SYNTHESIS AND STRUCTURAL CHARACTERIZATION OF COMPLEXES OF THE (CP(ASTERISK)RH) AND (MERE) CORES WITH PYRIDINE-2-THIOL LIGAND TYPES - STRUCTURES OF MEREO(ETA(2)-2-SC5H3N-3-SIME)(2) AND (ETA(5)-ME(5)C(5))RH(ETA(2)-2-SC5H3N-3-SIME(3))(ETA(1)-2-SC5H3N-3-

摘要

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 degrees C affords dark green plates of MeReO(eta(2)-2-SC5H3N-3-SiMe(3))(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(eta(2)-2-SC5H3N-3-SiMe(3)) (eta(1)-SC5H3N-3-SiMe(3)) (5). Crystal data: 4: monoclinic, P2(1)/c, a=12.898(3), b=13.660(3), c=13.192(3) Angstrom, beta=97.58(1)degrees, V=2303(1) Angstrom(3), 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, Pna2(1), a=8.579(2), b=23.315(5), c=15.341(3) Angstrom, V=3068(2) Angstrom(3), Z=4, D-calc=1.305 g cm(-3); 1455 reflections, R=0.0572. [References: 56]