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将硝酸镍与烟酰胺混合,在EDTA存在和180℃温度下,水热反应,得到配合物{[N i4(nic)8(H2O)2].3H2O}∞(Hnic=烟酸).通过EA、IR和TG对其进行了表征,单晶X射线衍射对其结构进行了确证.晶体数据:monoclinic,space group P2(1)witha=10.7566(8),b=19.5438(15),c=13.7801(10),β=104.4860(3),Mr=1301.74,V=2804.8(4)3,Z=2,μ(MoKα)=1.405 mm-1,F(000)=1332,R=0.0625,wR=0.1541.结构分析表明:配合物是由四核[N i4(nic)8(H2O)2]单元,3个结晶水分子构成的三维网状{[N i4(nic)8(H2O)2].3H2O}∞配位聚合物.其中4个烟酸采用μ3-nic-N,O,O的三齿桥联配位方式,另外4个烟酸采用μ2-nic-N,O的双齿桥联配位方式,所有的N i原子都处在六配位的畸变八面体几何构型环境.TG结果表明:配合物具有很好的热稳定性.磁性研究表明:配合物中的N i2+与N i2+之间存在反铁磁性耦合,在2.0～300 K温度范围内,磁化率很好地遵循Curie-W eiss定律,拟合得C=5.24 cm3.K.mol-1,θ=-2.30 K.
The nickel nitrate is mixed with nicotinamide and hydrothermally reacted in the presence of EDTA at a temperature of 180 ° C. to obtain the complex {[N i4 (nic) 8 (H 2 O) 2] .3H 2 O} ∞ (Hnic = niacin) , IR and TG were used to characterize the structure and the crystal structures were confirmed by single crystal X-ray diffraction.Crystal data: monoclinic, space group P2 (1) witha = 10.7566 (8), b = 19.5438 (15), c = 13.7801 (10) β = 104.4860 (3) Mr = 1301.74 V = 2804.8 (4) 3 Z = 2 μ MoKα = 1.405 mm -1 F 000 = 1332 R = 0.0625 wR = The structure analysis shows that the complex is a three - dimensional network {[N i4 (nic) 8 (H2O) 2] composed of four core [N i4 (nic) 8 (H2O) 2] units and three crystal water molecules. 3H2O} ∞ coordination polymers, in which four nicotinic acids adopt the tridentate bridging coordination pattern of μ3-nic-N, O, O and the other four niacin adopt the bidentate bridging of μ2-nic-N, O Coordination mode, all the N i atoms are in hexacoordinated distorted octahedron geometry. TG results show that: the complex has good thermal stability. Magnetic studies show that: N i2 + and N In the temperature range of 2.0-300 K, the magnetic susceptibility follows the Curie-W eiss law, and the result shows that C = 5.24 cm3.K.mol-1 and θ = -2.30 K.