Compound 1a

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Compound data: CIF

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

The trimetallic cluster [Pd₃(μ³-S^2–)(bpy)₃](NO₃^–)₂ (3a·2NO₃, 25 mg) was combined with concentrated HNO₃ (2.5 ml) at room temperature, and the resulting mixture was stirred for 6 h. Yellow crystals suitable for X-ray single crystal diffraction analysis were obtained in high yield (81%) after standing for 30 min. X-ray crystallography confirmed the formation of mononuclear complex [(bpy)Pd](NO₃)₂ (1a). ¹H NMR (400 MHz, CD₃COCD₃/H₂O, 298 K, ppm) δ = 8.36 (m, 4H), 8.24 (d, J = 6.1 Hz, 2H), 7.78 (m, 2H). ESI-MS (CH₃CN) m/z: [1a-NO₃]⁺, calcd for C₁₀H₈N₃O₃Pd⁺, 323.96; found, 323.0. Found: C, 29.65; H, 2.51; N, 13.86. Calc. for C₃₆H₂₄N₆Pd₃S₂P₂F₁₂·H₂O (%): C, 29.68; H, 2.49; N, 13.85. The gas product NO₂ was confirmed by GC-FT-IR spectrum (ν/cm⁻¹: 2917 (N–O), 1618 (N=O)). The crystals were next collected by filtration and the filtrate was treated with 1M hydrochloric acid (10 mL), leading to a yellow suspension. After the filtration of the solid, 3 mL of an aqueous solution of BaCl₂ (1 mol/L) was added dropwise to afford a white precipitate. The precipitate was collected by filtration, washed with concentrated HNO₃ (5 mL) and water (10 mL) and dried in vacuo at 298K. The FT-IR spectrum confirmed the identity if the precipitate to be BaSO₄ (ν = 1067 and 609 cm^-1).