Publikation: Di-, Tri-, and Tetranuclear Cyclobutenylidene Complexes
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Pentacarbonyl(dimethylvinylidene)chromium, [(CO)5Cr=C=CMe2] (1), reacts with the butadiynyl complexes [Cp(CO)2FeC≡CC≡CR] [2; R = SiMe3 (a), nBu (b), Ph (c)] and [Cp(CO)(PPh3)FeC≡CC≡CSiMe3] (3a) by regiospecific cycloaddition of the Cα≡Cβ bond of the butadiynyl complexes to the C=C bond of 1 to form the 1,3-heterobinuclear cyclobutenylidene complexes 4a–c and 5a with an alkynyl substituent at C-2 of the bridging ring. Desilylation of the 2-C≡CSiMe3 substituent in 4a and 5a with tetrabutylammonium fluoride affords the 2-C≡CH-substituted complexes 6 and 7. Complex 4a reacts with HNMe2 and HN(CH2)5 by substitution of NR2 for the 3-Fe(CO)2Cp fragment to form the corresponding 3-aminocyclobutenylidene complexes 10 and 11. Sequential reactions of 4a with [nBu4N]F and nBu3SnNEt2 give the trinuclear 2-C≡CSnnBu3-substituted complex 12. Coupling of 12 with C6H4I2-p yields the 2-C≡CC6H4I-p-substituted complex 13. Coupling of 7 with C6H4I2-p yields a mixture of the mono-coupling product 14 and the tetranuclear C≡C–C6H4–C≡C-bridged bis(cyclobutenylidene) complex 15. Coupling of 7 with trans-[(Et3P)2MCl2] in the presence of CuI/[Pd(PPh3)4] gives the trinuclear 2-C≡C–M(PEt3)2X-substituted complexes 16 (M = Pd, × = I) and 17 (M = Pt, × = Cl). The spectroscopic data as well as the results of the X-ray-structural analysis of 5a indicate strong electronic communication between the metal centers. In the solid state, 5a exhibits a “butterfly” conformation.
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LEROUX, Frédéric, Rüdiger STUMPF, Helmut FISCHER, 1998. Di-, Tri-, and Tetranuclear Cyclobutenylidene Complexes. In: European Journal of Inorganic Chemistry. 1998, 1998(9), pp. 1225-1234. ISSN 1434-1948. eISSN 1099-0682. Available under: doi: 10.1002/(SICI)1099-0682(199809)1998:9<1225::AID-EJIC1225>3.0.CO;2-BBibTex
@article{Leroux1998Tetra-23045, year={1998}, doi={10.1002/(SICI)1099-0682(199809)1998:9<1225::AID-EJIC1225>3.0.CO;2-B}, title={Di-, Tri-, and Tetranuclear Cyclobutenylidene Complexes}, number={9}, volume={1998}, issn={1434-1948}, journal={European Journal of Inorganic Chemistry}, pages={1225--1234}, author={Leroux, Frédéric and Stumpf, Rüdiger and Fischer, Helmut} }
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