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Relevant academic research and scientific papers

Synthesis of single and double butterfly iron carbonyl complexes by reactions of [(μ-RSe)(μ-CO)Fe2(CO)6]- anions. Crystal structures of (μ-p-MeC6H4Se)[μ-PhCH2N(H)C=S]Fe 2(CO)6 and [(μ-PhSe)(μ-MeAs)Fe2(CO)6]2

The in situ reactions of the [Et3NH]+ and [MgBr]+ salts of [(μ-RSe)(μ-CO)Fe2(CO)6]- (1) anions with PhC(Cl)=NPh gave single butterfly complexes (μ-RSe)(μ-PhC=NPh)Fe2(CO)6 (2, R=Ph; 3, R=p-MeC6H4; 4, R=Et), whereas those of the [Et3NH]+ salts of 1 with R′N=C=S afforded single butterfly complexes (μ-RSe)[μ-R′N(H)C=S]Fe2(CO)6 (5, R=Ph, R′=Ph; 6, R=p-MeC6H4 R′=Ph; 7, R=p-MeC6H4, R′=PhCO; 8, R=p-MeC6H4, R′=PhCH2). Compound 8 could also be prepared by reaction of the [MgBr]+ salt of 1 (R=p-MeC6H4) with PhCH2NCS followed by treatment with CF3CO2H. More interestingly, while the [Et3NH]+ salt of 1 (R=Ph) reacted with Et3OBF4 to give a carbyne ligand-bridged single butterfly complex (μ-PhSe)(μ-EtOC)Fe2(CO)6 (9), reaction of the [Et3NH]+ salt of 1 (R=Ph) with MeAsI2 produced a MeAs-AsMe ligand-bridged double butterfly complex [(μ-PhSe)(μ-MeAs)Fe2(CO)6]2 (10). All the new complexes, 2-10, were characterized by elemental analysis and various spectroscopic methods, for complexes 8 and 10, the structures were also confirmed by X-ray diffraction techniques.

Remarkable reactions of cationic carbyne complexes of manganese and rhenium with diiron anions [Fe2(μ-CO)(μ-SeR)(CO)6]-. A route to RSe-bridged dimetal bridging carbene complexes

The reactions of cationic carbyne complexes of manganese and rhenium, [η-C5H5(CO)2M≡CC6 H5]BBr4 (1, M = Mn; 2, M = Re), with diiron anionic compounds [Et3NH][Fe2(μ-CO) (μ-SeR)(CO)6] (3, R = C6H5; 4, R = p-CH3C6H4) in THF at low temperature gave the dimetal bridging carbene complexes [MFe{μ-C(SeR)C6H5} (CO)5(η-C5H5)] (10, M = Mn, R = C6H5); 11, M = Mn, R = p-CH3C6H4; 13, M = Re, R = C6H5; 14, M = Re, R = (p-CH3C6H4), [η-C5H5M(CO)3] (7, M = Mn; 12, M = Re), and [Fe2(μ-SeR)2(CO)6] (8, R = C6H5; 9, R = p-CH3C6H4). Complexes 1 and 2 also react with [MgBr][Fe2(μ-CO) (μ-SeC2H5)(CO)6] (5) to produce [Fe2(μ-SeC2H5)2(CO)6] (15) and dimetal bridging carbene complexes [MnFe{μ-C(SeC2H5)C6H5} (CO)5(η-C5H5)] (17) and [ReFe{μ-C(SeC2H5)C6H5} (CO)5(η-C5H5)] (18), respectively. 2 reacts similarly with [MgBr][Fe2(μ-CO)(μ-SeC4H9-n) (CO)6] (6) to give [Fe2(μ-SeC4H9-n)2(CO)6 ] (16) and a Re-Fe bridging carbene complex [ReFe{μ-C(SeC4H9-n)C6H5}(CO) 5(η-C5H5)] (19), while the analogous reaction of 1 with 6 produced an unexpected trimetal bridging carbyne complex [MnFe2(μ-H)(μ-CO)2(μ3 -CC6H5(CO)6) (η-C5H5)] (20). The structures of complexes 9, 10, 13, 18, and 20 have been established by X-ray diffraction studies.

Synthesis of doubly-bridged Fe/Se and Fe/Te complexes via reactions of the [MgX]+ salts of anions [(μ-RE)(μ-CO)Fe2(CO)6]- (E=Se,Te).: Crystal structure of (μ-p-MeC6H4Te)(μ-PhC=NPh)Fe2(CO) 6

The reactions of Grignard reagents RMgX with elemental Se or Te in THF, followed by treatment of the intermediates RSeMgX or RTeMgX with Fe3(CO)12 at room temperature (r.t.), were found to give [MgX]+ salts of anions [(μ-RSe)(μ-CO)Fe2(CO)6]- (2) and [(μ-RTe)(μ-CO)Fe2(CO)6]- (3), respectively. Furthermore, the [MgX]+ salts of anions 2 (R=Et) reacted in situ with the electrophile Ph2AsCl to afford (μ-EtSe)(μ-Ph2As)Fe2(CO)6 (4), whereas the [MgX]+ salts (R=p-MeC6H4) reacted with the electrophile PhNCS, followed by treatment with another electrophile MeI to give (μ-p-MeC6H4Se)(μ-PhN(Me)C=S)Fe2(CO) 6 (5). Similarly, the [MgX]+ salts of anions 3 (R=Et, t-Bu, i-Bu) were found to react sequentially with the electrophiles PhCCPh and CF3COOH to yield (μ-RTe)(μ-σ,π-PhC=CHPh)Fe2(CO)6 (6a, R=Et; 6b, R=t-Bu; 6c, R=i-Bu), whereas reactions of the [MgX]+ salts of anions 3 (R=Et, Ph, p-MeC6H4) with the electrophiles Ph2AsCl or PhC(Cl)NPh produced (μ-RTe)(μ-Ph2As)Fe2(CO)6 (7a, R=Et; 7b, R=p-MeC6H4) and (μ-RTe)(μ-PhC=NPh)Fe2(CO)6 (8a, R=a(axial)-Ph; 8b, R=e(equatorial)-Ph; 9a, R=a-p-MeC6H4; 9b, R=e-p-MeC6H4), respectively. The reaction courses for the formation of Fe/Se and Fe/Te complexes 4-9 were discussed briefly and the structures of these new complexes, along with two other new Fe/Te complexes (μ-RTe)2Fe2(CO)6 (R=Et, i-Bu), were characterized by elemental analysis and spectroscopy, as well as for complex 9b, whose structure was confirmed further by X-ray diffraction analysis.