The reaction of UO_(2)(OAc)_(2) and Na_(9)[A-PW_(9)O_(34)]in solution with different pH values leads to the formation of two Keggin-type sandwich polyoxometalates,namely Na11H(H_(2)O)_(31)[Na(UO_(2))(A-PW_(9)O_(34))]_...The reaction of UO_(2)(OAc)_(2) and Na_(9)[A-PW_(9)O_(34)]in solution with different pH values leads to the formation of two Keggin-type sandwich polyoxometalates,namely Na11H(H_(2)O)_(31)[Na(UO_(2))(A-PW_(9)O_(34))]_(2)·7H_(2)O(1)and Na_(12)(H_(2)O)_(29)[Na(UO_(2))(A-PW_(9)O_(34))]_(2)·7H_(2)O(2),which have been characterized by single-crystal X-ray diffraction,FT-IR spectroscopy,and PXRD techniques.Compounds 1 and 2 crystallize in similar conditions with different pH values and show similar sandwich crystal structures except that one extra Na(I)ion acts as a bridging linker in compound 2 than in 1.It is notable that 1 exhibits excellent catalytic activity for the synthesis of sulfonyl pyrazoles via the condensation and cyclization reaction of sulfonyl hydrazides with 1,3-diketones,and the yield of the desired product is up to 99%.This is the first report to investigate the catalytic properties of U-containing polyoxometalates.展开更多
基金supported by the National Natural Science Foundation of China(22001034,22071045,21871026)the Open Fund of the Jiangxi Province Key Laboratory of Synthetic Chemistry(JXSC202008)the Research Found of the East China University of Technology(No.DHBK2019264,DHBK2019265,DHBK2019267).
文摘The reaction of UO_(2)(OAc)_(2) and Na_(9)[A-PW_(9)O_(34)]in solution with different pH values leads to the formation of two Keggin-type sandwich polyoxometalates,namely Na11H(H_(2)O)_(31)[Na(UO_(2))(A-PW_(9)O_(34))]_(2)·7H_(2)O(1)and Na_(12)(H_(2)O)_(29)[Na(UO_(2))(A-PW_(9)O_(34))]_(2)·7H_(2)O(2),which have been characterized by single-crystal X-ray diffraction,FT-IR spectroscopy,and PXRD techniques.Compounds 1 and 2 crystallize in similar conditions with different pH values and show similar sandwich crystal structures except that one extra Na(I)ion acts as a bridging linker in compound 2 than in 1.It is notable that 1 exhibits excellent catalytic activity for the synthesis of sulfonyl pyrazoles via the condensation and cyclization reaction of sulfonyl hydrazides with 1,3-diketones,and the yield of the desired product is up to 99%.This is the first report to investigate the catalytic properties of U-containing polyoxometalates.