【作者】 张晓峰； 黄德光； 陈昌能； 刘秋田；

【Author】 Zhang Xiao-feng Huang De-guang Chen Chang-neng Liu Qiu-tian(State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences Fuzhou 350002)

【机构】 中国科学院福建物质结构研究所；

【摘要】 <正> 我们在用Mn(Ⅲ)或Mn(Ⅱ)同乙酰丙酮及2,5-dimercapto-1,3,4-thiadiazole的二钾盐反应时得到了两个24员大环二锰配合物,但利用其它金属离子的类似反应未获成功。为此我们用氯代乙酰丙酮与2,5-dimercapto-1,3,4-thiadiazole二钾盐直接反应,制备了配体2,5-di-(3-pentanedionylthio)-1,3,4-thiadiazole)(H2L),然后用该配体分别与Mn(Ⅱ),Ni(Ⅱ)及Fe(Ⅱ)的盐进行反应,获得了四个[ML(solvent)2]2类的24员大环二核金属化合物,分别为配合物[Mn2L2(DMF)4](1):[Mn2L2(H2O)2(DMSO)2]·2DMSO(2);[Ni2L2(H2O)2(DMF)2]·2DMF(3)和[Fe2L2(DMF)2(DMSO)2]·2CH2Cl2(4)。配合物1属三斜晶系,空间群P-1,晶胞参数:a=10.0088(8)A,b=11.3527(9)A,c=11.9496(9)A,α=69.39°,β=81.425(2)°,γ=84.084(2)°,V=1254.83(17)A3,Z=1,最后的修正因子R1=0.1074,wR2=0.2546。更多还原

【Abstract】 A novel ligand 2,5-di-(3-pentanedionylthio)-l,3,4-thiadiazole) (H2L) has been synthesized by the reaction of dipotassium l,3,4-thiadiazole-2,5-dithiolate with 3-chloroacetylacetone, and used to directly react with the metal (Ⅱ) (M = Mn, Ni, Fe) salt to get four 24-membered macrocyclic di-metal complexes: [Mn2L2(DMF)4] (1); [Mn2L2(H2O)2(DMSO)2] ·2DMSO (2) ; [Ni2L2(H2O)2(DMF)2]·2DMF (3) [Fe2L2(DMF)2(DMSO)2]·2CH2Cl2 (4). These complexes were characterized by elemental analyses, IR and X-ray diffractions.更多还原