Crystal structures are reported for 2,4-(O2N)2C6H3X (2: X = NMe,; 3: X = C6H4N02-2) and Ph3MSC6H4N02-2 (4: M=Ge; 5; MtSn; 6: M=Pb). Compound 2 is triclinic, Pbarl, a = 7.931( 5), b = 8.159(7), c = 9.090(7) A, a = 100.35(6), /j=81.00(6), y = 110.74(6)", D, = 1.500 Mg.m -', Z = 2, observed reflections = 834, R = 0.066 (Rw = 0.049). Compound 3 is orthorhombic, P212121, a = 11.1424(18), b = 11.8067(18), c = 20.363(3) A, D,= 1.593 Mg.m-', Z = 8, observed reflections = 925, R = 0.061 (Rzu = 0.074). Compound 4 is monoclinic, PZ1 /a, a = 14.73(4), b = 10.091(5), c = 15.526(4) A, /I= 107.43(7), D, = 1.382 Mg.m ', Z = 4, observed reflections = 2034, R1 = 0.0426 (wR2 = 0.0834). Compound 5 is orthorhombic, Pbca, n = 15.489(10), b = 15.701(5), c = 17.558(7) A, D, = 1.569Mg.mp', Z = 8, observed reflections = 2537,Rl = 0.0327 (zuR2 = 0.0700). Compound 6 is orthorliombic, Pbca, a = 15.569(5), b = 15.702(3), c = 17.651(6) A, D, = 1.825Mg.mp', Z = 8, observed reflections = 2536, R 1 = 0.0323 (wR2 = 0.0737). There are short non-bonded S-0 interactions and near ?inear 0-S-Xangles In bott 2 and 3; values are 2.166(6) A and 177.1(3)" for 2; 2.582(14) A and 177.1(8)", and 2.609(13)A and 177.9(6) (in two independent molecules) for 3. The S -0 interaction in 3 involves the ovtho nitro group of the dinitrophenyl ring. Intramolecular S -0 interactions are absent in 4-6; however there are weak intermolecular M-0 bonding in 5 and 6, which results in molecules being linked into chains; the geometries at the metal centres in 5 and 6 are distorted trigonal bipyramidal with Sn-0 and Pb-0 bond lengths of 3.337(3) and 3.180(5) A, respectively, and Saxla~-M-Oa,,,~ angles of 173.19(5) and 173.96(9)", respectively. Compound 4 is essentially tetrahedral.
