Synthesis and structure of tetrakis(tetramethylammonium) octacosachlorooctaantimonate(III) [(CH3)(4)N](4)Sb8Cl28

The reaction between antimony trichloride and tetramethylammonium chloride in nitromethane gives transparent, irregular crystals of tetrakis(tetrameth ylammonium) octacosachlorooctaantimonate(LII) [(CH3)(4)N](4)Sb8Cl28. Crysta ls are triclinic, space group P-l, a = 11.846(2), b = 12.217(2), c = 14.120 (3) Angstrom, alpha = 95.71(3), beta = 101.39(3), gamma = 118.59(3)Angstrom , V = 1713.7(5) Angstrom (3), Z = 1, d(c) = 2.193, d(m) = 2.17(2) Mg m(-3). The structure contains a structurally novel Sb8Cl284- anion. It is compose d of eight deformed octahedra, connected with each ether by faces. In cavit ies formed by inorganic sublattice are located two crystallographically non equivalent tetramethylammonium cations. One of them is disordered in such a way that all (C, N, H) atoms are split between two positions with occupanc y factors 0.5. (C) 2000 Elsevier Science B.V. All rights reserved.