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Thioglycolic acid (CH2COOHSH, 95%), anhydrous bismuth chloride (BiCl3), antimony chloride (SbCl3), 1,5-pentanediol (95%), technical grade trioctylphosphine (TOP),  200-mesh tellurium shots and 100-mesh selenium shots obtained from Sigma Aldrich were used without further purification. In a typical small-scale synthesis, we added ~0.08 mmol of tellurium or selenium to 2 ¨C 5 mL TOP and heated in the multimode 1250 W domestic microwave oven for 90 ¨C 120 s to obtain a faint yellow TOPchalcogen complex. We added ~0.04 mmol of BiCl3 or SbCl3 to 2.5 ¨C 10 ml of 1-5
pentanediol followed by sonication for 5 min to obtain a bismuth chloride or antimony chloride solution. The bismuth chloride solution turns yellow upon addition of 100 ¨C 350 µL of thioglycolic acid (TGA) due to thioligated bismuth complex formation. The solutions with TOP-chalcogen and thioligated bismuth (or antimony) were mixed and exposed to microwaves for ~30-60 s in a multi-mode domestic microwave oven or a
single-mode variable power 300 W CEM microwave oven equipped with the IR sensor for temperature control.

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