The rhenium dithiodiolate, Hydrido-tris-(3 ,5-dimethyl- 1 -pyrazol yl) borato(ethane- 1 ,2-dithiodiolato)(oxo)rheni um(V), and Hydrido-tris-(3 ,5-dimethyl- 1 -pyrazolyl)borato(phenylethanedithiodiolato)(oxo)rhenium(V), were synthesized by reductive cyclocondensation of alkane-1,2-dithiols with Tp'Re0₃ in a one pot fashion. The rhemium monothiodiolate, Hydrido-tris-(3 ,5-dimethyl- 1 -pyrazolyl) borato(ethane- 1 ,2-monothiodiolato)(oxo)rhenium(V), and Hydrido-tris-(3 ,5- dimethyl- 1 -pyrazolyl)borato(propanemonothiodiolato)(oxo)rhenium(V), were also synthesized...