We demonstrate an ew material by intercalating Mo 3 S 13 2À into Mg/Al layered double hydroxide (abbr.Mo 3 S 13 -LDH), exhibiting excellent capture capability for toxicH g 2+ and noble metal silver (Ag). The as-prepared Mo 3 S 13 -LDH displays ultra-high selectivity of Ag + ,H g 2+ and Cu 2+ in the presence of various competitive ions,w ith the order of Ag + > Hg 2+ > Cu 2+ > Pb 2+ ! Co 2+ ,N i 2+ ,Z n 2+ ,C d 2+ .F or Ag + and Hg 2+ ,e xtremely fast adsorption rates ( % 90 %w ithin 10 min, > 99 %i n1h) are observed. Much high selectivity is present for Ag + and Cu 2+ ,e specially for trace amounts of Ag + ( % 1ppm), achieving al arge separation factor (SF Ag/Cu )o f % 8000 at the large Cu/Ag ratio of 520. The overwhelming adsorption capacities for Ag + (q m Ag = 1073 mg g À1 )a nd Hg 2+ (q m Hg = 594 mg g À1 )p lace the Mo 3 S 13 -LDH at the top of performing sorbent materials.M ost importantly,M o 3 S 13 -LDH captures Ag + via two paths:a )f ormation of Ag 2 Sd ue to Ag-S complexation and precipitation, and b) reduction of Ag + to metallic silver (Ag 0 ). The Mo 3 S 13 -LDH is ap romising material to extract low-grade silver from copper-rich minerals and trap highly toxic Hg 2+ from polluted water.

We demonstrate an ew material by intercalating Mo 3 S 13 2À into Mg/Al layered double hydroxide (abbr.Mo 3 S 13 -LDH), exhibiting excellent capture capability for toxicH g 2+ and noble metal silver (Ag). The as-prepared Mo 3 S 13 -LDH displays ultra-high selectivity of Ag + ,H g 2+ and Cu 2+ in the presence of various competitive ions,w ith the order of Ag + > Hg 2+ > Cu 2+ > Pb 2+ ! Co 2+ ,N i 2+ ,Z n 2+ ,C d 2+ .F or Ag + and Hg 2+ ,e xtremely fast adsorption rates ( % 90 %w ithin 10 min, > 99 %i n1h) are observed. Much high selectivity is present for Ag + and Cu 2+ ,e specially for trace amounts of Ag + ( % 1ppm), achieving al arge separation factor (SF Ag/Cu )o f % 8000 at the large Cu/Ag ratio of 520. The overwhelming adsorption capacities for Ag + (q m Ag = 1073 mg g À1 )a nd Hg 2+ (q m Hg = 594 mg g À1 )p lace the Mo 3 S 13 -LDH at the top of performing sorbent materials.M ost importantly,M o 3 S 13 -LDH captures Ag + via two paths:a )f ormation of Ag 2 Sd ue to Ag-S complexation and precipitation, and b) reduction of Ag + to metallic silver (Ag 0 ). The Mo 3 S 13 -LDH is ap romising material to extract low-grade silver from copper-rich minerals and trap highly toxic Hg 2+ from polluted water.