NDLI: Synthesis of the triply-bonded dimolybdenum anions [Mo2(η5-C5H5)2(μ-PA2)(μ-CO)2]− (A = Cy, Et, Ph, OEt): unsaturated hydride and carbyne derivatives

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Synthesis of the triply-bonded dimolybdenum anions [Mo₂(η⁵-C₅H₅)₂(μ-PA₂)(μ-CO)₂]⁻ (A = Cy, Et, Ph, OEt): unsaturated hydride and carbyne derivatives

Content Provider	Royal Society of Chemistry (RSC)
Author	Ramos, Alberto Ruiz, Miguel A. Melón, Sonia García, M. Esther
Copyright Year	2009
Abstract	Tetrahydrofuran solutions of the 30-electron anions [Mo2Cp2(μ-PA2)(μ-CO)2]− (A = Cy, Et, Ph, OEt) are conveniently prepared through a two-step approach. In the first step, [Mo2Cp2(CO)6] is treated with the chlorophosphines ClPR2 (R = Cy, Et, Ph) or the chlorophosphite ClP(OEt)2, in refluxing toluene or diglyme respectively, to give the corresponding 32-electron chloro-complexes [Mo2Cp2(μ-Cl)(μ-PA2)(CO)2] as major products. In the second step, these air-sensitive intermediates are treated in tetrahydrofuran solution at room temperature with one of several reducing agents such as Li[BHEt3], Li(Hg), Na(Hg) or K[BHsBu3] to give red solutions of the corresponding alkali-metal salts of the anions, which display significant ion pairing involving one or both oxygen atoms of the bridging carbonyl ligands, depending on the cation. All these triply bonded species are quite air-sensitive and could not be isolated as pure solids, but they can be easily protonated using a weak acid such as [NH4]PF6 to give with good yield the corresponding unsaturated hydrides [Mo2Cp2(μ-H)(μ-PA2)(CO)2], which are species of low to moderate sensitiveness to air, and also formally containing an intermetallic triple bond. The reactivity of the dicyclohexylphosphide-bridged anion (mainly as its Li+ salt) towards different hydrocarbon halides RX was studied in detail. These reactions were found to be rather complex, critically depending on the reagent used, and generally resulting in the formation of several products, of which four types were identified: (a) the known agostic products [Mo2Cp2(μ-PCy2)(μ-R)(CO)2] (R = Me, CH2Ph), (b) the new alkoxycarbyne products [Mo2Cp2(μ-COR)(μ-PCy2)(μ-CO)] [R = Me, Et, C(O)Ph, iPr, Cy], which could be conveniently isolated as pure solids, (c) the iodoxycarbyne complex [Mo2Cp2(μ-COI)(μ-PCy2)(μ-CO)], a very unstable species formed in the reaction with EtI, and (d) the halide complexes [Mo2Cp2(μ-PCy2)(μ-X)(CO)2] [X = Cl, Br, I], which were more conveniently prepared by the direct reaction of the anion with the pertinent halogen (X = Br, I). The analysis of the above results suggests that at least three primary reaction pathways are in operation: (a) nucleophilic attack of the anion through its dimetal centre, (b) nucleophilic attack of the anion through the oxygen atoms of its bridging carbonyls and (c) electron-transfer with the reagent, this being the main path to the halo-complexes [Mo2Cp2(μ-PCy2)(μ-X)(CO)2].
Starting Page	8171
Ending Page	8182
Page Count	12
File Format	HTM / HTML PDF
ISSN	14779226
Volume Number	0
Issue Number	39
Journal	Dalton Transactions
DOI	10.1039/b909493h
Language	English
Publisher	Royal Society of Chemistry
Access Restriction	Open
Subject Keyword	Li Tetrahydrofuran Toluene Diglyme Ion Nucleophile Metal carbonyl Carboxylic acid Intermetallic Triple bond Alkane Reagent Halide Halogen
Content Type	Text
Resource Type	Article
Subject	Inorganic Chemistry

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Fulvalene titanium and zirconium complexes: synthesis and NMR study of phosphanido-, alkyl-, and alkynyl-derivatives. X-ray crystal structures of [{Ti(η5−C5H5)(μ−PPH2)}2{μ−(η5−C5H4−η5−C5H4)}] and [{Zr(η5−C5H5)(μ−C≡CSiMe3)}2{μ−(η5−C5H4−η5−C5H4)}]

Synthesis and Characterization of Hydride−Alkynyl, Allenylidene, Carbyne, and Functionalized-Alkynyl Complexes Containing the [Os(η5-C5H5)(PiPr3)2]+Fragment: The Complex [Os(η5-C5H5)(CCCPh2)(PiPr3)2]PF6, a New Type of Allenylidene Derivative from the Reactivity Point of View

Detection of σ-alkane complexes of manganese by NMR and IR spectroscopy in solution: (η5-C5H5)Mn(CO)2(ethane) and (η5-C5H5)Mn(CO)2(isopentane)

Application of electron-transfer chain catalysis: preparation of bridged 〚{(η5-C5H5)Fe(CO)2}2(μ-diphosphine)2+〛 complexes without chelated 〚(η5-C5H5)Fe(CO)(η2-diphosphine)+〛 byproducts

Reactivity of the dinuclear fulvalene cyclopentadienyl zirconium cationic species [{Zr(η5-C5H5)}2(μ-CH2)(μ-Cl)(μ-η5-C5H4-η5-C5H4)]+ with isocyanides and carbon monoxide: insertion reactions, spectroscopic characterization and synthetic aspects

Tetracarbonylbis(η5-cyclopentadienyl)bis[(dec-9-en-1-yl)diphenylphosphine]dimolybdenum(0)(Mo--Mo) tetrahydrofuran disolvate

Linking of Main Group Metals via Bridging Halide Ligands: Structures of the Bromo-indanediyl Dimer [{(η5-C5H5)Fe(CO)2}2InBr]2 and the Related Lithium Bromide Adduct [(η5-C5H5)Fe(CO)2]2In(μ-Br)2Li(OEt2)2

Lewis acid promoted terminal-to-bridge carbonyl shift in [(π-C₅H₅)Ru(CO)₂]₂

Organotitanium oxides as Lewis acidic supports of metal carbonyl species: [{Ti₃(η⁵-C₅Me₅)₃(µ-O)₃Me}{(µ-OC)M(CO)₂(η⁵-C₅H₅)}₂](M = Mo, W)

Synthesis of the triply-bonded dimolybdenum anions [Mo₂(η⁵-C₅H₅)₂(μ-PA₂)(μ-CO)₂]⁻ (A = Cy, Et, Ph, OEt): unsaturated hydride and carbyne derivatives

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Synthesis of the triply-bonded dimolybdenum anions [Mo₂(η⁵-C₅H₅)₂(μ-PA₂)(μ-CO)₂]⁻ (A = Cy, Et, Ph, OEt): unsaturated hydride and carbyne derivatives