期刊
INORGANIC CHEMISTRY
卷 55, 期 9, 页码 4173-4182出版社
AMER CHEMICAL SOC
DOI: 10.1021/acs.inorgchem.5b02888
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资金
- University of Pisa
The 1:1 molar reactions of NbOX3 with SnBu3H, in toluene at 0 degrees C in the presence of oxygen/nitrogen donors, resulted in the formation of NbOX2L2 (X = Cl, L-2 = dme, 2a; X = Br, L-2 = dme, 2b; X = Cl, L = thf, 2c; X = Cl, L = NCMe, 2d; dme = 1,2-dimethoxyethane, thf = tetrahydrofuran), in good yields. The 1:2 reactions of freshly prepared 2d and 2b with the bulky NHC ligands 1,3-bis(2,4,6-trimethylphenyl)imidazol-2-ylidene, Imes, and 1,3-bis(2,6-dimethylphenyl)imidazol-2-ylidene, Ixyl, respectively, afforded the complexes NbOCl2(Imes)2, 3, and NbOBr2(Ixyl)(2), 4, in 5060% yields. The reactions of 2b with NaOR, in tetrahydrofuran, gave NbOCl(OR) (R = Ph, 5; R = Me, 6) in about 60% yields. All the products were characterized by analytical and spectroscopic techniques; moreover DFT calculations were carried out in order to shed light on synthetic and structural features. Compounds 3 and 4, whose molecular structures have been ascertained by X-ray diffraction, represent very rare examples of crystallographically characterized niobium-NHC systems.
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