Unprecedented Calcium Metalla-macrocycle Having Phosphinoselenoic Amide and Diphenylphosphinate in the Coordination Sphere
作者:Kishor Naktode、Jayeeta Bhattacharjee、Sayak Das Gupta、Hari Pada Nayek、Bhabani S. Mallik、Tarun K. Panda
DOI:10.1002/zaac.201300492
日期:2014.4
2P(Se)N(Ar)}Ph2P(O)O}(THF)2]2 (2) (Ar = 2, 6-dimethylphenyl) can be isolated with a good yield by the reaction of neutral phosphinoselenoic amide [Ph2P(Se)NH(Ar)] (1) and calcium bis(trimethylsilyl)amides [CaN(SiMe3)2} 2(THF)2] in toluene followed by crystallization in air. The homoleptic calcium phosphinoselenoic amido complex of the composition [CaPh2P(Se)N(Ar)}2(THF)2] (3) can also be obtained
组成 [CaPh 2P(Se)N(Ar)}Ph2P(O)O}(THF)2]2 (2) (Ar = 2, 6-二甲基苯基) 的八元钙金属大环可以通过中性膦基硒酸酰胺 [Ph2P(Se)NH(Ar)] (1) 和双(三甲基甲硅烷基)酰胺钙 [CaN(SiMe3)2} 2(THF)2] 在甲苯中的反应,以良好的收率分离然后在空气中结晶。组成[CaPh2P(Se)N(Ar)}2(THF)2](3)的均配钙磷酰硒酰氨基络合物也可以通过两种合成途径获得。在第一条路线中,[CaN(SiMe 3)2}2(THF)2] 在环境温度下用膦亚硒酰胺 [Ph2P(Se)NH(Ar)] (1) 处理,然后在惰性气氛以提供高纯度的配合物 3。在第二条路线中,进行一锅反应,涉及 1、二碘化钙、CaI2、和双(三甲基甲硅烷基)酰胺钾 [KN(SiMe3)2}] 在惰性气氛中的甲苯中。当配合物3在THF中用二苯