Reactions of an Iron Chlorodistannane with Hydroxide: Isolation and Structural Characterization of {(η5-Me3SiC5H4)Fe(CO)[(SntBu2)2(μ-OH)]···DMAP}, DMAP = 4-(N,N-Dimethylamino)pyridine, a μ-OH-Stannyl(stannylene)–Iron Complex

Abstract

Reacting the silylated ferrate [(η5-Me3SiC5H4)Fe(CO)2]−Li+, obtained from the reaction of [(η5-C5H5)Fe(CO)2SiMe3], FpSiMe3, and LDA with ClSntBu2SntBu2Cl, we have synthesized the distannane (η5-Me3SiC5H4)Fe(CO)2-SntBu2SntBu2Cl, 5, together with (η5-Me3SiC5H4)Fe(CO)2-SntBu2Cl, 6. Photochemical irradiation of 5 resulted in formation of [(η5-Me3SiC5H4)Fe(CO)(SntBu2)2(μ-Cl)], 8, which we have characterized spectroscopically. Treatment of 8 with Bu4N+OH– led to the formation of the μ-hydroxyl-stannyl(stannylene) complex, which could be further stabilized, via a H-bonding interaction, with 4-(N,N-dimethylamino)pyridine, DMAP, [(η5-Me3SiC5H4)Fe(CO)(SntBu2)2(μ-OH-DMAP)] (11). The crystal structure of 11 is reported together with those of 5, 6, (η5-Me3SiC5H4)Fe(CO)2SntBu2OH, 15, and the unusual product (η5-Me3SiC5H4)Fe(CO)2-SntBu2-(η5-Me3SiC5H3)-Fe(CO)2SntBu2Cl, 7, obtained from the reaction between FpSiMe3 and a large excess of LDA after quenching with tBu2SnCl2.