Rhenium Tris(pyrazolyl)Borate Oxothiolate Complexes: Syntheses and Structures
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The rhenium complexes TpReOCl(StBu) (I), TpReO(StBu)2 (II), and TpReO(SnC3H7)2 (III) are synthesized using two methods by analogy to the known thiophenyl complexes. Complexes I–III having more electron-donating alkylthiolate ligands are characterized by IR and NMR spectroscopy. The structures of complexes I–III are determined by X-ray diffraction analysis (СIF files CCDC nos. 1892096 (I), 1892097 (II), and 1892098 (III)). The temperature dependence of the spectra of the bis(thiolate) complexes allows one to determine the activation energy for the hindered rotation about the Re–thiolate ligand bond. The by-product of the reaction of TpReOCl2 with NaS-tert-Bu, binuclear oxygen-bridged complex TpReIVCl(S-tert-Bu)O(S-tert-Bu)2ReIVTp, is isolated and structurally characterized (СIF file CCDC no. 1892099).
Keywords:rhenium complexes thiolate complexes tris(pyrazolyl)borate hindered rotation temperature-dependent NMR
The quantum chemical calculations were performed in the framework of the state task of the Kurnakov Institute of General and Inorganic Chemistry (Russian Academy of Sciences) in the sphere of basic research. The study was carried out using the equipment of the Center for Collective Use Physical Methods of Investigation at the Kurnakov Institute of General and Inorganic Chemistry (Russian Academy of Sciences).
This work was supported by the Russian Foundation for Basic Research (project no. 16-03-00798) and the Presidium of the Russian Academy of Sciences (program no. I.35.2.3).
CONFLICT OF INTEREST
The authors declare that they have no conflict of interest.