Reactions of an Iron Chlorodistannane with Hydroxide: Isolation and Structural Characterization of {(η⁵-Me₃SiC₅H₄)Fe(CO)[(Sn^tBu₂)₂(μ-OH)]···DMAP}, DMAP = 4-(N,N-Dimethylamino)pyridine, a μ-OH-Stannyl(stannylene)–Iron Complex

Abstract

Reacting the silylated ferrate [(η 5 -Me 3 SiC 5 H 4 )Fe(CO) 2 ] − Li + , obtained from the reaction of [(η 5 -C 5 H 5 )Fe(CO) 2 SiMe 3 ], FpSiMe 3 , and LDA with ClSn t Bu 2 Sn t Bu 2 Cl, we have synthesized the distannane (η 5 -Me 3 SiC 5 H 4 )Fe-(CO) 2 -Sn t Bu 2 Sn t Bu 2 Cl, 5, together with (η 5 -Me 3 SiC 5 H 4 )Fe(CO) 2 -Sn t Bu 2 Cl, 6. Photochemical irradiation of 5 resulted in formation of [(η 5 -Me 3 SiC 5 H 4 )Fe(CO)-(Sn t Bu 2 ) 2 (μ-Cl)], 8, which we have characterized spectroscopically. Treatment of 8 with Bu 4 N + 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, [(η 5 -Me 3 SiC 5 H 4 )Fe(CO)(Sn t Bu 2 ) 2 -(μ-OH-DMAP)] (11). The crystal structure of 11 is reported together with those of 5, 6, (η 5 -Me 3 SiC 5 H 4 )Fe(CO) 2 Sn t Bu 2 OH, 15, and the unusual product (η 5 -Me 3 SiC 5 H 4 )Fe(CO) 2 -Sn t Bu 2 -(η 5 -Me 3 SiC 5 H 3 )-Fe(CO) 2 Sn t Bu 2 Cl, 7, obtained from the reaction between FpSiMe 3 and a large excess of LDA after quenching with t Bu 2 SnCl 2 .