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- W2012114516 abstract "The chloro(alkyl)metallocenes[MR*(Cl)(η-C 5H 5) 2][R* = -CH(SiMe 3)C 6H 4Me-o; M = Zr 1 or Hf 2] have beenprepared from[MCl 2(η-C 5H 5) 2] andLiR*(tmen)(tmen = N,N,N′,N′-tetramethylethane-1,2-diamine); further alkylationoccurred only for M = Zr, affording rac-3a andmeso-3b,[ZrR* 2(η-C 5H 5) 2]. Incontrast, reaction of 2 equivalents ofLi[CH(SiMe 3) 2](tmen) with[ZrCl 2(η-C 5H 5) 2] yieldedan alkyl elimination product possessingµ-η 1∶η 5-C 5H 4 2- ligands. Compound 1 was reversiblyreduced(E 1/2 red = -1.72 Vvs. saturated calomel electrode, SCE) whereas 2, 3a or 3b wereirreversibly reduced(E red = -2.12,-2.08, -2.00 V respectively vs. SCE). Thermolysisof 3b in toluene gave 3a (80 °C) or‘Zr(C 10H 8)’ (120 °C).Photolysis of 3a or 3b at 20 °C in tetrahydrofuran(thf) yielded a 1∶1 mixture of 3a and 3b; a d 1intermediate has been unambiguously identified as[ZrR*(η-C 5H 5) 2]. Reduction of 1(Na–Hg), or 3a and 3b (Na[C 10H 8]), in thfalso gave [ZrR*(η-C 5H 5) 2] but thisslowly transformed into[ZrR*(η-C 5H 5) 2(thf)], and 1with Na[C 10H 8] and PPh 3 gave[ZrR*(η-C 5H 5) 2(PPh 3)].Reduction of 1, 3a or 3b, or photolysis of 3a or 3b, in the presence ofPMe 3 gave[ZrR*(η-C 5H 5) 2(PMe 3)].Crystal structure determinations showed a slightly more crowded metalenvironment in 2 than in 1, consistent with the view that dialkylationin 2 is limited on steric grounds; M–σ-C 2.359(4) (1),2.322(8) (2), metal–centroid 2.22 (1), 2.21 (2), M–Cl2.444(1) (1), 2.418(3) (2) A. The structure of 3a confirms therac assignment, M–σ-C 2.37 4 A,metal–centroid 2.23, 2.24 A." @default.
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- W2012114516 title "C-Centred chiral metal alkyls, [MR*(Cl)(η-C5H5)2], rac- and meso-[ZrR*2(η-C5H5 )2] [R* = CH(SiMe3)C6H4 Me-o], and their one-electron reductions; reaction of Li[CH(SiMe3)2](Me2NCH2CH 2NMe2) with [MCl2(η-C5H5)2] (M = Zr or Hf )" @default.
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- W2012114516 doi "https://doi.org/10.1039/a701586k" @default.
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