1291079-00-9Relevant academic research and scientific papers
Lewis base character of the phosphorus atom in phosphanido-niobocene complexes. Synthesis of new early-early homo- and heterobimetallic entities
Reguillo-Carmona,Antinolo,Garcia-Yuste,Lopez-Solera,Otero
, p. 2622 - 2630 (2011/05/04)
The reaction of phosphanido complexes [Nb(η5-C 5H4SiMe3)2(L)(PPh2)] [L = CO (1), CNXylyl (2)] with early transition metal halides in high oxidation states has been carried out. New bimetallic niobocene complexes [{Nb(η5-C5H4SiMe3) 2(L)}(μ-PPh2)(MCl5)] [M = Nb, L = CO (3), L = CNXylyl (4); M = Ta, L = CO (5), L = CNXylyl (6)] have been successfully synthesized by the reaction with [MCl5]2 (M = Nb or Ta). In a similar way [{Nb(η5-C5H4SiMe 3)2(L)}(μ-PPh2)(MCl4)] [M = Ti, L = CO (13), CNXylyl (14); M = Zr, L = CO (15), CNXylyl (16)] were synthesized using MCl4 (M = Ti or Zr). Solutions of complexes 4-6 in chloroform produced new ionic derivatives [Nb(η5-C5H 4SiMe3)2(P(H)Ph2)(L)] [MCl 6] [M = Nb, L = CO (7), L = CNXylyl (8); M = Ta, L = CO (9), L = CNXylyl (10)]. Ionic complexes [Nb(η5-C5H 4SiMe3)2(P(Cl)Ph2)(L)] [NbCl 4O(thf)] [L = CO (11), CNXylyl (12)] were formed from solutions in thf - rapidly in the case of 3 but more slowly for 4. New heterometallic complexes [Nb(η5-C5H4SiMe3) 2(L)(μ-PPh2){(Ti(η5-C5R 5)Cl3}] [R = H, L = CO (17), CNXylyl (18); R = CH 3, L = CO (19), CNXylyl (20)] were synthesized by the reaction of 1 or 2 with [Ti(η5-C5R5)Cl3] (R = H or CH3). All of these compounds were characterized by IR and multinuclear NMR spectroscopy, and the molecular structures of 9 and 12 were determined by single-crystal X-ray diffraction.
