201501组会探索.pptx

Group Meeting 报告人：孙龙辉 the combination of polydentate ligands and POM assemblies with multiple coordination sites [{Ni(H2O)3}2(WO2)2(SbW9O33)2] (Ni2Sb2) containing six accessible water molecules being stable in solution in a wide pH range showing a structure that allows systematic compositional variations organic-ligand 2,5-pyzdc showed to be inert planar N,O-bis(bidentate) linkers 2,3-pyzdc Method 1. To a hot solution of Na10[{Ni(H2O)3}2(WO2)2(SbW9O33)2]·40H2O (620 mg, 0.10 mmol) in aqueous 1 M acetic acid/sodium acetate buffer (30 mL) pyrazine-2,3-dicarboxilic acid (33 mg, 0.20 mmol) was added. The resulting green solution was kept for 1 h at 90 °C, left to cool to room temperature, filtered to remove any insoluble residue, and placed in an open container. Green needles suitable for X-ray diffraction were obtained by slow evaporation of this solution at room temperature for ca. 1 month (final volume ca. 1 0 mL). (M2Sb2:2L) Method 2. To a hot solution of Na9[SbW9O33]·19H2O (251 mg, 0.10 mmol) in aqueous 1 M acetic acid/sodium acetate buffer (30 mL) NiCl2·6H2O (71 mg, 0.30 mmol) was added. After stirring for 10 min at 90 °C, pyrazine-2,3-dicarboxilic acid (33 mg, 0.20 mmol) was added. The resulting green solution was kept for 1 h at 90 °C, left to cool to room temperature, filtered to remove any insoluble residue, and placed in an open container. Green needles suitable for X-ray diffraction were obtained by slow evaporation of this solution at room temperature for ca. 1 month (final volume ca. 10 mL). ([SbW9O33]:3M:2L) [μ-(2,3-pyzdc)2{NaNi2(H2O)4Sb2W20O70}2] Infrared spectrum of Na-Ni4 compared to that of the Na10[{Ni(H2O)3} 2(WO2)2-(SbW9O33)2] precursor (Ni2Sb2) highlighting the modifications in the POM domain upon coordination of the 2,3-pyzdc anions. Thermal decomposition starts at room temperature with three severely overlapping mass loss stages of endothermic nature that correspond to dehydration, which is completed at ca. 335 °C and involves the release of 93