Compound 3a

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Compound data: CIF

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

[(bpy)₂Pd₂(NO₃)₂](NO₃)₂ (2a·2NO₃) (19.4 mg, 0.025 mmol) was added to a suspension of CS₂ (7.6 mg, 0.1 mmol) in H₂O (3 mL) in a 10 mL reaction tube assembly, and the mixture was stirred for 2 h at room temperature to give a yellow emulsion. Next, a 10-fold excess of KPF₆ was added to the solution of 3a·2NO₃ in water/acetone and the mixture was stirred for 2 h at 40 °C, and then cooled to room temperature to obtain a light yellow precipitate (3a·2PF₆), which was collected by filtration. The yellow hexagonal block crystals were grown by vapor diffusion of diethyl ether into a solution of 3a·2PF₆ in acetonitrile at room temperature (yield, 94%). ¹H NMR (400 MHz, CD₃CN, 298 K, ppm) δ = 8.92 (d, J = 8.1 Hz, 6H), 8.37 (d, J = 6.8 Hz, 6H), 8.27 (d, J = 8.4 Hz, 6H), 7.76 (d, J = 6.8 Hz, 6H). ¹³C NMR (100 MHz, CD₃CN, 298 K, ppm): δ 155.47, 151.04, 140.76, 127.61, 123.79. ESI-MS (CH₃CN) m/z: [3a]²⁺, calcd for C₃₀H₂₄N₆Pd₃S₂²⁺, 425.97; found, 425.86. Found: C, 30.99; H, 2.24; N, 7.28. Calc. for C₃₀H₂₄N₆Pd₃S₂P₂F₁₂•H₂O (%): C, 31.07; H, 2.26; N, 7.25.