Compound 8

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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 (53.0 mg, 0.100 mmol), NH₄PF₆ (163 mg, 1.00 mmol), 2a (490 mg, 0.600 mmol), and MeCN (4 mL). Then, 2,4,6-collidine (0.130 mL, 1.00 mmol) dissolved in MeCN (1 mL) was added dropwise to the mixture. The mixture was stirred at room temperature for 10 min. After addition of saturated aqueous NH₄PF₆ (ca. 5 mL), the resulting precipitate (including some crystals of 8·2H₂O suitable for X-ray analysis) was filtered and washed with water, CH₂Cl₂ and MeOH. The residue was extracted with MeCN and dried in vacuo to afford 8 as an orange solid (34.3 mg, 0.0197 mmol, 39 % yield). Anal. calcd. for C₄₈H₄₄Cl₁₂N₉O₁₀Ru₂Sb₂ (8·2H₂O): C, 32.43; H, 2.49; N, 7.09. Found: C, 32.07; H, 2.56; N, 7.44. ESI-TOF-MS (MeCN): 1074 (m/z).