Structural and two-dimensional phosphorus-31 nuclear magnetic resonance studies of derivatives from (RP)<sub>5</sub>(R = Et or Ph) and activated triosmium clusters [Os<sub>3</sub>(CO)<sub>10</sub>X<sub>2</sub>](X =µ-H or NCMe)
作者:How-Ghee Ang、Siau-Gek Ang、Qi Zhang
DOI:10.1039/dt9960002773
日期:——
The reaction of the cyclophosphane (EtP)(5) with the activated triosmium cluster [Os-3(mu-H)(2)(CO)(10)] at 80 degrees C gave [Os-3(mu-H)(CO)(8)(mu-eta(3)-P(5)Et(5)H)] 1 and [Os-3(CO)(10)1,3-(PEt)(5)}] 2. The compound (PhP)(5) reacted with [Os-3(mu-H)(2)(CO)(10)] at room temperature to give [Os-3(mu-H)(CO)(8)(mu-eta(3)-P(5)Ph(5)H)] 3. Treatment of (EtP)(5) with [Os-3(CO)(10)(NCMe)(2)] at room temperature afforded [Os-3(CO)(10)1,2-(PEt)(5)}] 4, while the reaction at 80 degrees C yielded only 2. All the reaction products have been characterized by elemental analysis and IR, H-1 and P-31 NMR spectroscopy. The solid-state structures of compounds 1, 2 and 4 established by single-crystal X-ray diffraction showed that the phosphorus ring in ! has undergone one P-P bond cleavage while those in 2 and 3 are intact. The solution structure of 3 has been fully characterized by two-dimensional P-31 NMR spectroscopy.