Preparations, crystal structures, and molybdenum-95 nuclear magnetic resonance spectroscopic studies of triphenylphosphine–gold–tetrathiomolybdate(VI) clusters

Abstract

The preparation, spectroscopic properties, and X-ray crystal structures of two triphenylphosphine–gold–thiomolybdate clusters are reported. [MoS₄(AuPPh₃)₂] crystallises in the triclinic space group P with a= 9.596(1), b= 10.630(1), c= 19.712(2)Å, α= 89.06(1), β= 80.87(1), γ= 66.99(1)°, and Z= 2. [MoOS₃(AuPPh₃){Au(PPh₃)₂}] crystallises in the monoclinic space group P2₁/c with a= 21.251(2), b= 10.535(1), c= 23.167(2)Å, β= 104.20(1)°, and Z= 4. The structures have been solved from 5 748 and 7 476 unique observed diffractometer data and have been refined to R= 0.031 and 0.036, respectively. The ⁹⁵Mo n.m.r. spectra of these and related copper and silver tetrathiomolybdate(VI) clusters consist of a single resonance, whose chemical shift depends on the mole ratio of added PPh₃ to Mo in the solution.