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Molybdenum complexes bearing the tris(1-pyrazolyl)methanesulfonate ligand: synthesis, characterization and electrochemical behaviour

2010-05-21Journal article Restricted access
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dc.contributor.authorDinoi, Chiara
dc.contributor.authorGuedes Da Silva, M. Fátima C.
dc.contributor.authorAlegria, Elisabete
dc.contributor.authorSmolenski, Piotr
dc.contributor.authorMartins, Luisa
dc.contributor.authorPoli, Rinaldo
dc.contributor.authorPombeiro, Armando
dc.date.accessioned2020-07-20T14:02:10Z
dc.date.available2020-07-20T14:02:10Z
dc.date.issued2010-05-21
dc.description.abstractThe tris(1‐pyrazolyl)methanesulfonate lithium salt Li(Tpms) [Tpms = SO3C(pz)3–] reacts with [Mo(CO)6] in NCMe heated at reflux to yield Li[Mo(Tpms)(CO)3] (1 ), which, upon crystallization from thf, forms the coordination polymer [Mo(Tpms)(CO)2(μ‐CO)Li(thf)2]n (2 ). Reaction of 1 with I2, HBF4 or AgBF4 yields [Mo(Tpms)I(CO)3] (3 ), [Mo(Tpms)H(CO)3] (5 ) or [Mo(Tpms)O2]2(μ‐O) (7 ), respectively. The high‐oxidation‐state dinuclear complexes [{Mo(Tpms)O(μ‐O)}2] (4 ) and [{Mo(tpms)OCl}2](μ‐O) (6 ) are formed upon exposure to air of solutions of 3 and 5 , respectively. Compounds 1 –7 , which appear to be the first tris(pyrazolyl)methanesulfonate complexes of molybdenum to be reported, were characterized by IR, 1H and 13C NMR spectroscopy, ESI‐MS, elemental analysis, cyclic voltammetry and, in the cases of Li(Tpms) and compounds 2 , 4· 2CH3CN, 6· 6CHCl3 and 7 , by X‐ray diffraction analyses. Li(Tpms) forms a 1D polymeric structure {i.e., [Li(tpms)]n } with Tpms as a tetradentate N2O2 chelating ligand that bridges two Li cations with distorted tetrahedral coordination. Compound 2 is a 1D coordination polymer in which Tpms acts as a bridging tetradentate N3O ligand and each Li(thf)2+ moiety is coordinated by one bridging CO ligand and by the sulfonyl group of a contiguous monomeric unit. In 4 , 6 and 7 , the Tpms ligand is a tridentate chelator either in the NNO (in 4 ) or in the NNN (in 6 and 7 ) fashion. Complexes 1 , 3 and 5 exhibit, by cyclic voltammetry, a single‐electron oxidation at oxidation potential values that indicate that the Tpms ligand has an electron‐donor character weaker than that of cyclopentadienyl.pt_PT
dc.description.versioninfo:eu-repo/semantics/publishedVersionpt_PT
dc.identifier.citationDINOI, Chiara; [et al] – Molybdenum complexes bearing the tris(1-pyrazolyl)methanesulfonate ligand: synthesis, characterization and electrochemical behaviour. European Journal of Inorganic Chemistry. ISSN 1099-0682. Volume 2010, N.º 16 (2010), pp. 2415-2424pt_PT
dc.identifier.doi10.1002/ejic.201000018pt_PT
dc.identifier.issn1099-0682
dc.identifier.urihttp://hdl.handle.net/10400.21/12061
dc.language.isoengpt_PT
dc.peerreviewedyespt_PT
dc.publisherWiley-VCH Verlagpt_PT
dc.relationGrant Number: MRTN‐CT‐2003‐503864 - European Commissionpt_PT
dc.relationGrant Number: BPD/20869/04 - FCTpt_PT
dc.relation.publisherversionhttps://chemistry-europe.onlinelibrary.wiley.com/doi/epdf/10.1002/ejic.201000018pt_PT
dc.subjectMolybdenumpt_PT
dc.subjectScorpionatespt_PT
dc.subjectElectrochemistrypt_PT
dc.subjectSolid‐state structurespt_PT
dc.titleMolybdenum complexes bearing the tris(1-pyrazolyl)methanesulfonate ligand: synthesis, characterization and electrochemical behaviourpt_PT
dc.typejournal article
dspace.entity.typePublication
oaire.citation.endPage2424pt_PT
oaire.citation.issue16pt_PT
oaire.citation.startPage2415pt_PT
oaire.citation.titleEuropean Journal of Inorganic Chemistrypt_PT
oaire.citation.volume2010pt_PT
person.familyNameDinoi
person.familyNameGuedes da Silva
person.familyNameAlegria
person.familyNameSmolenski
person.familyNameMartins
person.familyNamePoli
person.familyNamePombeiro
person.givenNameChiara
person.givenNameM. Fátima C.
person.givenNameElisabete
person.givenNamePiotr
person.givenNameLuisa
person.givenNameRinaldo
person.givenNameArmando
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