Synthesis and crystal structures of bis-[1-oxopyridin-2-olato(1-)]bis-(penta-fluoro-phen-yl)silicon(IV)-tetra-hydro-furan-pentane (2/1/1), bis-[1-oxopyridin-2-olato(1-)]bis-(p-tol-yl)silicon(IV), and dimesitylbis[1-oxopyridin-2-olato(1-)]silicon(IV)

双-[1-氧代吡啶-2-醇(1-)]双-(五氟苯基)硅(IV)-四氢呋喃-戊烷(2/1/1)、双-[1-氧代吡啶-2-醇(1-)]双-(对甲苯基)硅(IV)和二甲基双[1-氧代吡啶-2-醇(1-)]硅(IV)的合成和晶体结构

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Abstract

The neutral organosilicon(IV) complex, (C(6)F(5))(2)Si(OPO)(2) (OPO = 1-oxopyridin-2-one, C(5)H(4)NO(2)), was synthesized from (C(6)F(5))(2)Si(OCH(3))(2) and 2 equiv. of 1-hy-droxy-pyridin-2-one in tetra-hydro-furan (THF). Single crystals grown from the diffusion of n-pentane into a THF solution were identified as a THF hemisolvate and an n-pentane hemisolvate, (C(6)F(5))(2)Si(OPO)(2)·0.5THF·0.5C(5)H(12) (1). p-Tol-yl(2)Si(OPO)(2) (2) and mesit-yl(2)Si(OPO)(2) (3) crystallized directly from reaction mixtures of 2 equiv. of Me(3)Si(OPO) with p-tol-yl(2)SiCl(2) and mesit-yl(2)SiCl(2), respectively, in aceto-nitrile. The oxygen-bonded carbon and nitro-gen atoms of the OPO ligands in 1, 2, and 3 were modeled as disordered indicating co-crystallization of up to three possible diastereomers in each. Solution NMR studies support the presence of exclusively the all-cis isomer in 1 and multiple isomers in 2. Poor solubility of 3 limited its characterization in solution.

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