3 NEW COMPOUNDS CONTAINING MO3S4, W3S4 CORES PREPARED FROM M3S7X4 (M = MO, W,X = CL, BR) STARTING MATERIALS

Mo3(mu-3-S)(mu-S)3Cl4(PEt3)3(H2O)2.OPEt3 (1), Mo3(mu-3-S)(mu-s)3Br4(PEt3)3(OPEt2H)(H2O).2THF (2), and W3(mu-3-S)(mu-S)3Br4-(PEt3)3(OPEt2H)(H2O).2THF (3) were prepared by reacting triethylphosphine with Mo3S7Cl4, Mo3S7Br4, and W3S7Br4, respectively, in THF at room temperature. Compound 1 crystallizes in the monoclinic space group P2(1)/n with a = 13.290 (2) angstrom, b = 18.282 (4) angstrom, c = 17.934 (4) angstrom, beta = 93.95 (2)-degrees, V = 4347 (3) angstrom3, and Z = 4. Compounds 2 and 3 are isostructural and crystallize in the triclinic space group P1BAR. For 2, a = 12.908 (4) angstrom, b = 18.299 (6) angstrom, c = 12.153 (4) angstrom, alpha = 98.26 (2) degrees, beta = 116.69 (2) degrees, gamma = 77.21 (2) degrees, V = 2498 (3) angstrom 3, and Z = 2. For 3, a = 12.925 (4) angstrom, b = 18.318 (6) angstrom, c = 12.141 (4) angstrom, alpha = 98.41 (3) degrees, beta = 116.51 (3) degrees, gamma = 77.00 (3) degrees, V = 2503 (2) angstrom3, and Z = 2. All three compounds belong to the B1, M3X13 structure family. An explanation for the formation of the Et2HPO ligand in 2 and 3 is proposed.