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A selection of metallocene inclusion compounds with channel structured MOFs (MOF = Metal-Organic Framework) were obtained via solvent-fee adsorption of the metallocenes from the gas-phase. The adsorbate structures ferrocene 0.5@MIL-53(Al) (MIL-53(Al) = [Al(OH)(bdc)]n with bdc = 1,4-terephthalate), ferrocene0.25@MIL-47(V) (MIL-47(V) = [V(O)(bdc)]n), cobaltocene0.25@MIL-53(Al), cobaltocene0.5@MIL-47(V), 1-formylferrocene0.33@MIL-53(Al) , 1,1?dimethylferrocene0.33@MIL-53(Al), 1,1?- diformylferrocene0.5@MIL-53(Al) were determined from powder X-ray diffraction data and were analyzed concerning the packing and orientation of the guest species. The packing of the ferrocene guest molecules inside MIL-47(V) is significantly different compared to MIL-53(Al) due to the lower breathing effect and weaker hydrogen bonds between the guest molecules and the host network in the case of MIL-47(V). The orientation of the metallocene molecule is also influenced by the substituents (CH3 and CHO) at the cyclopentadienyl ring and the interaction with the bridging OH group of MIL-53(Al). The inclusion of redox active cobaltocene into MIL-47(V) leads to the formation of a charge transfer compound with a negatively charged framework. The reduction of the vanadium centers is stoichiometric. The resulting material is a mixed valence compound with a V3+/V4+ ratio of 1:1. The new compounds were characterized via thermal gravimetric analysis, infrared spectroscopy, solid state NMR, and differential pulse voltammetry. Both systems are 1D-channel pore structures. The metallocene adsorbate induced breathing effect of MIL-53(Al) is more pronounced compared to MIL-47(V), this can be explained by the different bridging groups between the MO6 clusters. The Royal Society of Chemistry 2010.
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Reference：
Iron Catalysis in Organic Synthesis | Chemical Reviews,
Iron Catalysis in Organic Synthesis: A Critical Assessment of What It Takes To Make This Base Metal a Multitasking Champion