Compound 2

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Compound data: CIF

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

Synthesis of [(Anth•C^NHNS)Fe(CO)₂(I)(PPh₃)] (2): complex 1 (146 mg, 240 µmol) and PPh₃ (63 mg, 240 µmol) were mixed in 4 mL of DCM, and the reaction mixture was either stored at -30 ^oC overnight or simply allowed to warm to ambient temperature (note that the same result was obtained by either method, or by adding PPh₃ at ambient temperature). The solvent was removed in vacuo at ambient temperature, and the resulting yellow solid was re-dissolved in THF. Batches single crystals were obtained via pentane vapor diffusion at -30 ºC for X-ray diffraction. Yield: 199 mg (90%). The complete conversion of 1 to 2 was observed by the ¹H and ³¹P NMR spectra. ¹H NMR (d₈-THF, 400 MHz): δ 2.81 (s, 3H), 7.00 (m, 1H), 7.06 (s, 2H), 7.24 (m, 11H), 7.30 (m, 8H), 7.45 (d, 1H), 7.51 (m, 2H), 7.61 (s, 2H), 7.64 (s, 1H), 7.94 (d, 1H), 8.37 (s, 1H), 8.60 (s, 1H) ppm. ³¹P NMR (d₈-THF): δ 39.39 ppm. IR (solid state): ν_C≡O 2031, 1975; ν_C=O 1663, ν_C=N 1613 cm^–1. Anal. calcd. for C₄₇H₃₄FeIN₂O₃PS: C 61.32, H 3.72, N 3.04; found: C 61.31, H 3.93, N 3.02.