Micro tof q daltonics spectrometer

The reactions were carried out under an argon atmosphere using standard Schlenk-line techniques. Dry solvents were obtained from a Solvent Purification System from Innovative Technology Inc. The thiaborane arachno-4-SB 8 H 12 , 28 the [PSH][arachno-4-SB 8 H 11 ] salt and Wilkinson's compound [RhCl(PPh 3 ) 3 ] were prepared according to the literature methods. 14, 29 All other reactants were used as received.
Infrared spectra were recorded on a Perkin-Elmer 100 spectrometer, using a Universal ATR Sampling Accessory. NMR spectra were recorded on Brüker Avance 300 MHz and AV 400 MHz spectrometers, using 31 P-{ 1 H}, 11 B, 11 B-{ 1 H}, 1 H, 1 H-{ 11 B} and 1 H-{ 11 B(selective)} techniques. Residual solvent protons were used as the reference (δ, ppm, dichloromethane, +5.32). 11 B chemical shifts are quoted relative to [BF 3 (OEt) 2 ] and 31 P chemical shifts are quoted relative to H 3 PO 4 . Mass spectra were obtained on a Micro Tof-Q Bruker Daltonics spectrometer. Elemental analyses C/H/N were carried out using a Perkin-Elmer 2400 CHNS/O analyzer.
Compounds 1 and 2 were prepared using optimized procedures that are different from those published by us in ref. 14. The new synthesis of 1 and 2 is reported below.