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Incorporation of cubane-type Mo3S4 molybdenum cluster sulfides in the framework of mesoporous silica

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Incorporation of cubane-type Mo3S4 molybdenum cluster sulfides in the framework of mesoporous silica

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dc.contributor.author Carrillo, Adela I. es_ES
dc.contributor.author García-Martínez, Javier es_ES
dc.contributor.author Llusar, Rosa es_ES
dc.contributor.author Serrano, Elena es_ES
dc.contributor.author Sorribes, Ivan es_ES
dc.contributor.author Vicent, Cristina es_ES
dc.contributor.author Vidal Moya, José Alejandro es_ES
dc.date.accessioned 2017-06-19T09:04:01Z
dc.date.available 2017-06-19T09:04:01Z
dc.date.issued 2012-03-15
dc.identifier.issn 1387-1811
dc.identifier.uri http://hdl.handle.net/10251/83157
dc.description.abstract [EN] A new molybdenum siloxo cluster of formula [Mo3S4(dmpe)(3)(MPTES)(3)]PF6 (dmpe = 1,2-(bis)dimethylphosphinoethane; MPTES = (3-mercaptopropyl)triethoxysilane) has been synthesized with the ultimate goal of incorporating it into ordered mesoporous silica via covalent attachment. For this purpose, two different approaches, in situ and grafting, are employed. The first one is based in the co-condensation of the Mo3S4 siloxo cluster and tetraethylorthosilicate (TEOS) as mixed silicon sources in the presence of a surfactant (CTAB). The use of this approach allows for the incorporation of the Mo3S4 siloxo cluster into the structure of the mesoporous silica. For comparison purposes, the same Mo3S4 siloxo cluster has been immobilized on the surface of conventional mesoporous silica MCM-41, using more traditional grafting techniques. The physical and structural properties of both series of materials, containing different Mo3S4 cluster loadings, have been thoroughly investigated by means of powder X-ray diffraction (XRD), N-2 adsorption/desorption isotherms, transmission electron microscopy (TEM), magic-angle spinning (MAS) P-31 and CP/MAS Si-29 NMR, Fourier transform infrared (FT-IR) and UV-Vis diffuse reflectance (DRUV-Vis) spectroscopies. The chemical and structural integrity of the diphosphino Mo3S4 siloxo cluster is preserved in both the in situ and grafted mesoporous silica based materials. Depending on the incorporation approach, immobilization of the trinuclear sulfido cluster occurs into the silica matrix structure for the in situ materials or on the surface for the grafted ones. With these results, we show that it is possible to extend the incorporation of chemical functionalities into the structure of mesoporous materials to Mo3S4 siloxo clusters. (C) 2011 Elsevier Inc. All rights reserved. es_ES
dc.description.sponsorship The financial support of the Spanish Ministerio de Ciencia e Innovacion (CTQ2005-09385-C03-02 and CTQ2008-02670), Fundacio Bancaixa-UJI (P1.1B2010-46), and Generalitat Valenciana (ACOMP/2011/037 and Prometeo/2009/053) is gratefully acknowledged. I.S. thanks the Spanish Ministerio de Ciencia e Innovacion (MICINN) for a doctoral fellowship (FPU). E.S. acknowledges financial support from Spanish MICINN through the Juan de la Cierva Program (ref. JCI-2008-2165) and from Generalitat Valenciana (ref. BEST2011/223). The authors thank Dr. Cristina Almansa Carrascosa, for assistance with the Transmission Electron Microscopy. Special thanks go to Dr. Wieslaw Roth for his advice and helpful comments on the work presented in this manuscript. The authors also thank the Servei Central d'Instrumentacio Cientifica (SCIC) of the University Jaume I and the Technical Services of the University of Alicante.
dc.language Inglés es_ES
dc.publisher Elsevier es_ES
dc.relation MICINN/CTQ2005-09385-C03-02 es_ES
dc.relation Fundacio Bancaixa-UJI/P1.1B2010-46 es_ES
dc.relation GV/ACOMP/2011/037 es_ES
dc.relation info:eu-repo/grantAgreement/MICINN//CTQ2008-02670/ES/NUEVOS ASPECTOS SOBRE LA QUIMICA DE LOS CALCOGENUROS CLUSTER DE METALES DE TRANSICION DIRIGIDOS A SUS APLICACIONES EN CATALISIS Y ELECTRONICA MOLECULAR/
dc.relation GV/PROMETEO/2009/053
dc.relation info:eu-repo/grantAgreement/MICINN//JCI-2008-2165/ES/JCI-2008-2165/
dc.relation GV/BEST2011/223
dc.relation.ispartof Microporous and Mesoporous Materials es_ES
dc.rights Reserva de todos los derechos es_ES
dc.subject Molybdenum clusters es_ES
dc.subject Siloxo ligands es_ES
dc.subject Mesoporous silica materials es_ES
dc.subject Adsorption es_ES
dc.title Incorporation of cubane-type Mo3S4 molybdenum cluster sulfides in the framework of mesoporous silica es_ES
dc.type Artículo es_ES
dc.identifier.doi 10.1016/j.micromeso.2011.10.005
dc.rights.accessRights Cerrado es_ES
dc.contributor.affiliation Universitat Politècnica de València. Instituto Universitario Mixto de Tecnología Química - Institut Universitari Mixt de Tecnologia Química es_ES
dc.description.bibliographicCitation Carrillo, AI.; García-Martínez, J.; Llusar, R.; Serrano, E.; Sorribes, I.; Vicent, C.; Vidal Moya, JA. (2012). Incorporation of cubane-type Mo3S4 molybdenum cluster sulfides in the framework of mesoporous silica. Microporous and Mesoporous Materials. 151:380-389. https://doi.org/10.1016/j.micromeso.2011.10.005 es_ES
dc.description.accrualMethod S es_ES
dc.relation.publisherversion http://doi.org/10.1016/j.micromeso.2011.10.005 es_ES
dc.description.upvformatpinicio 380 es_ES
dc.description.upvformatpfin 389 es_ES
dc.type.version info:eu-repo/semantics/publishedVersion es_ES
dc.description.volume 151 es_ES
dc.relation.senia 214905 es_ES
dc.contributor.funder Ministerio de Ciencia e Innovación
dc.contributor.funder Fundación Bancaja
dc.contributor.funder Universitat Jaume I
dc.contributor.funder Generalitat Valenciana


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