1261 Crystal structure analysis of [AuI, (AsMe,)]. monochic, P2Jm (No. 11). 2 = 4. R = 0.068 R, = 0.050 for 76 parameters and 759 observed reflections ( I > 3.00a(I)) collected at 296 K, Mo,,. p = 235.64cm-I. max. 28 = 47.1'. F(OO0) = 1192 on a Siemens R3VS diffractometer absorption correction applied (max./min. transmission 1.19l0.82). The structure was solved by direct methods. all non-hydrogen atoms were refined anisotropically. The hydrogen atoms were included in fixed calculated positions with assigned isotropic temperature factors.[27] Crystal structure analysis of [AuI,(PMe,j,]: orthorhombic, Pnma (No. 62). 0.047, R, = 0.052 for 65 parameters and 817 observed reflections ( I > 3.00 a(1)) collected at 296 K, Mo,,. p = 144.68 cm-I , max. 28 = 49.9". F(OO0) = 1288 on a Rigaku R6S diffractometer, absorption correction applied (max./min. transmission 1.00/-0.13). Thestructure wassolved by direct methods, all non-hydrogen atoms were refined anisotropically. The hydrogen atoms were included in fixed calculated positions with assigned isotropic temperature [28] Crystal structure analysis of [(Me,PO),H][AuI,]: monoclinic, 12/m (No. 12). =16.623(3), b = X.173(3), c = 6.228(2) A, 0 = 89.81(3)'. V = 846.0(7) A' , Z = 2, R = 0.037. R, = 0.043 for 38 parameters and 41 2 observed reflections ( I > 3.00 ~( 1 ) )collected at 296 K. Mo,,, p = 124.48 cm-', max. 20 = 45.0", F(000) = 572 on a Rigaku R6S diffractometer, absorption corrction applied (max./min. transmission 0.75/-0.66). The structure was solved by direct methods. all non-hydrogen atoms were refined anisotropically. The hydrogen atoms were included in fixed calculated positions with assigned isotropic temperature factors. Crystallographic data (excluding structure factors) for the structures reported in this paper have been deposited with the Cambridge Crystallogrdphic Data Centre as supplementary publication no. CCDC-179.108. Copies of the data can be obtained free of charge on application to The Director. CCDC, 12Union Road,