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[PtMe(iPr3P)(2)](+): a Pt(II) complex with an agostic interaction that undergoes C-H activation

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Abstract

SUPPORTING INFORMATION EXPERIMENTAL General Methods. All manipulations were performed under an inert atmosphere of argon, using standard Schlenk-line and glove box techniques. Glassware was dried in an oven at 130°C overnight and flamed with a blowtorch, under vacuum, three times before use. CH2Cl2, pentane was distilled from CaH2, C6H5F was distilled from P2O5 under vacuum and CD2Cl2 was distilled under vacuum from CaH2. 1H, 11B, 13C and 31P NMR spectra were recorded on a Bruker Advance 300 MHz or a Bruker Advance 400 MHz FT-NMR spectrometers. Residual protio solvent was used as reference for 1H NMR spectra (CD2Cl2: δ = 5.33) and 13C NMR spectra (CD2Cl2: δ = 53.8). 11B and 31P NMR spectra were referenced against BF3.OEt2 (external) and 85% H3PO4 (external) respectively. Infrared spectra were recorded on a Nicolet NEXUS FT-IR spectrometer. Solution spectra were recorded using a 0.1mm solution cell. Microanalysis of all the new compounds was consistently low in %C, even though performed on crystalline material pure by NMR spectroscopy (>99%). (iPr3P)2PtMe2, 1 [CPh3][1-H-closo-CB11Me11] 2 and [1-H-closo- C B11Me11]• 3 were synthesised using literature procedures or modifications thereof. The compounds B(C6F5)3 and 2,6 –di- tbutylpyridine were used as purchased. [(iPr3P)2Pt(Me)][1-H-closo-CB11Me11]: A Young’s ampoule was charged with equimolar quantities of [(iPr3P)2PtMe2] (0.020g) and [1-H-closo-CB11Me11]• (0.011g) (or alternatively 0.020g of CPh3[1-H-closo-CB11Me11] and then dissolved in 5ml of C6H5F, resulting in the formation of a yellow solution. Yellow crystals were obtained (0.024g) by the slow diffusion of pentane at -20ºC. Yield: 79% δ1H (298K, CD2Cl2): 2.56 (m, 6H, iPr CH), 1.69 (t, 3H, Pt-Me, 2J(PtH) 106, 3J(PH) 5.6), 1.34 (dd, 42H, iPr CH3, 3J(PH) 14.8 3J(HH) 7.6), 1.15 (s, 1H CHcage), -0.18 (s, 15H, B-CH3(2-6)), -0.43 (s, 15H, B-CH3(7-11)), -0.55 (s, 3H, B-CH3(12)). δ31P{1H} (298K, CD2Cl2): 47.1 ( 1J(PtP) 2757) δ11B (298K, CD2Cl2): -0.51 (s, 1B), -8.60 (s,

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