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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

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Figshare2016-02-22 更新2026-04-29 收录
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https://figshare.com/articles/dataset/Reactions_of_an_Iron_Chlorodistannane_with_Hydroxide_Isolation_and_Structural_Characterization_of_sup_5_sup_Me_sub_3_sub_SiC_sub_5_sub_H_sub_4_sub_Fe_CO_Sn_sup_t_sup_Bu_sub_2_sub_sub_2_sub_OH_DMAP_DMAP_4_i_N_i_i_N_i_Dimethylamino_pyridine_a_OH_Stannyl_sta/2561947
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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.
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2016-02-22
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