Crystal and molecular structure of trans-diazido(C-meso-5,12-dimethyl-1,4,8,11-tetra-azacyclotetr aecane)cobalt(III) azide

Abstract

Crystals of the blue-violet title complex are triclinic, space group P, with Z= 1 in a unit cell of dimensions a= 7.932(4), b= 7.232(4), c= 10.392(5)Å, α= 109.71(3), β= 124.07(2), and γ= 80.78(3)°, molecular symmetry required for both ions. The structure has been solved by the heavy-atom method and refined by full-matrix least-squares calculations to R 0.073 for 1 291 reflections measured by diffractometer. The cation has octahedral co-ordination with the macrocycle in C-meso configuration and trans azide groups. Principle bond lengths are Co–N(azide) 1.953(11), Co–N(macrocycle) 1.986(7) and 2.016(6), and N–N(azide) 1.172(15) and 1.166(21)Å. The crystal structure contains azide ions [N–N 1.165(17)Å] and macrocyclic cations linked to form sheets parallel to (010) by N–H⋯N hydrogen bonds (2.96 Å) which utilise all the N–H and terminal azide groups.