期刊
INORGANIC CHEMISTRY
卷 50, 期 14, 页码 6711-6718出版社
AMER CHEMICAL SOC
DOI: 10.1021/ic200683e
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资金
- Ministry of Education, Culture, Sports, Science and Technology of Japan
- Engineering and Physical Sciences Research Council [EP/C542819/1] Funding Source: researchfish
- EPSRC [EP/C542819/1] Funding Source: UKRI
- Grants-in-Aid for Scientific Research [23350085, 22655038, 23655109, 23245027] Funding Source: KAKEN
Hydrogen-bonded assemblies of the two-electron reduced mixed-valence Keggin clusters [PMo12O40](5-) and [SiMo12O40](6-) were obtained by the one-pot electron-transfer reactions between p-phenylenediamine (PPD) or 2,3,5,6-tetramethyl-PPD (TMPPD) (donors) and H-3(+)[PMo12O40](3-) or H-4(+)[SiMo12O40](4-) (acceptors) in CH3CN. The redox states of the [PMo12O40](5-) and [SiMo12O40](6-) clusters were confirmed by the redox titrations and electronic absorption measurements. In (HPPD+)(3)(H+)(2)[PMo12O40](5-)(CH3CN)(3-6) (1), the N-H similar to O hydrogen-bonded interactions between the monoprotonated HPPD+ (or diprotonated H2PPD(2+)) and the [PMo12O40](5-) resulted in a windmill like assembly and hydrophilic one-dimensional channels are formed with a cross-sectional area of 0.065 nm(2), and these are filled by the CH3CN molecules. Also, the CH3CN molecules in salt 1 were removed by immersing the single crystals of 1 into H2O, CH3OH, and C2H5OH solvents. In the compound, (HTMPPD+)(6)[SiMo12O40](6-) (CH3CN)(6) (2), the N-H similar to O hydrogen bonded interactions between the monoprotonated HTMPPD+ molecules and the [SiMo12O40](6-) formed a Saturn-ring-like assembly. Each Saturn-ring was arranged into an hexagonally packed array via hydrogen-bonded and pi-stacking interactions of HTMPPD+, while the CH3CN solvent present in salt 2 are only found in the zero-dimensional isolated cavities.
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