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• W2022231330 endingPage "1774" @default.
• W2022231330 startingPage "1765" @default.
• W2022231330 abstract "TaCl5 reacts with two equivalents of lithium 2,6-di-t-butylphenoxide in benzene to give [TaCl3(2,6-di-t-butylphenoxide)2] (1) in 70% yield and with three equivalents of the lithium phenoxide in diethyl ether to give [TaCl2(2,6-di-t-butylphenoxide)3] (2) which can also be prepared by reaction of (1) with one equivalent of the lithium phenoxide. Three equivalents of lithium 2,6-di-isopropylphenoxide react with TaCl5 to give [TaCl2(diethylether)(2,6-di-isopropylphenoxide)3] (4) which, on attempted recrystallization in the presence of air, gave [Ta2Cl(μ-Cl)2(2,6-di-isopropylphenoxide)5(μ-O)] (5). Complexes (1), (2), and (4) were characterized by elemental analysis, IR, and 1H and 13C NMR spectra. Coordination of the phenoxide ligand in (2) is accompanied by downfield shifts of the phenyl ring ipso, ortho and para carbon resonances of 9.6, 3.6 and 3.1 ppm respectively, compared with the free ligand. For complex (4) the relative shifts are 5.9, 6.1 and 2.9 ppm. The structures of (2) and (5) have been determined by single-crystal X-ray diffraction methods. Crystals of (2) are monoclinic, space group P21/c with a = 18.902(6) Å, b = 10.815(8) Å, c = 20.259(4) Å and β = 92.62(2)°; crystals of (5) are monoclinic, space group P21/c with a = 11.174(1) Å, b = 20.402(4) Å, c = 27.143(3) Å and β = 94.58(1)°. Both structures were solved by Patterson and Fourier methods and refined to R values of 0.063 for the 1690 observed data for (2) and 0.062 for the 3693 observed data for (5). Complex (2) is monomeric with a square pyramidal coordination geometry about Ta. Observed distances are: TaOaxial 1.83(2) Å; TaObasal each 1.90(2) Å; TaClbasal each 1.37(1) Å. Complex (5) is binuclear with a distorted octahedral geometry about each tantalum atom. The structure consists essentially of TaCl2(2,6-di-isopropylphenoxide)3 and TaCl2(O)(2,6-di-isopropylphenoxide)2 units bridged through the oxygen and Cl atoms. Observed distances are TaObridge 1.69(1) and 2.10(1) Å; TaClbridge 2.498(7), 2.396(8), 2.634(7) and 2.781(7) Å; TaClterminal 2.309(8) Å. The TaOphenoxide distances range from 1.77(2) to 2.19(2) Å. In both (2) and (5) the phenyl rings are orientated such as to minimise interactions between the 2- and 6-substituents. In both molecules electron counts are maximized using π-electron density from the terminal ligands." @default.
• W2022231330 created "2016-06-24" @default.
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• W2022231330 date "1987-01-01" @default.
• W2022231330 modified "2023-10-16" @default.
• W2022231330 title "Sterically congested tris phenoxide complexes of tantalum(V). The x-ray crystal structures of [TaCl2(2,6-di-t-Butylphenoxide)3] and [Ta2Cl(μ-Cl)2(2,6-di-isopropylphenoxide)5(μ-O)]" @default.
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• W2022231330 doi "https://doi.org/10.1016/s0277-5387(00)86548-1" @default.
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