Synthesis, structure, and reactivity of niobocene imido complexes containing alkynyl ligands.: X-ray crystal structure of [Nb(=NPh) (η5-C5H4SiMe3)2(C≡CPh)]

被引:9
作者
Antiñolo, A
Fajardo, M
López-Mardomingo, C
López-Solera, I
Otero, A
Pérez, Y
Prashar, S
机构
[1] Univ Castilla La Mancha, Fac Quim, Dept Quim Inorgan Organ & Bioquim, E-13071 Ciudad Real, Spain
[2] Univ Rey Juan Carlos, ESCET, Dept Ciencias Expt & Ingn, Madrid 28933, Spain
[3] Univ Alcala de Henares, Dept Quim Organ, Madrid 28871, Spain
关键词
D O I
10.1021/om010064y
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
The following alkynyl niobocene imido complexes have been prepared: [Nb(=NBut)(eta (C5H5)-C-5)(2)(C drop CR)] (R = Me (1), SiMe3 (2), Bu-t (3), CH2Ph (4)), [Nb(=NC6H4Me-4)(eta (5)-C5H5)(2)(C drop CR)] (R = SiMe3 (5), Bu-t (6)), [Nb(=NBut)(eta (5)-C5H4SiMe3)(2)(C drop CR)(3) (R = SiMe3 (7), Bu-t (8)), [Nb(=NPh)(eta (5)-C5H4SiMe3)(2)(C drop CR)(3) (R = Ph (9), Bu-t (10)), [Nb(=NC6H4Me-4)(eta (5)-C5H4SiMe3)(2)(C drop CR)] (R = SiMe3 (11), Bu-t (12)), [Nb(=NC6H4OMe-4)(eta (5)-C5H4SiMe3)(2)(C drop CR)] (R = SiMe3 (13), Bu-t (14)), and [Nb(=NBut)(Me2Si(eta (5)-C5H4)(2))(C-CR)] (R = SiMe3 (15), Bu-t (16)). The synthetic path involved the reaction of either BrMg(C drop CR) or Mg(C drop CR)(2) with the metallocene imido complex Nb(=NR ')(Cp)(2)Cl, Cp = eta (5)-cyclopentadienyl. The molecular structure of 9 has been determined by single-crystal X-ray diffraction studies. Protonation of 2 by CF3COOH and 9 by HBF4 gave the cationic amide species [Nb(NHBut)(eta (5)-C5H5)(2)(C drop CSiMe3)](+) (17) and [Nb(NHPh)(eta (5)-C5H4SiMe3)(2)(C drop CPh)](+) (18), respectively.
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页码:3132 / 3138
页数:7
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