Synthesis and structural characterization of complexes of the {Cp * Rh} and {MeRe} cores with pyridine-2-thiol ligand types.

Article abstract of DOI:10.1016/0020-1693(95)04785-9

Complexes of trimethylsilyl substituted pyridine-2-thiol with rhenium and rhodium have been prepared and structurally characterized. The reaction of methyltrioxorhenium with 3-trimethylsilylpyridine-2-thiol in toluene at 0 °C affords dark green plates of MeReO( η²-2-SC₅H₃N-3-SiMe₃)₂ (4). The reaction of [Cp *RhCl₂]₂ with 3-trimethylsilylpyridine-2-thiol in THF, followed by extraction in hexanes and recrystallization yields Cp *Rh( η²-2-SC₅H₃N-3-SiMe₃)( η¹-2-SC₅H₃N-3-SiMe₃) (5). Crystal data: 4: monoclinic, P2₁/c, a= 12.898(3), b =13.660(3), c = 13.192(3) A, β = 97.58(1)°, V = 2303(1) A³, Z = 4, D_calc= 1.010 g cm^-3; structure solution and refinement based on 2297 reflections converged at a conventional residual of 0.0465. 5: orthorhombic, Pna2₁, a = 8.579(2), 6 = 23.315(5), c = 15.341 (3) A, V = 3068(2) A³, Z = 4, D_calc = 1.305 g cm^-3; 1455 reflections, R = 0.0572.