Synthesis and Structure of Cluster Monomer Fe2(CO)6(μ-SCH2CHCH2)(μ3-S)Fe(CO)2(η5-C5H5)

Konchenko, Sergey N.; Максаков, В. А.; Filippov, I. Yu.; Вировец, А. В.; Podberezskaya, N. V.

doi:10.1070/mc1992v002n04abeh000189

Mendeleev Communications

1992

DOI: 10.1070/mc1992v002n04abeh000189

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Synthesis and Structure of Cluster Monomer Fe2(CO)6(μ-SCH2CHCH2)(μ3-S)Fe(CO)2(η5-C5H5)

Sergey N. Konchenko

В. А. Максаков

I. Yu. Filippov

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“…4 The IR spectrum of 2b in the carbonyl region almost repeats the spectrum of 2a. The main difference is a small shift of the absorption bands to lower frequencies ( Table I).…”

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Synthesis of clusters Fe2(CO)6(μ-XCH2CH=CH2)(μ3-X)Fe(CO)2Cp (X = Se, S; Cp = η5-C5H5)

et al. 1997

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The clusters Fe?(CO)6(g-XCH2CH=CH2)(~t3-X)Fe(CO)2Cp (X = S, Se) were prepared by the successive treatment of the bi-and trimetallic complexes Fe2(CO)6(u-Se2) and Fe3(CO)gQa3-X) with allylmagnesium chloride and CpFe(CO)2t. The clusters obtained contain a noncoordinated C=C bond. The structure of the Se-containing cluster was suggested on the basis of comparison of its spectral data (IR, tH NMR, and M6ssbauer spectra) with the spectra of the analogous S-containing complex, which was previously characterized by X-ray diffraction analysis.Key words: carbonyl clusters, cluster monomers, iron, sulfur, selenium, synthesis.Interest in cluster compounds of transition metals containing ligands with free olefin substituents is caused by the possibility of their copolymerization with traditional organic monomers. 1 This method for preparing metal-immobilized polymeric materials has been previously used for a series of Os3(CO)x2 derivatives z obtained by the coordination of unsaturated ligands on clusters containing the Os3-metallocycle. 3 Recently, we have suggested another approach to preparing "cluster monomers" (Scheme I). 4In this case, along with the addition of an unsaturated radical to the coordinated ligand, the skeleton of a new cluster is formed during the synthesis, which makes it possible to vary. the composition and structure of the obtained compounds more extensively. In terms of this approach, one may plan the development of "homologous" series of clusters. For this purpose, complexes containing not only S, but Se and Te as well, and at the second stage of the synthesis, electrophilic complexes of The present work is devoted to applying this synthetic approach to Se-containing iron carbonyl derivatives.

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“…4 The IR spectrum of 2b in the carbonyl region almost repeats the spectrum of 2a. The main difference is a small shift of the absorption bands to lower frequencies ( Table I).…”

mentioning

confidence: 82%

“…3 Recently, we have suggested another approach to preparing "cluster monomers" (Scheme I). 4 In this case, along with the addition of an unsaturated radical to the coordinated ligand, the skeleton of a new cluster is formed during the synthesis, which makes it possible to vary. the composition and structure of the obtained compounds more extensively.…”

mentioning

confidence: 99%

Synthesis of clusters Fe2(CO)6(μ-XCH2CH=CH2)(μ3-X)Fe(CO)2Cp (X = Se, S; Cp = η5-C5H5)

et al. 1997

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Organoiron chemistry. Annual survey for the year 1992

Kerber

1994

Journal of Organometallic Chemistry

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Organometallic Selenolates. 5.¹ Synthesis and Complexing Properties of 2-Propene- and 2-Methyl-2-propeneselenolato Molybdenum and Tungsten Compounds. Crystal Structures of cp(CO)₃WSeCH₂C(CH₃)CH₂, [cp(CO)₂MoSeCH₂C(CH₃)CH₂]₂, [cp(CO)₃Mo(μ-SeCH₂C(CH₃)CH₂)W(CO)₅], [cp(CO)₃Mo(μ-SeCH₂C(CH₃)CH₂)Mo(CO)_5<

1997

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2-Propene- and 2-methyl-2-propeneselenolato complexes of molybdenum(II) and tungsten(II) have been prepared via insertion of gray selenium into alkali-metal-molybdenum and -tungsten bonds and subsequent reaction with allyl and beta-methallyl chlorides. The complexes are monomeric in the solid state. The (beta-methallyl)molybdenum compound cp(CO)(3)MoSeCH(2)C(CH(3))=CH(2) (2) decomposes slowly in solution with CO loss and formation of the corresponding dimer [cp(CO)(2)MoSeCH(2)C(CH(3))=CH(2)](2) (3), whose crystal structure has been determined (C(22)H(24)Mo(2)O(4)Se(2), monoclinic, P2(1)/c, a = 11.151(2) Å, b = 13.436(3) Å, c = 16.872(3) Å, beta = 102.42(2) degrees, Z = 4). A monomeric structure has been found for cp(CO)(3)WSeCH(2)C(CH(3))=CH(2) (5) (C(12)H(12)O(3)SeW, triclinic, P&onemacr;, a = 7.592(3) Å, b = 7.700(3) Å, c = 12.296(5) Å, alpha = 98.31(4) degrees, beta = 104.24(2) degrees, gamma = 108.49(3) degrees, Z = 2). Additionally, the complexing properties of the selenolato complexes have been investigated. The reactions of the molybdenum complexes cp(CO)(3)MoSeCH(2)CH=CH(2) (1) and (2) with the metal(0)-carbonyl complexes W(CO)(5)(THF), (CH(3)CN)(3)Mo(CO)(3), and (eta(6)-C(7)H(8))Mo(CO)(3) (C(7)H(8) = cycloheptatriene) led to the formation of [cp(CO)(3)Mo(&mgr;-SeCH(2)C(CH(3))=CH(2))M(CO)(5)] (M = W (6), Mo (7)) and [cp(CO)(3)Mo(&mgr;-SeCH(2)CH=CH(2))Mo(CO)(5)] (8), respectively. 6 and 7 are isostructural and crystallize in the monoclinic space group P2(1)/n (6, C(17)H(12)MoO(8)SeW, a = 14.708(2) Å, b = 9.837(2) Å, c = 14.958(2) Å, beta = 103.030(10) degrees, Z = 4; 7, C(17)H(12)Mo(2)O(8)Se, a = 14.712(2) Å, b = 9.8670(10) Å, c = 14.982(2) Å, beta = 103.100(10) degrees, Z = 4), whereas [cp(CO)(3)Mo(&mgr;-SeCH(2)CH=CH(2))Mo(CO)(5)] (8) crystallizes in the noncentrosymmetric orthorhombic space group Pna2(1) (C(16)H(10)Mo(2)O(8)Se, a = 18.638(4) Å, b = 9.707(2) Å, c = 11.169(3) Å, Z = 4). Furthermore, (77)Se-NMR spectra displayed chemical shifts consistent with earlier results on related complexes.

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Synthesis and Structure of Cluster Monomer Fe2(CO)6(μ-SCH2CHCH2)(μ3-S)Fe(CO)2(η5-C5H5)

Cited by 3 publications

References 3 publications

Synthesis of clusters Fe2(CO)6(μ-XCH2CH=CH2)(μ3-X)Fe(CO)2Cp (X = Se, S; Cp = η5-C5H5)

Synthesis of clusters Fe2(CO)6(μ-XCH2CH=CH2)(μ3-X)Fe(CO)2Cp (X = Se, S; Cp = η5-C5H5)

Organoiron chemistry. Annual survey for the year 1992

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Synthesis and Structure of Cluster Monomer Fe2(CO)6(μ-SCH2CHCH2)(μ3-S)Fe(CO)2(η5-C5H5)

Cited by 3 publications

References 3 publications

Synthesis of clusters Fe2(CO)6(μ-XCH2CH=CH2)(μ3-X)Fe(CO)2Cp (X = Se, S; Cp = η5-C5H5)

Synthesis of clusters Fe2(CO)6(μ-XCH2CH=CH2)(μ3-X)Fe(CO)2Cp (X = Se, S; Cp = η5-C5H5)

Organoiron chemistry. Annual survey for the year 1992

Organometallic Selenolates. 5.1 Synthesis and Complexing Properties of 2-Propene- and 2-Methyl-2-propeneselenolato Molybdenum and Tungsten Compounds. Crystal Structures of cp(CO)3WSeCH2C(CH3)CH2, [cp(CO)2MoSeCH2C(CH3)CH2]2, [cp(CO)3Mo(μ-SeCH2C(CH3)CH2)W(CO)5], [cp(CO)3Mo(μ-SeCH2C(CH3)CH2)Mo(CO)5<

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