(Bu_4N)[Ni(dmit)_2]的一步合成及一种新晶相  

One-step Synthesis of (Bu_4N)[Ni(dmit)_2] and Its New C2/c Crystalline Phase

作　　者：方奇[1] 夏光明[1] 刘国群[1] 许文[1] 

机构地区：[1]山东大学晶体材料国家重点实验室,济南250100

出　　处：《化学学报》2003年第8期1319-1322,共4页Acta Chimica Sinica

基　　金：国家自然科学基金 (No.2 0 1 72 0 34);高等学校骨干教师资助计划;国家重点基础研究发展规划 (No.G1 9980 61 4 0 2 )资助项目

摘　　要：用中心离子替代和空气自动氧化的方法由 (Bu4N) 2 [Zn(dmit) 2 ]一步合成了 (Bu4N) [Ni(dmit) 2 ] .这种方法可推广到其它Z[M(dmit) 2 ]配合物和Z[M(dmit) 2 ] 2 导电配合物的合成 .(Bu4N) [Ni(dmit) 2 ]结晶过程中出现两个晶相 ,其中空间群为C2 /c的侧心单斜相为新晶相 .X射线结构测定结果为 :a =2 0 191(2 )nm ,b =1 3 40 4(1)nm ,c =1 2 14 1(1)nm ,β =10 5 5 5 (1)° ,V =3 165 5 (6)nm3 ,R =0 0 5 5 .晶体中的 [Ni(dmit) 2 ] -呈D2h点群对称性 ,平面性接近完美 ,共轭性相当显著 .相邻 [Ni(dmit) 2 ] -平面间的夹角为 75 5 6(3 )° .(Bu4N)[Ni(dmit)(2)] was synthesized by substituting Zn2+ in (Bu4N)(2)[Zn(dmit)(2)] with Ni2+ and by auto-oxidation in acetone solution. This simple method can be extended to synthesize other Z [M(dmit)(2)] type complexes and Z[M(dmit)(2)](2) type conductive complexes. Two crystalline phases of (Bu4N) [Ni(dmit)(2)], namely triclinic P (1) over bar phase and monoclinic C2/c phase which has been proved new, were obtained. The crystalline data of the C2/c phase are: a = 2.0191(2) nm, b = 1.3404(1) nm, c = 1.2141(1) nm, beta = 105.554(8)degrees, V = 3165.5(6) nm(3), R = 0.055, C2/c space group.

关 键 词：(Bu4N)[Ni(dmit)2] 合成 晶相 侧心单斜相 晶体结构 配合物 配位阴离子 

分 类 号：O641.4[理学—物理化学] O76[理学—化学]