铅(Ⅱ)与三(2-(6-甲基吡啶基)甲基)胺配合物的合成及晶体结构的研究

SYNTHESIS AND CRYSTAL STRUCTURE OF THE COMPLEX OF LEAD(Ⅱ) WITH TRIS(2 (6 METHYLPYRIDYL) METHYL) AMINE

本文合成了标题配合物［Ｐｂ（ＴＬＡ）·ＮＯ３］·ＮＯ３（ＴＬＡ＝三（２－（６－甲基吡啶基）甲基）胺，对其红外光谱及晶体结构进行了研究。结果表明，晶体属单斜晶系，Ｐ２１／ｎ空间群，晶胞参数如下：ａ＝１０．２３４（２），ｂ＝１５．３４７（３），ｃ＝１５．３９５（３），β＝９９．９３（２）°，Ｖ＝２３８２（２）３，Ｚ＝４，ＤＣ＝１．８５ｋｇ／ｍ３。晶体采用直接方法和Ｆｏｕｒｉｅｒ合成解出，经全矩陈最小二乘法对原子参数进行结构修正，最后的偏差因子Ｒ＝０．０４３，ＲＷ＝０．０５４。单晶结构表明：中心铅离子是处于四方单锥配位环境，由三（２－（６－甲基吡啶基）甲基）胺的四个氮原子和一个硝酸根的氧原子形成了五配位的几何构型。

The new complex [Pb(TLA)NO 3]NO 3(TLA=tris(2 (6 methylpyridyl)methyl)amine)has been synthesized and characterized. Its cyrstal structure has been determined by X ray diffraction method. The crystal is monoclinic system, and P 2 1/ n space group. The crystal cell parameters are found to be a =10.234(2), b =15.347(3), c =15.395(3), β =99.93(2)°, V =2382(2) 3,Z=4, D C=1.85 kg/m 3. The structure was solved by directed methods and Fouries syntheses. Final refinement by full matrix least squares methods carried out. Convergence resulted in final unweighted and weighted agreement factors of 0.043 and 0.054. The Pb(Ⅱ) ion lies in a distorted square pyramid environment composed of three N pyridyl and N amine from TLA ligand and one oxygen atom from nitrate group.