Reactions of an iron chlorodistannane with hydroxide: Isolation and structural characterization of {(η~5-Me_3SiC _5H_4)Fe(CO)[(SntBu_2) _2(μ-OH)]···DMAP}, DMAP = 4-(N, N -dimethylamino)pyridine, a μ-OH-stannyl(stannylene)-iron complex

摘要

Reacting the silylated ferrate [(η_5-Me_3SiC _5H_4)Fe(CO)_2]~-Li~+, obtained from the reaction of [(η~5-C_5H _5)Fe(CO)_2SiMe_3], FpSiMe_3, and LDA with ClSn~tBu_2Sn~tBu_2Cl, we have synthesized the distannane (η~5-Me_3SiC _5H_4)Fe(CO)_2-SntBu_2Sn tBu_2Cl, _5, together with (η~5-Me _3SiC_5H_4)Fe(CO)_2-Sn tBu_2Cl, 6. Photochemical irradiation of 5 resulted in formation of [(η~5-Me_3SiC_5H _4)Fe(CO)(Sn~tBu_2)_2(μ-Cl)], 8, which we have characterized spectroscopically. Treatment of 8 with Bu _4N~+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_3SiC_5H_4)Fe(CO)(Sn ~tBu_2)_2(μ-OH-DMAP)] (11). The crystal structure of 11 is reported together with those of 5, 6, (η~5- Me_3SiC_5H_4)Fe(CO)_2Sn ~tBu_2OH, 15, and the unusual product (η~5- Me_3SiC_5H_4)Fe(CO)_2-Sn tBu_2-(η~5-Me_3SiC _5H_3)-Fe(CO)2Sn~tBu_Cl, 7, obtained from the reaction between FpSiMe_3 and a large excess of LDA after quenching with ~tBu_2SnCl_2.