Compound 5

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InChIKey XUCNZFGLAQZSQP-UHFFFAOYSA-N

Compound data: CIF

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

A J. Young valve NMR tube was charged with 3a (39 mg, 0.028 mmol) and connected to a vacuum line. The sample was kept under vacuum (1.1×10^-5 Torr) at 80 °C for 18 h, and its color changed gradually from orange to black. Toluene-d₈ was added and the subsequent ¹H NMR analysis suggested almost quantitative formation of 5. Single crystals of 5·C₇H₈ suitable for X-ray analysis were grown in a concentrated toluene solution at –35 °C (20 mg, 0.015 mmol, 54%). ¹H NMR (300 MHz, C₆D₆, rt): 6.32 (brs, 3H, Y-H-Y), 2.64 (s, 24H, C₅Me₄SiMe₃), 2.24 (s, 24H, C₅Me₄SiMe₃), 2.09 (s, 15H, C₅Me₅), 0.51 (s, 36H, C₅Me₄SiMe₃), –8.86 (qt, J_HY = 8.7 Hz, 4H, Mo-H-Y). ¹H NMR (300 MHz, C₆D₆, 50 °C): δ 6.04 (brs, 5H, Y-H-Y), 2.61 (s, 24H, C₅Me₄SiMe₃), 2.23 (s, 24H, C₅Me₄SiMe₃), 2.12 (s, 15H, C₅Me₅), 0.47 (s, 36H, C₅Me₄SiMe₃), –8.84 (qt, J_HY = 8.9 Hz, 4H, Mo-H-Y). ¹H NMR (300 MHz, toluene-d₈, –60 °C): δ 6.39 (t, J_HY = 30.0 Hz, 4H, Y-H-Y), 4.04 (brs, 1H, Y-H-Y), 2.69 (s, 24H, C₅Me₄SiMe₃), 2.25 (s, 24H, C₅Me₄SiMe₃), 2.10 (s, 15H, C₅Me₅), 0.57 (s, 36H, C₅Me₄SiMe₃), –8.91 (brs, 4H, Mo-H-Y). ¹³C NMR (100 MHz, C₆D₆, rt): δ 129.6 (s, C₅Me₄SiMe₃), 123.8 (s, C₅Me₄SiMe₃), 115.5 (s, ipso-C₅Me₄SiMe₃), 96.8 (s, C₅Me₅), 17.2 (s, C₅Me₄SiMe₃), 16.7 (s, C₅Me₅), 12.7 (s, C₅Me₄SiMe₃), 2.5 (s, C₅Me₄SiMe₃). IR (Nujol mull): ν 2953 (s), 2922 (s), 2853 (s), 1458 (m), 1377 (w), 1246 (w), 1022 (w), 835 (w) cm^–1. Anal. calcd for C₅₈H₁₀₈MoSi₄Y₄·C₇H₈: C, 53.43; H, 7.95. Found: C, 53.41; H, 7.92.