Preparation and crystal structure of [Bi3I(C4H8O3H2)2(C4H8O3H)5]2-Bi8I30 containing the novel polynuclear [Bi8I30]6- anion

Preparation and crystal structure of the novel compound [Bi3I(C4H8O3H2)(2)(C4H8O3H)(5)](2)Bi8I30 are reported. The title compound is prepared by heating of BiI3 and diethylene glycol at 413 K in a sealed quartz glass tube filled with argon. Deep red single crystals are grown and applied to perform X-ray powder diffraction and X-ray single-crystal diffraction measurements. The compound crystallizes triclinic with space group P-1: Z = 2, a = 13.217(1) Angstrom, b = 15.277(1) Angstrom, c = 22.498(1) Angstrom, alpha = 84.33(1), beta = 73.18(1), gamma = 67.48(1). [Bi3I(C4H8O3H2)(2)(C4H8O3H)(5)](2)Bi8I30 comprises the novel polynuclear [Bi8I30](6-) anion and [Bi3I(C4H8O3H2)(2) (C4H8O3H)(5)](3+) as the cation. Cation as well as the anion can be assumed to represent intermediates between solid BiI3 and BiI3 completely dissolved in diethylene glycol. (C) 2002 Elsevier Science (USA). All rights reserved.