吡啶-2-甲酸镍的合成及其晶体结构

以吡啶 2 甲酸和Ni(ClO4)2·6H2O为原料反应制得配合物Ni(C5H4NCOO)2(H2O)2]2H2O,并通过X 射线衍射法测定其晶体结构.该化合物属于单斜晶系,空间群P21/n,晶胞参数:a=0.97351(15)nm,b=0.52254(8)nm,c=1.4483(2)nm,β=90.119(3)°,V=0.7367(2)nm3,Z=2,Dc=1.690g/cm3,μ=1.362mm 1,F(000)=388,结构偏离因子R1=0.0316,wR2=0.0902,共收集到4771个强度数据,其中1700个独立衍射点,1489个(I>2σ(I))可观测点.X 射线分析表明晶体是由分子间氢键和π π弱相互作用堆积而成的二维层状结构.

Synthesis and Crystal Structure of Nickel (Ⅱ) Complex with Picolinic Acid

The title complex was synthesized by the reaction of picolinic acid and Ni(ClO4)2·6H2O in mixed solvents of water and ethanol. The crystal structure was determined by single crystal X ray diffraction method and characterized by elemental analysis and IR spectrum. The main crystal date is as follows: monoclinic, space group P21/n with cell parameters, a=0.973 51(15) nm,b=0.522 54(8) nm, c=1.448 3(2) nm,β=90.119(3)°, V=0.736 7(2) nm3, Z=2, Dc=1.690 g/cm3, μ =1.362 mm-1, F(000) =388, R1=0.031 6, wR2=0.090 2. A total of 4 771 reflections were collected, of which 1 700 reflections were independent and 1 489 were observed. The structure was solved with direct method and refined with full matrix least squares method. The X ray structure analysis reveals that the crystal structure is two dimensional sheet structure through intermolecular hydrogen bonding and π π stacking.