A Folded Conformation of 1,4,8,11-Tetrathiacyclotetradecane in its Mercury Compound: l,4,8,11-Tetrathiacyclotetradecanedipicratomercury( II) Heminitromethane, [Hg(C10H20S4)· (C6H2N307)2] · 1/2CH3N02

Abstract

The crystals of 1,4,8,11-tetrathiacyclotetradecanedipicratomercury( II) heminitromethane, [Hg(C10H20S4) · (CsH2Ns01h] · 1/2CHsN02, are triclinic, spcrce group Pl with a = 1.2794(6), b = 1.3108(5), c = = 1.0090(3) nm, a= 92.85(3) 0 , fJ = 107.67(3)0 , y = 94.54(4) 0 , V = 1.60236 nm3, and Z = 2. The structure was solved by the heavy atom method and refined by the least-squares method to R = 0.030 for the 7321 unique reflections. It consists of discrete, well separated molecules. Coordination of the mercury atom is a distorted octahedron with four sulfur atoms (Hg-S distances are 245.8(1), 251.9(1), 262 .. 9(2), and 305.0(2) pm) from the macrocycle and two oxygen moms (Hg-0 distances are 253.1(3) and 255.8(3) pm) from the two picrates. The macrocycle is folded so that three sulfur atoms with short Hg-S bonds are in an equatorial and the fourth in an apical position. The conformation of the coordinated macrocycle is compared to the conformation of cyclotetradecane at 116 K and to the conformation of the free crysta-lline macrocycle