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Relevant academic research and scientific papers

Facile synthesis of σ,μ-iminoacyl bridged butterfly clusters (μ-RE)(σ,μ-ArC=NAr′)Fe2(CO)6 (E=S, Se)

The reactive anionic salts [Et3NH][(μ-RE)(μ-CO)Fe2(CO)6] (1) (RE=PhS, PhSe) reacted with N-arylbenzimidoyl chloride Ph(Cl)C=NAr′ (2) (Ar=Ph, 4-MeC6H4, 4-C6H4) in THF to give butterfly σ,μ-iminoacyl bridged hexacarbonyldiiron clusters (μ-RE)(σ,μ-PhC=NAr′)Fe2(CO)6 (3a-e) in moderate yields. The structure of the new clusters was characterized by elemental analyses, IR and 1H-NMR spectroscopy. X-ray diffraction confirmed the crystal structure of (μ-PhSe)(σ,μ-PhC=NPh)Fe2(CO)6 (3a). It crystallizes in the triclinic space group P1 (no. 2) with a=11.224(3), b=13.542(4), c=8.9559(2) A, α=102.32(2), β=91.95(2), γ=70.20(2)°, V=1250.1(6) A3, Z=2 and Dcalc=1.636 g cm-3.

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.

Reaction of [μ-RE(μ-CO)Fe2(CO)6]- (E = S, Se) with N2CHCO2Me. Synthesis and characterisation of (μ-RE)[μ-η2-N=NCH(R′)CO2Me]Fe 2(CO)6 and (μ-PhSe)[μ-η1<

Reaction of [M][(μ-RE)(μ-CO)Fe2(CO)6] (E = S, Se; M = Et3NH, Na) with N2CHCO2Me give the intermediate [M][(μ-RE)(μ-N2CHCO2Me)Fe2(CO) 6] (II). Action of II with counterion Et

Chemical reactivity of [(μ-RSe) (μ-S) {Fe2(CO)6}2(μ4-S)]-: Synthesis and characterization of (μ-RSe) (μ-R'S) {Fe2(CO)6}2(μ4-S) and (μ3-S)2

The reaction Of (μ-S2)Fe2(CO)6 with [(μ-RSe) (μ-CO)Fe2(CO)6]- gives the anionic complexes [(μ-RSe) (μ-S){Fe2(CO)6}2(μ4-S)]- (1). Reactions of 1 w

Reaction of [Et3NH][(μ-RE)(μ-CO)Fe2(CO)6] (E=S, Se) with azides. Synthesis of (μ-RE)(μ-p-R1C6H4N3H)Fe 2(CO)6 and crystal structure of (μ-ButS)(μ-PhN3H)Fe2(CO)6

The reaction of [Et3NH][(μ-RE)(μ-CO)Fe2(CO)6] (E=S, Se) (1) with aryl azides gives bridging triazenido complexes (μ-RE)(μ-p-R1C6H4N3H)Fe 2(CO)6 (2-8) (2, RE=ButS, R1=H; 3, RE=PhS, R1=H; 4, RE=ButS, R1=Cl; 5, RE=ButS, R1=MeO; 6, RE=PhS, R1=MeO; 7, RE=PhSe, R1=H; 8, RE=PhSe, R1=Cl). These complexes were characterized by elemental analyses and 1H-NMR and IR spectroscopy. The structure of complex 2, established by single-crystal X-ray diffraction analysis, shows that the triazenido ligand binds to two iron centers in a bridging bidentate fashion.

Novel reaction of complex salts [(μ-RE)(μ-CO)Fe2(CO)6][HNEt3] (E = S, Se) with Phosphaalkene t-Bu(Me3SiO)C=PSiMe3. Synthesis and spectroscopic and crystallographic characterization of butterfly Fe2EP clusters (μ-RE)[μ-t-Bu(Me3SiO)CHPH]Fe2(CO)6 (E = S, Se)

Reaction of complex salts [(μ-RE)(μ-CC))Fe2(CO)6][HNEt3] (1, E = S, Se) with phosphaalkene t-Bu(Me3SiO)C=PSiMe3 (2) has been found to afford a series of new butterfly-shaped Fe2-EP clusters of type [(μ-RE)[μ-t-Bu(Me3SiO)CHPH]Fe2(CO)6 (3, RE = EtS; 4, n-PrS; 5, n-BuS; 6, t-BuS; 7, PhSe; 8, p-MeC6H4Se) in quite high yields. This type of cluster may exist as three isomers, namely, e(R)e(H), e(R)a(H), and a(R)a(H), which differ in whether the R group and H atom are attached to E and P atoms with an axial or an equatorial bond. Clusters 3-8 have been characterized by elemental analysis and 1H, 31P, and 77Se NMR spectroscopy, as well as for isomers 3e(R)a(H), 6e(R)a(H), 8e(R)e(H), and 8a(R)a(H) by single-crystal X-ray diffraction analyses. In addition, a possible reaction mechanism has been preliminarily suggested.

Unexpected reactions of anionic intermediates [(μ-RE)(μ-S=CS)Fe2(CO)6]- with so2Cl2. Synthesis and characterization of novel dithioformato-bridged double clusters [(μ-RE)Fe2(CO)6]2(μ-S=CS-μ) (E = S, Se)

The dithioformato-bridged anionic salts [Et3NH][(μ-RE)(μ-S=CS)Fe2(CO)6], generated from CO-bridged anionic complexes [Et3NH][μ-RE)(μ-CO)Fe2(CO)6] and carbon disulfide, reacted in situ with SC2Cl2 in THF to afford a series of novel dithioformato-bridged double clusters [(μ-RE)Fe2(CO)6]2(μ-S=CS-μ) (3a-e) (3a, RE = EtS; 3b, n-PrS; 3c, t-BuS; 3d, PhSe; 3e, p-MeCe6H4Se). A single-crystal diffraction analysis of 3c was undertaken and has confirmed the proposed structure.

Formation of (μμ-RE)(μ-S-)Fe2(CO)6 and (μ-RE)(μ-Se-)Fe2(CO)6 (E = S, Se) anions and a comparative study of their reactions with SO2Cl2, ClC(O)ZC(O)Cl (Z = (CH2)2, C6H4), or P-MeC6H4SO2Cl.

The CO-bridged anions [(μ-RE)(μ-CO)Fe2(CO)6]- reacted with S8 to form the sulfur-centered anions (μ-RE)(μ-S-)Fe2(CO)6 (4; E = S, Se), whereas reaction of the anions with Se8 yielded the selenium-centered anions (μ-RE)(μ-Se-)Fe2(CO)6 (6; E = S, Se). Interestingly, reaction of 4 with SO2Cl2 afforded the S - S-bonded clusters [(μ-RE)Fe2(CO)6]2(μ-S-S) (5), whereas reaction of 6 with SO2Cl2 produced the μ4-Se clusters [(μ-RE)Fe2(CO)6]2(μ4-Se) (8); clusters 8 could also be produced by the action of anions 6 on succinoyl chloride or p-phthaloyl chloride, while the μ4-8 clusters [(μ-RE)Fe2(CO6]2(μ4-S) (9) were generated by reaction of anions 4 with the above organic bis acid chlorides under similar conditions. Also, reaction of 4 (E = S) with p-MeC6H4SO2Cl gave the μ4-S clusters [(μ-RE)Fe2(CO)6]2(μ4-S) (9; E = S) and the expected Fe2S2 butterfly clusters (μ-RE)(μ-p-MeC6H4SO2S)Fe 2(CO)6 (10), whereas anion 6 reacted with p-MeC6H4SO2Cl to afford the unexpected S=O-bridged complexes (μ-RE)(μ-p-MeC6H4SO2)Fe 2(CO)6 (11) and μ4-Se clusters 8. Clusters 11 could be also prepared through direct reaction of the precursor of 6, i.e. [(μ-RE)(μ-CO)Fe2(CO)6]-, with p-MeC6H4SO2Cl. For some of these reactions the mechanisms were preliminarily proposed. The structures of 15 new cluster compounds have been characterized by C/H analysis and IR, 1H NMR, and MS spectroscopy; those of [(μ-EtS)Fe2(CO)6]2(μ4-Se) (8a) and (μ-EtS)(μ-p-MeC6H4SO2)Fe 2(CO)6 (11a) have been confirmed by X-ray diffraction analyses.

Reactions of [Et3NH][(μ-RE)(μ-CO)Fe2(CO)6] (E = S, Se) salts with sulfur(I) chloride and with carbon disulfide. Crystal structure of the (μ-PhSe) (μ-PhCH2SC=S)Fe2(CO)6 complex

The salts of [Et3NH][(μ-RE)(μ-CO)Fe2(CO)6] (1) react with S2Cl2 to give double-cluster complexes [(μ-RE)Fe2(CO)6]2(μ-S-S-μ) (2a-f) (2a, RE = EtS; 2b, PhS; 2c, n-BuS; 2d, t-BuS; 2e, PhSe; 2f, p-CH3C6H4Se), whereas the salt of [Et3NH][(μ-PhSe)(μ-CO)Fe2(CO)6] reacts with CS2 followed by treatment with diverse organic halides to afford single-cluster complexes (μ-PhSe)(μ-ZSC=S)Fe2(CO)6 (3a-c) (3a, Z = PhCH2; 3b, PhCOCH2; 3c, EtO2CCH2), double-cluster complexes [(μ-PhSe)Fe2(CO)6]2(1,3-(μ-S=C-SCH 2)2C6H4] (3d) and [(μ-PhSe)Fe2(CO)6]2-[1,4-(μ-S=C-SCH 2)2C6H4] (3e), and triple-cluster complex [(μ-PhSe)Fe2(CO)6]3[1,3,5-(μ-S=C-SCH 2)3C6H3] (3f). The crystal structure of 3a was determined by X-ray diffraction techniques.