Compound 2a

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InChIKey PEZNOFNPBPOBRU-UHFFFAOYSA-N

Compound data: CIF

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

[Cp'Y(μ-H)₂]₄(THF) (1) (31 mg, 0.025 mmol), Cp*Mo(PMe₃)H₅ (8 mg, 0.026 mmol), and hexane (0.3 mL) were mixed at room temperature to give immediately an orange solution. After being stirred at room temperature for a few minutes, the mixture was cooled to –33 °C to afford 2a as orange microcrystals (35 mg, 0.024 mmol, 96%). Single crystals of 2a suitable for X-ray analysis were grown in a concentrated toluene solution at –35 °C. ¹H NMR (300 MHz, toluene-d₈, –70 °C): δ 5.75 (t, J_HY = 33.3 Hz, 2H, Y-H-Y), 5.70 (t, J_HY = 34.2 Hz, 2H, Y-H-Y), 4.44 (t, J_HY = 25.5 Hz, 2H, Y-H-Y), 4.23 (brs, 1H, Y-μ₄-H-Y), 2.67 (s, 6H, C₅Me₄SiMe₃), 2.64 (s, 6H, C₅Me₄SiMe₃), 2.59 (s, 6H, C₅Me₄SiMe₃), 2.46 (s, 12H, C₅Me₄SiMe₃), 2.44 (s, 6H, C₅Me₄SiMe₃), 2.38 (s, 6H, C₅Me₄SiMe₃), 2.36 (s, 6H, C₅Me₄SiMe₃), 1.81 (s, 15H, C₅Me₅), 1.07 (d, J_HP = 7.5 Hz, 9H, PMe₃), 0.66 (s, 18H, C₅Me₄SiMe₃), 0.59 (s, 18H, C₅Me₄SiMe₃), –2.27 (d, J_HP = 37.2 Hz, 1H, Mo-μ₃-H-Y), –7.07 (brs, 2H, Mo-H-Y), –7.82 (brs, 1H, Mo-μ₃-H-Y). ¹H NMR (300 MHz, toluene-d₈, 90 °C): δ 5.73 (t, J_HY = 35.4 Hz, 2H, Y-H-Y), 4.92 (brs, 4H, Y-H-Y), 2.59 (s, 6H, C₅Me₄SiMe₃), 2.55 (s, 6H, C₅Me₄SiMe₃), 2.53 (s, 6H, C₅Me₄SiMe₃), 2.45 (s, 6H, C₅Me₄SiMe₃), 2.42 (s, 6H, C₅Me₄SiMe₃), 2.41 (s, 6H, C₅Me₄SiMe₃), 2.35 (s, 6H, C₅Me₄SiMe₃), 2.34 (s, 6H, C₅Me₄SiMe₃), 2.00 (s, 15H, C₅Me₅), 1.30 (d, J_HP = 7.2 Hz, 9H, PMe₃), 0.56 (s, 9H, C₅Me₄SiMe₃), 0.54 (s, 9H, C₅Me₄SiMe₃), 0.49 (s, 18H, C₅Me₄SiMe₃), –5.94 (brs, 3H, Mo-H-Y). ¹³C NMR (100 MHz, C₆D₆, rt): δ 126.1, 128.65, 128.63 128.4, 128.15, 128.10, 127.90, 127.89, 127.5, 125.2, 124.90, 124.87, 124.7 (s, C₅Me₄SiMe₃), 116.12, 116.11, 114.02, 114.00 (s, ipso-C₅Me₄SiMe₃), 97.4 (s, C₅Me₅), 25.8 (s, C₅Me₄SiMe₃), 25.7 (d, JCP = 25.6 Hz, PMe3), 18.1 (s, C5Me4SiMe3), 17.4 (s, C5Me4SiMe3), 16.22 (s, C5Me4SiMe3), 16.21 (s, C5Me4SiMe3), 14.55 (s, C5Me4SiMe3), 14.47 (s, C5Me5), 14.3 (s, C5Me4SiMe3), 14.1 (s, C5Me4SiMe3), 13.3 (s, C5Me4SiMe3), 12.9 (s, C5Me4SiMe3), 4.0 (s, C5Me4SiMe3), 3.41 (s, C5Me4SiMe3), 3.38 (s, C5Me4SiMe3). ³¹P NMR (162 MHz, toluene-d8, rt): δ 1.1 (Mo-PMe3). IR (Nujol mull): v 2953 (s), 2922 (s), 2852 (s), 1458 (m), 1377 (w), 1244 (w), 1020 (w), 847 (w), 833 (w) cm–1. Anal. calcd for C₆₁H₁₁₉MoPSi₄Y₄: C, 50.57; H, 8.22. Found: C, 50.90; H, 8.12