New sulfur-containing mixed-donor macrocycles L 1− L 4 with different donor sets and/or ring sizes (L 1, 20-membered O3S2; L 2, 20-membered NO2S2; L 3, 20-membered O2S3; and L 4, 23-membered O4S2) were synthesized and structurally characterized by X-ray analysis.