Synthesis of bimetallic complexes via 4-stanna-tetrahydro-s-indacenesстатьяИсследовательская статья
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Аннотация:4-Stanna-8-silatetrahydro-4,4,8,8-tetramethyl-s-indacene reacts with CpTiC13 and CpZrCl3*2THF in toluene (ratio 1:l) to give monotransmetallated products CpMCl2(h5-C5H4SiMe2C5H4SnMe2Cl (M = Ti (5), Zr (6)) in high yields. These compounds can be transformed into heteronuclear complexes of type LnMCp-SiMe2-CpM'L'm (MLn = TiCl2Cp, M'L'm = Rh(COD), 10; MLn = ZrCl2Cp, M'L'm = Rh(COD), 11; MLn = ZrCl2Cp, M'L'm = TiCl2Cp, 12; MLn = ZrCl2Cp, M'L'm = ZrCl2Cp*, 13) in reactions with [Rh(COD)Cl]2, CpTiCl3, and Cp*ZrCl3, respectively. Compound 4 and its heteroanalog 4-stannatetrahydro-4,4,8,8-tetramethyl-s-indacene (14) react with CpTiCl3 (ratio 1:2) and (Cl3TiCp)22SiMe2 (16) (ratio 1:1) to give the corresponding monobridged [CpTiCl2(h5-C5H4)]2XMe2 X = C (15), Si (8)) and doubly-bridged (h5:h5-C5H4SiMe2C5H4)(h5:h5-C5H4XMe2C5H4)(TiCl2)2 (X = C(17), Si (18)) Ti(IV) derivatives. They may be reduced by powdered zinc in toluene to the corresponding Ti(III) complexes, [CpTiCl(h5-C5H4)]2XMe2 (X = C (20), Si (21)) and (h5:h5-C5H4SiMe2C5H4)(h5:h5-C5H4XMe2C5H4)(TiCl)2 (X = C (22), Si (23)). Crystals of 23 are monoclinic, space group P2(1)/a with unit cell dimensions a = 16.033 (3) A, b = 18.859 (4) A, c = 7.997 (2) A, gamma = 96.82 (2), and Z = 4.