摘要
室温下将[Ni(L)](ClO4)2(L=3,10-diethyl-1,3,5,8,10,12-hexaazacycloctadecane)的DMF溶液和K3[Cr(CN)6]的水溶液在U型管中扩散反应合成了标题化合物:{[Ni(L)]3[Cr(CN)6]2·9H2O}n(化学式为C48H108Cr2N30 Ni3O9,Mr=1 529.77),晶体属三方晶系,空间群P3,晶胞参数a=1.4895(2)nm,b=1.4895(2)nm,c=0.9774(2)nm,α=90°,β=90°,γ=120°,V=1.8779(5)nm3,Z=1,dc=1.353g·cm-3,F(000)=810,R1=0.0474,wR2=0.1579.该化合物为二维蜂窝网状层结构,每个[Cr(CN)6]3-通过三个C3对称轴以氰基与三个[Ni(L)]2+顺式配位,其余三个CN-为端基,而每个[Ni(L)]2+中的Ni为六配位的八面体构型,其中赤道平面上的四个N原子来自于大环配体,轴向位置上的两个N原子分别来自于两个不同的[Cr(CN)6]3-中的氰基N原子.
The title compound {[Ni(L)]3[Cr(CN)6]2·9H2O}n(L=3,10-diethyl-1,3,5,8,10,12-hexaazacy-cloctadecane) was synthesized by slow diffusion of an aqueous solution of K3[Cr(CN)6] and a solution of [Ni (L)](C1O4)2 in DMF,which were installed by agar in the U-shape tube at room temperature. The crystal of the compound is trigonal system,space group P3,a = 1.489 5(2) nm,b = 1.489 5(2) nm,c = 0.977 4(2)nm,α=β =90°,γ= 120°, V= 1.8779(5) nm3,Z= l,Dc = 1.353g·cm-3,F(000) = 810,R1=0.047 4,wR2 = 0.1579[Ⅰ >2a(Ⅰ)].The complex shows a 2D honeycomb- like layered structure. Each [Cr(CN)6]3- is coordinated to three [NiL]2+ by three C3-related cis cyanide groups. Each nickel(Ⅱ) ion is six-coordinate with four nitrogen atoms from the macrocyclic ligand in the equatorial plane and two nitrogen atoms from the bridging cyanide groups on different [Cr(CN)6]3- anions in axial positions.
出处
《苏州大学学报(自然科学版)》
CAS
2004年第4期67-71,共5页
Journal of Soochow University(Natural Science Edition)
基金
江苏省教育厅自然科学基金资助项目(01KJB150010)