Compound 3

[(4,5-bis(2,6-diisopropylanilido)-2,7-di-tert-butyl-9,9-dimethylxanthene)aluminyl](tri-tert-butylphosphine)gold

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 tBu3PAuI (0.143 g, 0.271 mmol) in toluene (10 mL) over 5 minutes at room temperature. The reaction mixture was stirred for a further 16 hours at room temperature before being filtered. The orange filtrate was concentrated in vacuo (ca. 5 mL) and slowly cooled to 5 °C overnight to give 3 as small colourless crystals (0.155 g, 52%). 1H NMR (400 MHz, C6D6, 298 K): δ = 0.96 (d, 3JHP = 12.1 Hz, 27H, PC(CH3)3), 1.21 (d, 3JHH = 6.8 Hz, 12H, CH(CH3)2), 1.25 (s, 18H, C(CH3)3), 1.50 (d, 3JHH = 6.9 Hz, 12H, CH(CH3)2), 1.64 (s, 6H, C(CH3)2), 3.76 (sept., 3JHH = 6.8 Hz, 4H, CH(CH3)2), 6.35 (d, 4JHH = 1.9 Hz, 2H, XA-o-CH), 6.76 (d, 4JHH = 1.9 Hz, 2H, XA-p-CH), 7.17-7.26 (m, 6H ArH); 13C{1H} NMR (126 MHz, C6D6): δ = 25.5, 25.6 (CH(CH3)2) 27.7 (C(CH3)2), 29.4 (CH(CH3)2), 31.9 (C(CH3)3), 32.4 (d, 2JCP = 5.9 Hz, P{C(CH3)3}3), 35.2 (C(CH3)3), 37.3 (C(CH3)2), 39.0 (P{C(CH3)3}3), 106.8, 110.9, 123.9, 125.7, 133.5, 142.2, 143.2, 143.9, 147.7, 148.5 (Ar-C); 31P{1H} NMR (162 MHz, C6D6): 107.3 (br.); anal. calc. for C59H89AlAuN2OP: C 64.58%, H 8.18%, N 2.55 %, found: C 64.29%, H 8.30%, N 2.64%.

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