Compound 3a

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InChIKey SRTBMLLWXRWMOX-UHFFFAOYSA-N

Compound data: CIF

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

Complex 2a (138 mg, 0.0953 mmol) and toluene (4 mL) were placed in a Schlenk flask that contained a stir bar. The solution was irradiated under stirring by use of a UV lamp (365 nm) at room temperature for 2 h. After removal of all the volatiles under vacuum, the resulting orange-red solid was dissolved in toluene (4 mL) and further irradiated for 1h to complete the reaction. After removal of the solvent under vacuum, the brown residual solid was taken up in a minimal amount of toluene and recrystallized under 1 atm hydrogen to give 3a·C₇H₈ (90 mg, 0.061 mmol, 64%) as orange crystals. Single crystals of 3a·C₆H₁₄ suitable for X-ray analysis were grown in a concentrated hexane solution under hydrogen at room temperature. ¹H NMR (400 MHz, C₆D₆, rt): δ 4.73 (qt, J_HY = 13.8 Hz, 6H, Y-H-Y), 2.61 (s, 24H, C₅Me₄SiMe₃), 2.33 (s, 24H, C₅Me₄SiMe₃), 2.01 (s, 15H, C₅Me₅), 0.49 (s, 36H, C₅Me₄SiMe₃), –6.68 (s, 5H, Mo-H-Y). ¹³C NMR (100 MHz, C₆D₆, rt): δ 129.1 (s, C₅Me₄SiMe₃), 123.9 (s, C₅Me₄SiMe₃), 114.7 (s, ipso-C₅Me₄SiMe₃), 95.9 (s, C₅Me₅), 17.3 (s, C₅Me₄SiMe₃), 15.1 (s, C₅Me₄SiMe₃), 13.0 (s, C₅Me₅), 2.6 (s, C₅Me₄SiMe₃). IR (Nujol mull): ν 2953 (s), 2924 (s), 2853 (s), 1458 (m), 1377 (w), 1246 (m), 1020 (w), 847 (m), 835 (m) cm^–1. Anal. calcd for C₅₈H₁₁₀MoSi₄Y₄·C₇H₈: C, 53.36; H, 8.07. Found: C, 53.52; H, 7.88.