双(二叔丁基苯基膦)二卤化Pt(Ⅱ)配合物的合成及结构测试

Synthesis and structure test of bis(di-tert-butylphenylphosphine)platinum(Ⅱ)dihalide complexes

采用铂替代钯合成了以二叔丁基苯基膦[(t-Bu)_(2)PPh]和卤素(Cl、Br)为配体的Pt(Ⅱ)配合物。以氯化铂(PtCl_(2))和溴化铂(PtBr_(2))为起始原料,二甲亚砜(DMSO)为溶剂,在氮气保护下与二叔丁基苯基膦反应,得到目标化合物。结果表明,Pt[(t-Bu)_(2)PPh]_(2)Cl_(2)产率为96.9%,Pt[(t-Bu)_(2)PPh]_(2)Br_(2)产率为94.1%,2种化合物的纯度均大于99%。通过元素分析、核磁共振(1H-NMR)分析和单晶X射线衍射(XRD)分析测定了目标化合物的化学结构,结果显示,配合物均为trans-四配位的平面正方形配合物,Pt(Ⅱ)处于配位平面的中心,分别与2个Cl或者Br和P键合,形成4配位的平面四边形的结构,2个卤素原子和膦配体处于反位。

Two new platinum complexes,Pt[(t-Bu)_(2)PPh]_(2)X_(2)(X=Cl,Br)were synthesized using platinum chloride(PtCl_(2)),platinum bromide(PtBr_(2))and di-tert-butyl phenyl phosphine as starting materials,dimethyl sulfoxide(DMSO)as a solvent under nitrogen protection.Their structures were characterized by MS,NMR and X-ray single-crystal diffraction analysis.The results showed that the yield of Pt[(t-Bu)_(2)PPh]_(2)Cl_(2)was 96.9%,and that the yield of Pt[(t-Bu)_(2)PPh]_(2)Br_(2)was 94%.The purity of the two compounds was greater than 99%.The structure analysis results showed that the complexes were all trans-four-coordinated planar square complexes where Pt(Ⅱ)locates in the center of the coordination plane,bonds with 2 Cl or Br and P respectively,and 2 halogen atoms and the phosphine ligand are in the anti-position.