高い結晶性と純度を有する多孔性“貴金属”錯体の新合成法
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2010年度神奈川大学総合理学研究所共同研究助成論文We successfully synthesized high crystallinity Rh-based metal-organic frameworks (MOFs), {[Rh2(BDC)2][Cu2(BDC)2]}·4DMF (RhCu-DMF), {[Rh2(BDC)2]- [Zn2(BDC)2]}·3.8DMF (RhZn-DMF), and {[Rh2(BDC)2][Cu2(BDC)2]}·EtOH·2H2O (RhCu- EtOH), by assembly of discrete paddlewheel rhodium terephthalate (4) and Cu2+ or Zn2+ ions. We report these structures and their gas adsorption properties. RhCu-DMF, RhZn-DMF were synthesized by the reaction of 4 with Cu(NO3)2·3H2O or Zn(NO3)2·2H2O in DMF at 60°C for 2 h, and RhCu-EtOH was synthesized by solvothermal reaction of 4 with Cu(NO3)2·3H2O in EtOH at 100 ºC for 40 h. Elemental analysis data showed that rhodium and copper (or zinc) existed in a 1 : 1 mole ratio in these compounds. It is most likely that two types of paddlewheel cluster, i.e., Rh2 and Cu2/Zn2 units, alternately form vertices of a 2D square grid. X-ray powder diffraction (XRPD) data showed RhCu-DMF and RhZn-DMF to be isotypic with the structure of [Cu2(BDC)2] before desolvation. RhCu-EeOH was isotypic with that of [Cu2(BDC)2] re-solvated with EtOH. Although the reported Rh-based MOFs showed no diffraction pattern due to its low crystallinity, these three complexes show a sharp XRPD pattern. The N2 adsorption isotherms of RhCu-DMF, RhZn-DMF, and RhCu-EeOH revealed type I behavior, indicating the retention of microporous structures after removal of the solvent molecules from the channels.
- 2011-06-30
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