Notes. Synthesis and characterization of monocyclopentadienyl niobium derivatives. X-Ray crystal structure of di-µ-chloro-µ-oxo-bis[dichloro(η-trimethylsilylcyclo-pentadienyl)niobium(<scp>V</scp>)], [{Nb(η-C<sub>5</sub>H<sub>4</sub>SiMe<sub>3</sub>)Cl<sub>2</sub>}<sub>2</sub>(µ-O)(µ-Cl)<sub>2</sub>]
作者:Ana María Andreu、Félix A. Jalón、Antonio Otero、Pascual Royo、Anna M. Manotti Lanfredi、Antonio Tiripicchio
DOI:10.1039/dt9870000953
日期:——
[Nb(η-C5H4R)Cl4][R = H (1) or SiMe3(2)] are easily hydrolysed to give [Nb(η-C5H4R)Cl2}2(µ-O)-(µ-Cl)2][R = H (3) or SiMe3(4)] and finally [Nb(η-C5H4R)Cl3(OH2)}2(µ-O)][R = H (5) or SiMe3(6)]. The reduction of (1) and (2) with sodium amalgam in the presence of ligands allows isolation of [Nb(η-C5H4R)Cl3L2] and [Nb(η-C5H4R)Cl2(CO)L2](R = H or SiMe3; L2= 2PMe3,2PMe2Ph, or Ph2PCH2CH2PPh2) which have been
[铌(η-C 5 H ^ 4 R)氯4 ] [R = H(1)或森达3(2)]下容易水解,得到[铌(η-C 5 H ^ 4 R)氯2 } 2( μ-O) - (μ-Cl)的2 ] [R = H(3)或森达3(4)],最后[铌(η-C 5 H ^ 4 R)氯3(OH 2)} 2(μ -O)] [R = H(5)或SiMe 3(6)]。(1)和(2),在配体存在钠汞齐允许[铌(η-C的隔离5 ħ 4 R)氯3大号2 ]和[Nb的(η-C 5 H ^ 4 R)氯2(CO)L- 2 ](R = H或森达3:L 2 = 2PMe 3,2PMe 2 PH,或pH 2 PCH 2 CH 2 PPH 2已特点是磁测量和红外光谱和核磁共振光谱)。已确定(4)的晶体结构:单斜晶系,空间群P 2 1 / n其中a = 26.805(7),b = 7.310(2),c = 13.400(3)Å,β= 91.42(2)°和Z