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作 者:王虎林[1] 薛岗林[1] 王继武[2] 王大奇[3] 李君[1] 史启祯[1] WANG Hu-Lin;XUE Gang-Lin;WANG Ji-Wu;WANGDa-Qi;LI Jun;SHI Qi-Zhen(Shaanxi Key Laboratory of Physico-Inorganic Chemistry,Department of Chemistry.Northwuest University,Xi'an 710069;State Key Laboratory of Coordination Chemistry,Nanjing University,Nanjing 210093;Department of Chemistry and Chemical Engineering,Yan'an University,Yan'an 716000;Department of Chemistry,Liaocheng University,Liaocheng 252000)
机构地区:[1]西北大学化学系陕西省物理无机化学重点实验室,西安710069 [2]延安大学化学化工学院陕西省化学反应工程重点实验室,延安716000 [3]聊城大学化学系,聊城252000
出 处:《化学学报》2003年第11期1839-1843,共5页Acta Chimica Sinica
基 金:高等学校重点实验室访问学者基金;陕西省化学反应工程重点实验室开放基金资助项目
摘 要:在pH=75的水溶液中,咪唑与Na_(2)WO_(4),Bi(NO_(3))_(3)及Co(NO_(3))_(2)反应,得到了咪唑配位的新型杂多钨酸盐Na_(9)[{Na(H_(2)O)_(3)}{Co(C_(3)H_(4)N_(2))}_(3)(BiW_(9)O_(33))_(2)]·33H_(2)O,用X射线单晶衍射法及元素分析确定了其结构,晶胞参数为:空间群P3-,a=13904(4)nm,b=13904(4)nm,c=33169(13)nm,γ=120°,V=5553(3)nm^(3),Z=2,R_(1)=00361,wR_(2)=00507(I>2σ).杂多阴离子[{Na(H_(2)O)}_(3){Co(C_(3)H_(4)N_(2))}_(3)(BiW_(9)O_(33))_(2)]^(9-)为夹心式结构,两个三空缺Keggin离子αB BiW_(9)O^(9-)_(33)夹层中的中心离子为交替排列的三个Na(H_(2)O)+和三个Co(C_(3)H_(4)N_(2))^(2+),中心离子钴的配位数为5,该杂多阴离子具有C3v对称性.对标题化合物进行了磁性质表征,拟合结果为J=690cm^(-1),g=210,θ=025K,表明该化合物中的Co(II)The imidazole coordinated novel heteropolyoxometalate Na_(9)[{Na(H_(2)O)}_(3){Co(C_(3)H_(4)N_(2))}_(3)(BiW_(9)O_(33))_(2)]·33H_(2)O was synthesized by the reaction of Na_(2)WO_(4)·2H_(2)O with Bi(NO_(3))_(3)and Co(NO_(3))_(2)in pH=75 aqueous solution.The single crystal X ray diffraction study shows that the crystal belongs to trigonal system,space group P 3-,with a=13904(4)nm,b=13904(4)nm,c=33169(13)nm,γ=120°,V=5553(3)nm 3,Z=2,R_(1)=00361,wR_(2)=00507(I>2σ).The structure of anion[{Na(H_(2)O)}_(3){Co(C_(3)H_(4)N_(2))}_(3)(BiW_(9)O_(33))_(2)]9-reveals a sandwich like arrangement of two{αB AsW 9}moieties enclosing three Co(C_(3)H_(4)N_(2))^(2+)and three Na(H_(2)O)^(+).The coordination number of Co^(2+)and Na+in the sandwich anion are all five,and the polyanion has C_(3v)symmetry.Magnetic data have been fitted assuming that the only exchange coupled centers are the cobalts,the compound exhibits ferromagnetic coupling with J=690 cm^(-1),g=210,andθ=025 K.
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