Compound Fe63

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Compound data: LRESI-MS

Compound data: ESI-MS

Compound data: 1H NMR

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

[Fe₆1₆](PF₆)₁₂ (20 mg, 2.5 μmol) was placed under an atmosphere of argon in a flask equipped with a stirrer bar. In a separate flask, Hoveyda-Grubbs 2^nd generation catalyst (H₂IMes)(Cl)₂RuCH(o-OiPrC₆H₄) (1.6 mg, 2.5 μmol, 17 mol % per ligand 1) was dissolved in degassed anhydrous nitromethane (2.5 mL) and degassed anhydrous 1,2-dichloroethane (2.5 mL) under argon. The solution of the Hoveyda-Grubbs 2^nd generation catalyst was transferred to the starting material [Fe₆1₆](PF₆)₁₂ and the reaction was heated to 60 °C for 24 hours with stirring. After cooling to room temperature, the catalyst was quenched with excess ethyl vinyl ether (1.6 mL, 17 mmol) and stirred for 30 minutes. The solvent was removed under vacuum, and the resulting solid suspended in chloroform for 10 minutes with sonication. The suspension was filtered onto celite, washed thoroughly with fresh chloroform, and dissolved in acetonitrile. Saturated aqueous KPF₆ was added to the solution until a precipitate formed which was again filtered onto celite, washed with water, methanol, and dissolved in acetonitrile. The solvent was removed to afford a mixture of [Fe₆2](PF₆)₁₂ and [Fe₆3](PF₆)₁₂ as a red-purple solid (18 mg, 2.3 μmol, 92 %). Due to the broad and poorly resolved nature of the NMR signals, most peaks could not be assigned. ¹H NMR (600 MHz, CD₃CN) [assignments refer to lettering shown in Supplementary Scheme 1, page 4] δ 9.02 – 8.20 (m), 7.84 – 6.75 (m), 6.69 – 6.07 (m), 5.80 – 5.54 (m, H^r), 4.24 –3.86 (m, H^p), 3.08 – 1.99 (m, H^d, H^e, H^q). ¹³C NMR (151 MHz, CD₃CN) δ 162.10, 157.60, 157.16, 156.97, 156.41, 156.22, 155.23, 152.68, 151.87, 149.67, 149.15, 139.72, 137.73, 129.96, 129.84, 129.53, 128.71 (C^r), 124.84, 123.72, 123.06, 122.53, 117.47, 116.57, 68.78 (C^p), 33.61, 32.41 (C^q), 30.32. LRESI-MS: m/z = 1433.01 [M–5PF₆]⁵⁺ requires 1432.96; 1169.69 [M–6PF₆]⁶⁺ requires 1169.97; 982.00 [M–7PF₆]⁷⁺ requires 982.12; 840.94 [M–8PF₆]⁸⁺ requires 841.24; 731.76 [M–9PF₆]⁹⁺ requires 731.66. HRESI-MS: m/z = 841.2376 [M–8PF₆]⁸⁺ (calcd. for C₃₈₄H₃₁₂N₃₆O₂₄Fe₆P₄F₂₄, 841.2383).