论文部分内容阅读
将Ni(teta)(ClO_4)_2(teta=5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane)的DMF溶液和K_3[Fe(CN)_6]的水溶液在填充了琼脂冻胶的U型管中通过扩散反应,得到了标题化合物(H_2teta)_2{[Ni(teta)][Fe(CN)_6]_2}·17H_2O,该化合物晶体属三斜晶系,空间群P1,晶胞参数为a=0.9998(2)nm,b=1.5514(3)nm,c=1.6647(4)nm,α=114.15(2)°,β=100.91(2)°,γ=93.42(2)°,V=2.2863(10)nm3,z=1,Dc=1.196g?cm-3,F(000)=890,μ=5.84cm-1,GOF=0.894,R1=0.0582,wR2=0.1446[I>2σ(I)].该化合物的基本单元由2个[H_2teta]~(2+)阳离子、1个{[Ni(teta)][Fe(CN)_6]_2}~(4-)阴离子和17个水分子组成,它们之间通过N—H…N氢键而形成具有二维平面结构的超分子化合物.1.8～300K变温磁化率研究表明,化合物中三核体系Fe(s=1/2)-Ni(s=1)-Fe(s=1/2)中心原子间通过氰基桥联而发生强的铁磁相互作用,磁参数J=4.33cm-1,g=2.6,θ=60K.通过TG-DTG测定了配合物的热稳定性.
A DMF solution of Ni (teta) (ClO_4) _2 (teta = 5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane) and an aqueous solution of K_3 [Fe (CN) _6] The title compound (H 2 teta) _2 {[Ni (teta)] [Fe (CN) _6] _2} · 17H 2 O was obtained by diffusion reaction in a U-tube filled with agar jelly. The crystal of the compound belongs to the triclinic system Space group P1 with a = 0.9998 (2) nm, b = 1.5514 (3) nm and c = 1.6647 (4) nm with α = 114.15 (2) ° and β = 100.91 = 93.42 (2) °, V = 2.2863 (10) nm3, z = 1, Dc = 1.196g? Cm-3, F (000) = 890, μ = 5.84cm-1, GOF = wR2 = 0.1446 [I> 2σ (I)]. The basic unit of this compound consists of two [H 2 teta] 2+ cations and one {[Ni 4-) anions and 17 water molecules, which form a two-dimensional planar supramolecular compound through N-H ... N hydrogen bonds.The magnetic susceptibility of 1.8 ~ 300K shows that the three-core system Fe s = 1/2) -Ni (s = 1) -Fe (s = 1/2). The magnetic parameters J = 4.33cm-1 and g = 2.6, θ = 60K.The thermal stability of the complex was determined by TG-DTG.