Synthesis and structural characterization of complexes of the {Cp*Rh} and MeRe cores with pyridine-2-thiol ligand types. Structures of MeReO(η2-2-SC5H3N-3-SiMe)2 and (η5-Me5C5)Rh(η-2-SC5H3N-3-SiMe3) if(η1-2-SC5H3N-3-SiMe3)

Add time:07/18/2019    Source:sciencedirect.com

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 recrystalization 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) Å, ß=97.58(1)°, V=2303(1) Å3, Z=4, Dcalc=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), b=23.315(5), c=15.341(3) Å, V=3068(2) Å3, Z=4, Dcalc=1.305 g cm−3; 1455 reflections, R=0.0572.

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