [Pd(PNP)Cl]Cl (127 mg, 0.205 mmol) was dissolved in THF, and a solution of KOtBu (17.2 mg, 1.53 mmol) in THF was added. The reaction mixture was stirred overnight, and the reaction was filtered. The rusty red-colored solid was washed with THF, then extracted into MeCN. The rustcolored precipitate dissolved to give a bright orange color, and this solution was filtered. The filtrate was dried, giving 45.9 mg of yellow solid (47.5%). After crystallization from acetonitrile/diethyl ether, 35.4 mg of yellow crystals were obtained (37% yield). In the structure of 2, the phenyl groups comprising C7-12 and C13-18 were disordered and refined using EADP and SADI restraints.