Compound 1
[C5Me4SiMe3Y(μ-H)2]4(THF)
From: Molecular heterometallic hydride clusters composed of rare-earth and d-transition metals
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InChIKey QIHORIXEFOBKCO-UHFFFAOYSA-N
Synthetic procedure: See article for the definitive version of this procedure and for full experimental details.
A toluene solution of [(C5Me4SiMe3)Y(CH2SiMe3)2(thf)] (0.793 g, 1.5 mmol) in a 300-mL Schlenk flask equipped with a J. Young valve was frozen in liquid nitrogen, pumped, and backfilled with H2. The mixture was allowed to warm to room temperature and stirred for 2 h. For complete conversion, a second charge of H2 was carried out in an identical way and the solution mixture was then further stirred for 2 h. After removal of the solvent under vacuum, the resulting pale yellow residue was extracted with hexane and filtered in the glove box. Slow evaporation of the solvent under reduced pressure precipitated 1 as a pale yellow crystalline powder (0.345 g, 76% yield). Single crystals suitable for X-ray analysis were grown by recrystallization from hexane. 1H NMR (270 MHz, C6D6, rt): δ 0.53 (s, 36H, C5Me4SiMe3), 1.40 (br, 4H, THF), 2.25 (s, 24H, C5Me4), 2.33 (s, 24H, C5Me4), 3.61 (br s, 4H, THF), 4.32 (quintet, JY-H= 15.3 Hz, 8H, YH). 13C NMR (75 MHz, C6D6, rt):δ 3.13, 12.7, 15.4, 25.2, 70.7, 114.8, 124.5, 127.1. IR (nujol): ν 1405, 1340, 1322, 1260, 1244, 1130, 848, 838, 756, 684, 630 cm-1. Anal. Calcd for C52H100OSi4Y4: C, 51.65; H, 8.33. Found: C, 51.82; H, 8.14.
