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• W2014996990 abstract "The niobium complex [{Nb(η5-C5H4SiMe3)2Cl}2] 1 reacted with phenyl isocyanate, 1,3- and 1,4-phenylenediisocyanate to give the corresponding complexes [Nb(η5-C5H4SiMe3)2Cl(κ2N,C-OCNPh)] 2, [{Nb(η5-C5H4SiMe3)2Cl}2{κ2N,C-µ-1,3-(OCN)2C6H4}] 3 and [{Nb(η5-C5H4SiMe3)2Cl}2{κ2N,C-µ-1,4-(OCN)2C6H4}] 4, respectively. The spectroscopic data were not sufficient unequivocally to differentiate between the presence of a κ2C,N or κ2C,O co-ordination mode. However the crystal structure of 2 showed it to have κ2C,N co-ordination. Complexes 3 and 4 have an analogous structure in which two metal centres are linked through an aryl ring containing a diisocyanate ligand. The reactivity of these complexes under reduction and thermal decomposition conditions was examined. Complexes 2–4 with Na/Hg underwent a reduction at each metal centre followed by protonation to afford the corresponding [Nb(η5-C5H4SiMe3)2(OCHNPh)] 5, [{Nb(η5-C5H4SiMe3)2}2{µ-1,3-(OCHN)2C6H4}] 6 and [{Nb(η5-C5H4SiMe3)2}2{µ-1,4-(OCHN)2C6H4}] 7. The imido [Nb(η5-C5H4SiMe3)2Cl(NPh)] 8 and diimido derivatives [{Nb(η5-C5H4SiMe3)2Cl}2(µ-1,3-N2C6H4)] 9 and [{Nb(η5-C5H4SiMe3)2Cl}2(µ-1,4-N2C6H4)] 10 were isolated by heating 2, 3 or 4 or alternatively by treating 1 with the appropriate amount of the corresponding aniline, 1,3- or 1,4-phenylenediamine, respectively. The molecular crystal structure of 9 was determined by single-crystal diffractometry. It contains two bent niobocene units linked by a 1,3-diimidophenylene ligand, with the niobium atoms slightly deviating from the plane formed by this ligand. Complexes 8–10 reacted with Grignard reagents MgRCl (R = Me, Et or Pri) or MgMe2 in tetrahydrofuran solution to give the corresponding substitution products [Nb(η5-C5H4SiMe3)2R(NPh)] (R = Me 11, Et 12 or Pri 13), [{Nb(η5-C5H4SiMe3)2R}2(µ-1,3-N2C6H4)] (R = Me 14, Et 15 or Pri 16) and [{Nb(η5-C5H4SiMe3)2R}2(µ-1,4-N2C6H4)] (R = Me 17, Et 18 or Pri 19). The reaction of 8–10 with Na/Hg in appropriate molar ratios afforded the corresponding hydride complexes [Nb(η5-C5H4SiMe3)2H(NPh)] 20, [{Nb(η5-C5H4SiMe3)2H}2(µ-1,3-N2C6H4)] 21 and [{Nb(η5-C5H4SiMe3)2H}2(µ-1,4-N2C6H4)] 22. Finally, the monoimido complexes 8 and 11–13 were easily protonated with 1 equivalent of HBF4·OEt2 to give, in one step, the corresponding amido cationic complexes [Nb(η5-C5H4SiMe3)2X(NHPh)]+ [BF4]– (X = Cl 23, Me 24, Et 25 or Pri 26). The structures of the different families of complexes isolated were determined by spectroscopic methods." @default.
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• W2014996990 title "Synthesis and structural characterization of isocyanate, amido and imido niobocene derivatives: crystal structures of [Nb(η5-C5H4SiMe3)2Cl(κ2N,C-OCNPh] and [{Nb(η5-C5H4SiMe3)2Cl}2(μ-1,3-N2C6H4)] †" @default.
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• W2014996990 doi "https://doi.org/10.1039/a705352e" @default.
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