General considerations: All manipulations were performed using glove box and Schlenk/vacuum line techniques. Methanol and methylene chloride were dried over CaH 2 and distilled prior to use. Toluene and benzene were dried over Na and distilled prior to use. NMR spectra were acquired on a Bruker AMX 300 NMR spectrometer (300 MHz 1 H; 75.5 MHz 13 C; 121.5 MHz 31 P). 1 H and 13 C spectra were referenced to solvent signals. 31 P spectra were reference to an external H 3 PO 4 standard (δ = 0).

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... spectra were obtained on a Ocean Oprtics, Chem 2000-UV-VIS instrument. Photoluminescence spectra were obtained on a HoribaJobin Yvon FluoroMax-3 instrument. Micropowder analysis was preformed on a modified 1 Bruker SMART APEX system in Debye-Scherrer mode with exposures of 1200 x 2 seconds. Data was Collected using SMART 2 and interpreted and integrated using GADDS. 3 Synthesis of (Ph 3 P) 2 CuIn(S t Bu) 4 . Single source precursors were prepared according to a previously described procedure. 4 Na[InS t Bu] 4 was prepared by adding 0.48 ml (4.26 mmol) 2,2-dimethylpropanethiol to a methanol solution of NaOCH 3 formed by adding sodium (0.102 g, 4.45 mmol) to 15 mL methanol. After 30 min a methanol solution of InCl 3 (0.2308 g, 1.04 mmol) was added via cannula and the reaction mixture stirred for an 1 S.