Compound 4

(tri-tert-butylphosphine)aura-N,N’-bis(diisopropyl)amidinato(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.

To a solution of 3 (0.100 g, 0.091 mmol) in toluene (10 mL) was added diisopropylcarbodiimide (0.016 mL, 0.100 mmol) at room temperature. The reaction mixture was stirred for 12 hours at room temperature whereupon volatiles were removed in vacuo to give 4 as an off-white powder (0.109 g, 98%). N.B. X-ray quality crystals of 4 were obtained by dissolving this off-white powder in the minimum volume of warm benzene (ca. 1 mL) and allowing the solution to slowly cool to room temperature overnight. 1H NMR (400 MHz, C6D6, 298 K): δ = 0.46 (d, 3JHP = 6.6 Hz, 6H, NCH(CH3)2), 1.07 (d, 3JHP = 12.9 Hz, 27H, PC(CH3)3), 1.17 (d, 3JHH = 6.6 Hz, 6H, ArCH(CH3)2), 1.31 (s, 18H, C(CH3)3), 1.38 (d, 3JHH = 6.7 Hz, 6H, ArCH(CH3)2), 1.40 (d, 3JHH = 6.6 Hz, 6H, ArCH(CH3)2), 1.56 (d, 3JHP = 6.5 Hz, 6H, NCH(CH3)2), 1.59 (d, 3JHH = 6.8 Hz, 6H, ArCH(CH3)2), 1.68 (s, 3H, C(CH3)2), 1.89 (s, 3H, C(CH3)2), 3.52 (sept., 3JHH = 6.6 Hz, 1H, NCH(CH3)2), 3.72 (sept., 3JHH = 6.8 Hz, 2H, ArCH(CH3)2), 4.23 (sept., 3JHH = 6.8 Hz, 2H, ArCH(CH3)2), 4.34 (sept., 3JHH = 6.6 Hz, 1H, NCH(CH3)2), 6.22 (d, 4JHH = 1.8 Hz, 2H, XA-o-CH), 6.76 (d, 4JHH = 2.0 Hz, 2H, XA-p-CH), 7.28-7.45 (m, 6H ArH); 13C{1H} NMR (126 MHz, C6D6): δ = 23.5 (C(CH3)2), 24.8 (NCH(CH3)2), 25.2, 25.9, 26.4, 26.5 (CH(CH3)2) 26.6, 27.0 (CH(CH3)2), 29.1 (NCH(CH3)2), 32.0 (PC(CH3)3), 32.1 (C(CH3)3), 34.0 (C(CH3)2), 35.2 (C(CH3)3), 37.0 (C(CH3)2), 38.8 (d, 1JCP = 14 Hz, PC(CH3)3), 50.5, 51.9 (NCH(CH3)2), 105.7, 111.0, 124.0, 124.5, 125.6, 128.4, 128.6, 131.5, 139.6, 145.2, 145.4, 147.2, 147.3, 148.8 (Ar-C), 219.9 (d, 2JCP = 101 Hz, CAu); 31P{1H} NMR (162 MHz, C6D6): 90.6 (s); anal. calc. for C66H103AlAuN4OP: C 64.79%, H 8.49%, N 4.58%, found: C 64.91%, H 8.54%, N 4.44%.

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