作者:T.S.Andy Hor、Pauline M.N. Low、Yaw Kai Yan、Ling-Kang Liu、Yuh-Sheng Wen
DOI:10.1016/0022-328x(93)80077-o
日期:1993.4
of [Re(CO)5]− by a molar equivalent of PPh2Cl at ca. −70°C yielded three dinuclear complexes, Re2(μ-Cl)(μ-PPh2)(CO)8 (1), Re2(CO)9(PPh2H) (2) and Re2(μ-H)(μ-PPh2)(CO)8 (3), as major products. When PPh2Cl was present in two-fold excess, only 2 and ReCl(CO)4(PPh2H) (4) were isolated. All the complexes were characterized by IR and NMR (1H and 31P) spectroscopy. The crystal structures of 2 and 4 were determined
[Re(CO)5 ] -的摩尔等效当量PPh 2 Cl于大约20分钟被氧化。-70℃下产生了三种双核配合物中,Re 2(μ-Cl)的(μ-PPH 2)(CO)8(1)中,Re 2(CO)9(PPH 2 H)(2)和R e 2(μ- H)(μ-PPH 2)(CO)8(3),作为主要产品。当PPh 2 Cl的含量过量两倍时,只有2和ReCl(CO)4(PPh 2 H)(4)被隔离。通过IR和NMR(1 H和31 P)光谱对所有配合物进行表征。通过单晶X射线衍射分析确定2和4的晶体结构。晶体数据:ReCl(CO)4(PPh 2 H),空间群P 2 1 / c,a = 11.358(1),b = 10.365(1),c = 14.765(3)Å,β= 96.07(1) °,1891年观测的最终R = 0.022;Re 2(CO)9(PPh 2 H),空间群P 2 1 /a,a = 12.709(1),b