The volatile zinc thiolato complex Zn(SAr")2 (1) (Ar" = C6H2-f-Bu3-2,4,6) was characterized by variable-temperature and solid-state 13C CP-MAS NMR and X-ray crystallography. The compound is dimeric in the solid state, with trigonal-planar zinc coordinated to three sulfur ligands and asymmetric thiolato bridges. In benzene solution, 1 dissociates into two-coordinate monomers, while at low temperature dimeric species exist in dichloromethane or toluene. The skeletal bonding pattern and the asymmetry of the thiolato bridges are explained on the basis of EHMO calculations; the Zn-S bonds are essentially a in character, with negligible contributions from Zn-S (p-p)T interactions. Crystal data for 1: triclinic space group ; Z = 2; a = 10.333( 5), b -11.226( 9), c = 32.266(30) A; a = 81.29(2), ß = 86.12(2), y = 86.07(2)°; V= 3684.70 A1 23; R = 0.059, Re = 0.068 based on 4519 reflections with F0 > 2

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