Compound 2

[(4,5-bis(2,6-diisopropylanilido)-2,7-di-tert-butyl-9,9-dimethylxanthene)aluminyl]bis(triphenylphosphine)digold iodide

From: A nucleophilic gold complex

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Compound data: 1H NMR

Compound data: Crystallographic data

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

To a solution of 1 (0.200 g, 0.136 mmol) in toluene (10 mL) was added a solution of Ph3PAuI (0.318 g, 0.543 mmol) in toluene (20 mL) at room temperature over 5 minutes. The reaction mixture was stirred at room temperature for further 16 hours, whereupon volatiles were removed in vacuo. The dark red residue was extracted with diethyl ether (10 mL), the extract filtered and the filtrate slowly cooled to –30 °C overnight to give 2 as yellow crystals (0.305 g, 64%). 1H NMR (400 MHz, C6D6, 298 K): δ = 0.65 (s, 3H, C(CH3)2), 0.71 (d, 3JHH = 6.9 Hz, 6H, CH(CH3)2), 1.08 (d, 3JHH = 6.7 Hz, 6H, CH(CH3)2), 1.10 (d, 3JHH = 7.1 Hz, 6H, CH(CH3)2), 1.28 (s, 18H, C(CH3)3), 1.36 (d, 3JHH = 6.8 Hz, 6H, CH(CH3)2), 1.46 (s, 3H, C(CH3)2), 3.33 (sept., 3JHH = 6.7 Hz, 2H, CH(CH3)2), 4.34 (sept., 3JHH = 6.7 Hz, 2H, CH(CH3)2), 6.26 (s, 2H, XA-o-CH), 6.62 (d, 2H, XA-p-CH), 6.87-7.80 (m, 36H ArH); 13C{1H} NMR (126 MHz, C6D6): δ = 23.3 (C(CH3)2), 24.3, 26.0, 26.2, 27.5 (CH(CH3)2) 29.0, 29.6 (CH(CH3)2), 31.9 (C(CH3)3), 32.0 (C(CH3)2), 35.3 (C(CH3)3), 36.8 (C(CH3)2), 106.9, 110.5, 124.2, 124.9, 126.3 (Ar-C) 128.9 (d, 3JCP = 10.1 Hz, m-PPh3), 129.0 (d, 3JCP = 11.3 Hz, m-PPh3), 130.4 (d, 4JCP = 1.2 Hz, p-PPh3), 130.6 (d, 4JCP = 1.2 Hz, p-PPh3), 132.0 (Ar-C), 132.1 (d, 1JCP = 44.1 Hz, i-PPh3), 132.4 (d, 1JCP = 46.6 Hz, i-PPh3), 134.8 (d, 2JCP = 13.9 Hz, o-PPh3), 134.9 (d, 2JCP = 13.9 Hz, o-PPh3), 140.7, 141.9, 143.6, 148.0, 148.1, 149.3 (Ar-C); 31P{1H} NMR (162 MHz, C6D6): 55.0 (d, 3JPP = 131 Hz), 58.4 (d, 3JPP = 131 Hz); anal. calc. for C83H92AlAu2IN2OP2: C 57.18%, H 5.32%, N 1.61%, found: C 56.96%, H 5.55%, N 1.70%.

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