Abstract: The syntheses of 2, 8, 17-trithia-in-[35,'2][9] metacyclophane, 2, 7, 16-trithia-in- [35~''][8] metacyclophane, and 2, 6, 1 5-trithia-in-[34s10][7] metacyclophane are described. Due to the extreme proximity of the apical methine hydrogen atoms and the centers of the aromatic rings, the compounds display very high field'H NMR resonances and very high frequency IR CH stretching bands. X-ray crystallographic analyses of the latter two ...