Compound 5

(tri-tert-butylphosphine)aura-carboxylato(4,5-bis(2,6-diisopropylanilido)-2,7-di-tert-butyl-9,9-dimethylxanthene)aluminium

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.

A solution of 3 (0.100 g, 0.091 mmol) in toluene (10 mL) was prepared in 50 mL J. Young sample flask. The solution was frozen, the atmosphere evacuated (5.0 x 10–2 mbar) and refilled with dry CO2 (1.0 bar). The flask was slowly warmed to room temperature and stirred overnight, whereupon volatiles were removed in vacuo to give 5 as a colourless solid (0.099 g, 95%). N.B. X-ray quality crystals of 5 were obtained by recrystallizing this solid from warm benzene. 1H NMR (400 MHz, C6D6, 298 K): δ = 0.93 (d, 3JHP = 12.1 Hz, 27H, PC(CH3)3), 1.23 (d, 3JHH = 6.8 Hz, 12H, ArCH(CH3)2), 1.27 (s, 18H, C(CH3)3), 1.50 (d, 3JHH = 6.9 Hz, 12H, ArCH(CH3)2), 1.60 (s, 6H, C(CH3)2), 3.85 (sept., 3JHH = 6.8 Hz, 4H, ArCH(CH3)2), 6.39 (d, 4JHH = 1.9 Hz, 2H, XA-o-CH), 6.75 (d, 4JHH = 1.9 Hz, 2H, XA-p-CH), 7.24-7.33 (m, 6H ArH); 13C{1H} NMR (126 MHz, C6D6): δ = 25.3, 26.7 (CH(CH3)2) 27.9 (C(CH3)2), 28.5 (CH(CH3)2), 31.9 (d, 2JCP = 3.8 Hz, P{C(CH3)3}3), 32.0 (C(CH3)3), 32.3 (C(CH3)2), 35.2 (C(CH3)3), 37.2 (C(CH3)2), 38.5 (d, 1JCP = 15.9 Hz, P{C(CH3)3}3), 106.7, 110.8, 124.1, 125.7, 132.4, 136.2, 140.5, 142.3, 144.5, 147.6, 148.5 (Ar-C), 242.3 (d, 2JCP = 134 Hz, CAu); 31P{1H} NMR (162 MHz, C6D6): 88.0 (s).

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