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note
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2 (36.6 mg, 0.098 mmol) were dissolved in 1,2-dichlorobenzene (dcb, anhydrous, 3.0 mL) and ethanol (anhydrous, 2.0 mL). The solution was filtered and the filtrate collected in a small vial. The vial was then placed in ajar that had previously been charged with a mixture of dcb (anhydrous, 8.0 mL) and pentane (anhydrous, 8.0 mL). Slow vapor exchange between the reaction mixture (in the vial) and the reservoir (in the jar) over two weeks yielded black, blocklike crystals suitable for X-ray dataset collection (yield: 18.4 mg, 43% based on 1b). X-ray powder diffraction studies indicated a single phase consistent with the single crystal structure. EDX (using a Shimadzu energy dispersive fluorescence X-ray spectrometer, Rayny series, EDX-700/800) spectrometry of the product indicated the Te/I ratio to be 1.0/5.2. The EDX measurement also indicated a small amount of Sncontaining impurities (amorphous) in the product (Sn/Te ratio about 1/10). Experiments for better product purity and for characterizing the other products are ongoing (also see Supporting Information for a proposed equation of the overall reaction, Figure S5).
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note
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int= 2.6%, R1/wR2 = 6.54/18.48% for 4210 unique observed reflections [I > 2σ(I)] and 136 variables (R1/wR2 = 7.91/19.06% for all data).
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