Compound 2-K
4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane-potassium(I) 6,6',6''-((2,4,6-trimethylbenzene-1,3,5-triyl)tris(methylene))tris(2-(adamantan-1-yl)-4-methylphenolate)oxouranate(IV)
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 precooled solution of 2 (25.0 mg, 2.07 · 10–5 mol) and 2.2.2-cryptand (8.7 mg, 2.31 · 10–5 mol) in THF (10 mL, –35°C) was pipetted into a well stirred, precooled vial charged with KC8 (3.12 mg, 2.31 · 10–5 mol). The reaction was stirred for 1.5 h to reach room temperature. The orange solution was filtered over a glass filter pad, the solvent was removed in vacuo, and the obtained orange solid was stirred in pentane (5 mL) for 1 h. The orange brown powder was filtered off over a por. 4 frit, washed with pentane (3 x 1 mL) and dried in vacuo to yield the title compound. Single crystals suitable for XRD analysis were obtained from diffusion of pentane in a THF / DME (50:50) solution at –35 °C. Yield: 62% (20.0 mg, 1.29 10–5 mol) 1H NMR (400 MHz, benzene-d6, RT) δH = –18.82 (br. s., 18H), –9.90 (s., 3 H), –6.41 (s., 9 H), 2.58 (br. s., 9 H), 2.68 (br.s., 12 H, 2.2.2crypt), 3.52 (br.s., 4 H, 2.2.2crypt), 6.36 (br. s., 9 H), 16.16 (s, 9 H), 19.84 (s, 9 H), 21.25 (s, 6 H), 42.18 (br. s., 3 H) ppm. Elemental Analysis for C81H111KN2O10U: Calculated: C, 62.77, H, 7.22, N, 1.81; Found: C, 61.83, H, 7.39, N, 1.66. Samples of 2–K were repeatedly low on carbon. IR: ν [cm–1] = 2968 (s), 2893 (vs), 2844 (vs), 1475 (m), 1445 (s), 1354 (vs), 1283 (vs), 1257 (vs), 1184 (w), 1162 (w), 1135 (s), 1104 (vs), 1080 (s), 1026 (m), 980 (w), 949 (s), 933 (m), 914 (w), 858 (m), 832 (s), 805 (s), 768 (vs), 577 (w), 508 (s), 468 (w), 409 (w).
