Butatriene-hexacarbonyldiiron complexes via dehydroxylation of unsaturated diols by Fe(CO)1

Victor, Rae

doi:10.1016/s0022-328x(00)84209-6

Cited by 22 publications

(7 citation statements)

References 7 publications

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“…The neutral Fe(CO) 3 analogues of the Co(CO) 3 + cationic clusters can be prepared directly from cobalt precursors. Thus, as depicted in Scheme , treatment of (propargyl alcohol)Co 2 (CO) 6 with Fe(CO) 5 in refluxing acetone yields (HCCCH 2 )FeCo(CO) 6 ( 23 ); this same reaction is also applicable to the diol (HOCH 2 C⋮CCH 2 OH)Co 2 (CO) 6 , which, upon treatment with Fe(CO) 5 in acetone, gives (CH 2 CCCH 2 )Fe 2 (CO) 6 ( 24 ) 4 Isolobal Replacement of Co(CO) 3 Vertices by Fe(CO) 3 Fragments …”

Section: Resultsmentioning

confidence: 93%

“…(Me 3 SiC  C  C 9 H 8 )FeCo(CO) 6 (22). By analogy to the procedure previously described for (MeCCCH 2 )FeCo(CO) 6 , freshly distilled Fe(CO) 5 (2.19 g, 11.18 mmol) was added to a solution of 9 (0.784 g, 1.39 mmol) dissolved in acetone (35 mL), and the mixture was heated under reflux for 24 h. After removal of solvent, the residue was subjected to flash chromatography on silica gel. Elution with hexanes gave light red crystals of 22 (96 mg, 0.018 mmol, 13%), mp 300 °C dec. 1 H NMR (500 MHz, CD 2 Cl 2 ): δ 7.98 (H 5 ) § , 7.81 (H 8 ) § , 7.75 (H 4 ) ⧫ , 7.69 (H 1 ) ⧫ , 7.48 (H 7 ) § , 7.37 (H 2 ) ⧫ , 7.32 (H 6 ) § , 7.24 (H 3 ) ⧫ .…”

Section: Methodsmentioning

confidence: 99%

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Metal Cluster Stabilized Fluorenyl, Indenyl, and Cyclopentadienyl Antiaromatic Cations: An NMR and X-ray Crystallographic Study

et al. 1999

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Treatment of fluorenone, 2,3-diphenylindenone, tetraphenylcyclopentadienone, or 2,5-diethyl-3,4-diphenylcyclopentadienone with ((trimethylsilyl)ethynyl)lithium gives, after hydrolysis, the analogous alkynol; subsequent addition of dicobalt carbonyl and then fluoroboric acid yields the corresponding fluorenyl, indenyl, or cyclopentadienyl cation stabilized by complexation to a tricarbonylcobalt moiety. Variable-temperature NMR data on these cluster cations, and on their bis(diphenylphosphino)methane derivatives, reveal that the barrier to migration of the cationic center between cobalt cluster vertices increases in the order fluorenyl < indenyl < cyclopentadienyl and suggest that the cations with more antiaromatic character have the greatest need for charge delocalization onto the metal center. Replacement of a Co(CO)3 cationic fragment by an Fe(CO)3 unit yields the mixed-metal species [((fluorenyl)CCSiMe3)FeCo(CO)6] (22) and [((2,3-diphenylindenyl)CCSiMe3)FeCo(CO)6] (27). In these structural models for the cationic complexes, the Fe−C(9) distance in 22 is 2.626(11) Å, while in the indenyl system 27 the Fe−C(1) distance is 2.347(7) Å, again indicating that the 8π indenyl cation interacts more strongly with the metal center than does the 12π fluorenyl cation.

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Section: Resultsmentioning

confidence: 93%

Section: Methodsmentioning

confidence: 99%

Metal Cluster Stabilized Fluorenyl, Indenyl, and Cyclopentadienyl Antiaromatic Cations: An NMR and X-ray Crystallographic Study

et al. 1999

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“…spectrum. We believe that this coloured species is the carbocation ( 5 ) which is brightly coloured like other phenyl-substituted carbocations. A small rotation of the Ph2C3 ligand would allow the positive charge to be localised at the metal atoms as in (6) but then the cluster is unsaturated and nucleophilic addition of water would give (4).…”

Section: Resultsmentioning

confidence: 88%

Acid-induced lsomerisations of osmium and ruthenium clusters involving hydroxide transfer from carbon to metal atoms. X-Ray crystal structure of nonacarbonyl-µ₃-(3,3-diphenylallene- 1,1-diyl)-µ-hydrido-µ-hydroxo-triosmium(2 Os–Os)

Aime¹,

Deeming²,

Hursthouse³

et al. 1982

J. Chem. Soc., Dalton Trans.

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The complexes [M3H(CO)9(p3-C-CCPh20H)] (M = Ru or 0s) were prepared by reaction of [M3(C0)&J with HOCPh2C-CCPh20H in saturated hydrocarbon at 130 "C for M = 0 s or in refluxing cyclohexane from M = Ru. In the latter case the yield of cluster is low and there is some 1 ,I ,4,4-tetraphenylbutadiene formed. Treatment of the trinuclear clusters in chloroform with trifluoroacetic acid leads to isomerisation with migration of the OH group from carbon to metal atoms. This was confirmed by an X-ray structure determination for the osmium productThe crystals are monoclinic, space group P2,, a = 10.569( 1), b = 20.259(3), c = 12.287(2) A, p = 95.66(1)", and 2 = 4. The structure was refined to R = 0.0621 for 4 11 2 observed reflections. There are two independent molecules (A and B) in the'unit cell with very closely similar structures. Spectroscopically, an OH group was identified and another hydrogen bound to osmium but neither hydrogen atom was located by X-ray diffraction. The OH group bridges two non-bonded osmium atoms separated by 3.374(5) A in molecule A [3.372(5) A in B], while the p-H was deduced to be across the longer 0s-0s bond [2.905(5) versus 2.861 (5) A for molecule A and 2.902(5) versus 2.869( 5) A for molecule B]. The 3,3-diphenylallene-I ,1 -diyl ligand is bonded through two 0s-C CT bonds and a 1,2-q2-co-ordination to the other osmium atom and is bent about the central atom [145(3)" for molecule A and 144(3)' for B]. The orientation of the phenyl substituents at the non-co-ordinated allene carbon atom agrees with this interpretation of the bonding.We have been interested in introducing hydroxy-or aminosubstituted alkynes into triruthenium and triosmium clusters

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“…In this paper, we stated that we were reporting a novel synthesis for (butatriene)hexacarbonyldiiron complexes 1 from 2-butyne-1,4-diols 2 and enneacarbonyldiiron. We are sorry to say that we failed to notice an article by Victor in our literature searches. Victor reported the synthesis of 1 from 2 and dodecacarbonyltriiron.…”

Section: Volume 15mentioning

confidence: 96%

Novel Synthesis of (Butatriene)hexacarbonyldiiron Complexes. Stereochemical Aspects and an X-ray Crystal Structure Determination.

Eigemann¹,

Förtsch²,

Hampel³

et al. 1996

Organometallics

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Butatriene-hexacarbonyldiiron complexes via dehydroxylation of unsaturated diols by Fe(CO)1

Cited by 22 publications

References 7 publications

Metal Cluster Stabilized Fluorenyl, Indenyl, and Cyclopentadienyl Antiaromatic Cations: An NMR and X-ray Crystallographic Study

Metal Cluster Stabilized Fluorenyl, Indenyl, and Cyclopentadienyl Antiaromatic Cations: An NMR and X-ray Crystallographic Study

Acid-induced lsomerisations of osmium and ruthenium clusters involving hydroxide transfer from carbon to metal atoms. X-Ray crystal structure of nonacarbonyl-µ₃-(3,3-diphenylallene- 1,1-diyl)-µ-hydrido-µ-hydroxo-triosmium(2 Os–Os)

Novel Synthesis of (Butatriene)hexacarbonyldiiron Complexes. Stereochemical Aspects and an X-ray Crystal Structure Determination.

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Butatriene-hexacarbonyldiiron complexes via dehydroxylation of unsaturated diols by Fe(CO)1

Cited by 22 publications

References 7 publications

Metal Cluster Stabilized Fluorenyl, Indenyl, and Cyclopentadienyl Antiaromatic Cations: An NMR and X-ray Crystallographic Study

Metal Cluster Stabilized Fluorenyl, Indenyl, and Cyclopentadienyl Antiaromatic Cations: An NMR and X-ray Crystallographic Study

Acid-induced lsomerisations of osmium and ruthenium clusters involving hydroxide transfer from carbon to metal atoms. X-Ray crystal structure of nonacarbonyl-µ3-(3,3-diphenylallene- 1,1-diyl)-µ-hydrido-µ-hydroxo-triosmium(2 Os–Os)

Novel Synthesis of (Butatriene)hexacarbonyldiiron Complexes. Stereochemical Aspects and an X-ray Crystal Structure Determination.

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Acid-induced lsomerisations of osmium and ruthenium clusters involving hydroxide transfer from carbon to metal atoms. X-Ray crystal structure of nonacarbonyl-µ₃-(3,3-diphenylallene- 1,1-diyl)-µ-hydrido-µ-hydroxo-triosmium(2 Os–Os)