Synthetic procedures for new mixed-donor macrocycle compounds were reported. The macrocyclic compounds were used in solvent extraction metal picrates such as Ag+, Hg2+, Cd2+, Zn2+, Cu2+, Ni2+, Mn2+, Pb2+, and Co2+. The metal picrate extractions were investigated at 25 +/-0.18 degrees C with the aid of UV-visible spectrometry. It was found that 6,7,9,10,12,13,23,24-octahydro-19H,26Hdibenzo[ h,t](1,4,7,13,16,22,10,19) dioxatetrathiadiazasiclotetracosine-20,27(21H,28H)dione showed selectivity towards Ag+, Hg2+, and Cd2+ among the other metals. The extraction constants (Log K-ex) and complex compositions were determined for the Ag+ and Hg2+ complexes for this compound and 9,10,12,13,23,24,26,27,29,30-decahydro-5H,15H-dibenzo-[h,w][1,4,7,13,16, 19,25-,10,22] dioxapentathiadiazacycloheptacosine-6,16(7H,17H)-dione.