SYNTHESIS AND CRYSTAL-STRUCTURE OF A MACROTRICYCLIC CHELATING AGENT

The reaction between benzyl-2,2'-iminobis[N-(chloroethanoyl)ethylamine ] and 1,4-diazacycloheptane in acetonitrile furnished as the main prod uct the 7/15-membered macrobicycle 7-benzyI-3,11-dioxo-1,4,7,10,13-pen taazabicyclo [11.3.2]octadecane, and a 7,7,30-macrotricyclic compound as a minor product. The structure of the minor 2:2 cyclization product , tricyclo[27.3.2.2(13,17)]hexatriacontane,azatricyc was established b y X-ray diffraction analysis. The macrotricyclic compound crystallizes in the triclinic space group P-1, cell dimensions alpha = 8.352(2), b = 10.195(2), c = 12.064(3) Angstrom, alpha = 94.44(2), beta = 100.84( 2), gamma = 94.26(2) and Z = 1 (D-x = 1.34 g cm(-3))