Compound 2

6,6',6''-((2,4,6-trimethylbenzene-1,3,5-triyl)tris(methylene))tris(2-(adamantan-1-yl)-4-methylphenolate)uranium(V) oxide

From: The role of uranium–arene bonding in H2O reduction catalysis

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Compound data: CIF

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

A solution of [((Ad,MeArO)3mes)U] (45.0 mg, 4.02 · 10–5 mol) in benzene (20 mL) was stirred for 30 min. under 1 atm. of N2O. The solvent was removed in vacuo to obtain the title compound as a red-brown powder. Crystals suitable for XRD analysis were obtained from a concentrated pentane solution with 2 drops of THF per 5 ml pentane at –35 °C. Yield: 91% (44.0 mg, 3.65 · 10–5 mol) 1H NMR (400 MHz, benzene-d6, RT) δH = 0.95 (br. s., 18H), 1.36 (br. s., 4H), 2.62 (br. s., 9 H), 3.31 (br.s., 9 H), 3.49 (br. s., 4H), 3.78 (d, J = 11.0 Hz, 9 H), 3.94 (br. s., 9 H), 5.70 (br.s., 6 H), 6.20 (s, 3 H), 6.31 (s, 6 H), 6.49 (d, J = 11.0 Hz, 9 H) ppm. Elemental Analysis for C63H75O4U: Calculated: C, 66.71, H, 6.66; Found: C, 67.15; H, 6.60. IR: ν [cm-1] = 2900 (vs), 2846 (s), 1444 (s), 1230 (s), 1182 (w), 1159 (m), 839 (s), 802 (s), 677 (m), 522 (m), 416 (m).