The crystal structure determinations of some halide complexes of antimony

Abstract

Bispiperidinium Sb(III)Br₅ (piperidine = [see PDF for diagram] forms orthorhombic crystals, P2₁2₁2₁, a = 18.415(3), b = 12.507(3), c = 8.851(2) Å at 22°C, Z = 4. The structure is isomorphous with its Bi(III) Br₅. analogue. The anion has a distorted octahedron of Br atoms around Sb, with bridging distances Sb-Br(3) = 3.017(3), Sb-Br(31) = 3.125(3) Å, and angle Br(3)-Sb-Br(3') = 92.3(1)°. O Opposite the bridges are Sb-Br(2) = 2.625(3) Å and Sb-Br(5) = 2.569(3) A and the remaining distances are Sb-Br(l) = 2.766(3) Å and Sb-Br(4) = 2.828(2) Å. (No corrections were made for thermal motion.) The results of both photographic and diffractometer data are compared. From the diffractometer data it is possible to distinguish between (x,y,z) and ([x bar, y bar, z bar]) from effects due to anomalous dispersion. The rings are in the chair conformation and show normal distances and angles. The N atom positions were inferred from close contacts with Br atoms since the diffraction data alone did not permit a distinction to be made between N and C. ...