Compound 2b

[{(C5Me4SiMe3Y)4(μ-H)7}(μ-H)4WC5Me5(PMe3)]

From: Molecular heterometallic hydride clusters composed of rare-earth and d-transition metals

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InChIKey UVHNIGTWARSLKN-UHFFFAOYSA-N

Compound data: CIF 1

Compound data: CIF 2

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

[Cp'Y(μ-H)2]4(THF) (1) (66 mg, 0.053 mmol), Cp*W(PMe3)H5 (22 mg, 0.055 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 –35 °C to afford 2b as orange microcrystals (80 mg, 0.052 mmol, 98%). Single crystals of 2b suitable for neutron and X-ray analyses were grown in a concentrated hexane solution at room temperature and toluene at –35 °C, respectively. 1H NMR (400 MHz, toluene-d8, –40 °C): δ 5.85 (t, JHY = 34.4 Hz, 2H, Y-H-Y), 5.81 (t, JHY = 34.4 Hz, 2H, Y-H-Y), 4.48 (t, JHY = 20.4 Hz, 3H, Y-H-Y), 2.63 (s, 6H, C5Me4SiMe3), 2.59 (s, 6H, C5Me4SiMe3), 2.54 (s, 6H, C5Me4SiMe3), 2.43 (s, 6H, C5Me4SiMe3), 2.42 (s, 6H, C5Me4SiMe3), 2.41 (s, 6H, C5Me4SiMe3), 2.35 (s, 6H, C5Me4SiMe3), 2.33 (s, 6H, C5Me4SiMe3), 2.06 (s, 15H, C5Me5), 1.28 (d, JHP = 8.4 Hz, 9H, PMe3), 0.61 (s, 9H, C5Me4SiMe3), 0.60 (s, 9H, C5Me4SiMe3), 0.54 (s, 18H, C5Me4SiMe3), *0.5 (1H, W-H-Y obscured by SiMe3), –7.20 (brs, 2H, W-H-Y), –7.37 (brs, 1H, W-H-Y). *by HH COSY. 13C NMR (100 MHz, C6D6, rt): δ 129.1, 128.6, 128.1, 127.4, 125.2, 124.9, 124.8, 124.7 (s, C5Me4SiMe3), 116.0, 115.2, 113.8 (s, ipso-C5Me4SiMe3), 94.1 (s, C5Me5), 27.2 (d, JCP = 28.9 Hz, PMe3), 18.0, 17.4, 16.24, 16.21, 14.6 (s, C5Me4SiMe3), 14.5 (C5Me5), 14.3, 14.1, 13.3, 12.9 (s, C5Me4SiMe3), 4.0 (s, C5Me4SiMe3), 3.4 (s, C5Me4SiMe3). 31P NMR (162 MHz, toluene-d8, rt): δ –37.4 (s, JPW = 204.8 Hz, W-PMe3). IR (Nujol mull): ν 2953 (s), 2924 (s), 2853 (s), 1458 (m), 1377 (w), 1244 (m), 845 (w), 833 (w) cm–1. Anal. calcd for C61H119WPSi4Y4: C, 47.68; H, 7.75. Found: C, 48.24; H, 7.44.