Abstract
Sulfur/oxygen-bridged incomplete cubane-type triphenylphosphine molybdenum and tungsten-clusters [Mo3S4Cl4(H2O)2(PPh3)3]·3THF (1A), [Mo3S4Cl4(H2O)2(PPh3)3]·2THF (2A), [Mo3OS3Cl4(H2O)2(PPh3)3]·2THF (1B), and [W3S4Cl4(H2O)2(PPh3)3]·2THF (1C) were prepared from the corresponding aqua clusters and PPh3 in THF/MeOH. On recrystallization from THF, procedures with and without addition of hexane to the solution gave 1A and 2A, respectively, while the procedures gave no effect on the formation of 1B and 1C. Crystallographic results obtained are as follows: 1A: monoclinic, P21/n, a=17.141(4) A, b=22.579(5) A, c=19.069(4) A, β=96.18(2)°, V=7337(3) A3, Z=4, R(R w)=0.078(0.102); 1C: monoclinic, P2 1/c, a=12.635(1) A, b=20.216(4) A, c=27.815(3) A, β=96.16(1)°, V=7062(2) A3, Z=4, R(R w)=0.071(0.083). If the phenyl groups are ignored, the molecule [Mo3S4Cl4(H2O)2(PPh3)3] in 2A has idealized CS symmetry with the mirror plane perpendicular to the plane determined by the metal atoms, while the molecule in 1A does not have the symmetry. The tungsten compound 1C is isomorphous with the molybdenum compound 2A. 31P NMR spectra of 1A, 2A, and 1C were obtained and compared with similar clusters with dmpe (1,2-bis(dimethylphosphino)ethane) ligands.
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