SYNTHESIS AND STRUCTURAL CHARACTERIZATION OF MO2S4[S2CNC4H8]2 AND ITSREACTIONS WITH CU+, NI2+

Mo2S4[S2CNC4H8]2 (1) is obtained by the reaction of (NH4)2Mo2S12 . 2H2 O with (NH4) [S2CNC4H8] in the presence of PPh3. The compound 1 has be en characterized by IR, UV-Vis, electrochemistry, and X-ray crystallog raphy. Attempts have also been made to carry out [2 + 1] reactions bet ween 1 and several other metals such as Cu+ and Ni2+. It is found from the structural analysis of the products that there are three kinds of reactions including the capture of terminal S2- by the metal ions to yield Mo2O2S2[S2CNC4H8]2(2); the oxidation of Cu+ and the capture of [ S2CNC4H8] - ligands to form Cu [S2CNC4H8] 2(3) and the reduction of Mo (V) to Mo(IV) and the oxidation of S2- to (S2)2- to give {Mo3S7[S2CNC4 H8] 3 . I} (4). The crystal data of each compound are as follows, 1 tr iclinic, P1BAR, a = 0. 9057 (2), b = 1.7162, c = 0.6578(1)nm, alpha = 90.49(3)-degrees, beta = 102.12(2)-degrees, gamma = 96.57(3)-degrees, V = 0.9926(5) nm3, Z = 2, D(c) = 2.05 g/cm3, R = 0.045, R(w) = 0.052. 2 triclinic, P1BAR, a = 0.8754 (2), b = 1. 6560 (4), c = 0.6678(2)nm, alpha = 97.74(2)-degrees, beta = 97.90(2)-degrees, gamma = 80.31(2)-de grees, V = 0.9390(4)nm3, Z = 2, D(c) = 2.05 g/cm3, R = 0.036, R(w) = 0 . 043. 3 triclinic, P1BAR, a = 0. 7483 (2), b = 0.8070 (2), c = 0.6381 (1)nm, alpha = 104.86(2)-degrees, beta = 94.06(2)-degrees, gamma = 76. 59(2)-degrees, V = 0.3623(2)nm3, Z = 1, D(c) = 1.63 g/cm3, R = 0.042, R(w) = 0. 051. 4 Monoclinic, P2(1)/a, a = 1.6488(8), b = 1.7043(9), c = 1.1349(4)nm, beta = 90.34(5)-degrees, V = 3.189(3)nm3, Z = 4, D(c) = 2.24 g/cm3, R = 0.050, R(w) = 0.058. Finally, the reactivities of 1 a nd the structures of these crystals are discussed.