Synthesis and X-ray structures of new chiral Ag(I) complexes with biaryl-based N4-donor ligands |
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| Authors: | Guofu Zi Li Xiang Qiuwen Wang Yuan Yang |
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| Affiliation: | a Department of Chemistry, Beijing Normal University, Beijing 100875, China
b School of Environment and Energy Engineering, Beijing University of Civil Engineering and Architecture, Beijing 100044, China |
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| Abstract: | Condensation of (R)-2,2′-diamino-1,1′-binaphthyl or (R)-6,6′-dimethylbiphenyl-2,2′-diamine with 2 equiv of 2-pyridine carboxaldehyde in toluene in the presence of molecular sieves at 70 °C gives (R)-N,N′-bis(pyridin-2-ylmethylene)-1,1′-binaphthyl-2,2′-diimine (1), and (R)-N,N′-bis(pyridin-2-ylmethylene)-6,6′-dimethylbiphenyl-2,2′-diimine (3), respectively, in good yields. Reduction of 1 with an excess of NaBH4 in a solvent mixture of MeOH and toluene (1:1) at 50 °C gives (R)-N,N′-bis(pyridin-2-ylmethyl)-1,1′-binaphthyl-2,2′-diamine (2) in 95% yield. Rigidity plays an important role in the formation of helicate silver(I) complexes. Treatment of 1, or 3 with 1 equiv of AgNO3 in mixed solvents of MeOH and CH2Cl2 (1:4) gives the chiral, dinuclear double helicate Ag(I) complexes [Ag2(1)2][NO3]2 (4) and [Ag2(3)2][NO3]2 · 2H2O (6), respectively, in good yields. While under the similar reaction conditions, reaction of 2 with 1 equiv of AgNO3 affords the chiral, mononuclear single helicate Ag(I) complex [Ag(2)][NO3] (5) in 90% yield. [Ag2(1)2][NO3]2 (4) can further react with excess AgNO3 to give [Ag2(1)2]3[NO3]2[Ag(CH3OH)(NO3)3]2 · 2CH3OH (7) in 75% yield. All compounds have been fully characterized by various spectroscopic techniques and elemental analyses. Compounds 1 and 5-7 have been further subjected to single-crystal X-ray diffraction analyses. |
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| Keywords: | Ag(I) complexes Synthesis Crystal structure Helix |
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