Compound 7
[Ru(III)(bda)(pic)2NH3][PF6]
From: Ruthenium-catalysed oxidative conversion of ammonia into dinitrogen
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Compound data: Crystallographic data
Synthetic procedure: See article for the definitive version of this procedure and for full experimental details.
To a 50 mL Schlenk flask under Ar were placed 1b′ (69.1 mg, 0.102 mmol), NH3 solution (15 M in H2O; 13 μL, 0.20 mmol) and acetone (5 mL), and the mixture was stirred at room temperature for 10 min. After the reaction, onto the resulting acetone solution was layered Et2O (ca. 10 mL). The precipitate was collected by filtration and the solid was washed with Et2O and dried under stream of Ar to afford 7·C3H6O·0.5C4H10O as a purple solid (36.1 mg, 0.0459 mmol, 45% yield). Anal. Calcd. for C29H34F6N5O5.5PRu (7·C3H6O·0.5C4H10O): C, 44.28; H, 4.36; N, 8.90. Found: C, 44.38; H, 4.44; N, 9.16. Crystals of 7·H2O·CH4O suitable for X-ray analysis were obtained from recrystallization from wet MeOH-Et2O.
