Preparation and thennal alicUYus of 1,4-0xathian Complexes of Silver(I) perchlorate and Copper(I) perchlorate. CryBtalBtructures of perchlorato-l,4-oxathian silver(I), perchloratiobis-(1,4-oxathian) silver(I) and tetrakis (1,4-oxathian) copper(I) perchlor

The new compounds AgClO4 tx(lIl), AgCI04. 2tx(lV) and CuC104. 4tx (V) are reported. On heating, III and AgClO 4 3tx(I) explode without previous decomposition. IV and V also explode after partial loss of oxathian(tx). CuCIO 4' 3tx(lI) decomposes in two steps to CuCI without explosion. The crystal structures of III, IV and V havc been determined.III Orthorhombic Pea21, a = 9.597(5), b= 6.369(6), c= i3.643(4)A. Z'"4. R=0.080 for 836 rc­flexions. The structure is polymeric with square pyramidal coordination at the silver atom. Ag-S = 2.59 A, Ag-Q = 2.47 - 2.67 A. IV Monoclinic P21, a = 6.62(1), b = 16.80(2), c = 6.34(2) A, C'" 94.5°, z =2. R = 0.073 for 1303 reflexions. The structure is trigonal monomeric, with Ag-g = 2.44 A, Ag-Q = 2.62 A, S-Ag-S = 160.3°.V Monoclinic P21/n, a = 18.47(2), b = 7.75(1), c = 17.64(2) A, c = 92 5°, Z= 4. R = 0.097 for 1433 reflexions. The structure contains tetrahedral Cu (tx) 4+ cations Cu-S = 8.32 A. 

J D PATON ,J C BARNES ,C S BLYTH ,