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The intercalated LDH and the mixed metal oxide (MMO) obtained after its calcination were characterized by elemental and thermogravimetric analyses, powder X\u2010ray diffraction (PXRD), FT\u2010IR and FT\u2010Raman spectroscopy, <jats:sup>13<\/jats:sup>C and <jats:sup>27<\/jats:sup>Al MAS NMR, and scanning electron microscopy. The observed basal spacing of 17.1 \u00c5 for the LDH Zn,Al\u2010Cp*MoO<jats:sub>3<\/jats:sub> (corresponding to a gallery height of 12.3 \u00c5) suggests that the guest anions self\u2010assemble into dimers via offset face\u2010to\u2010face Cp*<jats:bold>\u00b7\u00b7\u00b7<\/jats:bold>Cp* interactions, which facilitates hydrogen\u2010bonding interactions between the oxido ligands of the complexes and the layer hydroxyl groups, while positioning the hydrophobic aromatic rings towards the center of the galleries. Calcination of Zn,Al\u2010Cp*MoO<jats:sub>3<\/jats:sub> at 550 \u00b0C under air gave an MMO comprising well\u2010dispersed ZnO, \u03b1\u2010ZnMoO<jats:sub>4<\/jats:sub> and ZnAl<jats:sub>2<\/jats:sub>O<jats:sub>4<\/jats:sub> (spinel) oxides in a molar of ca. 1.4:1.6:1. The MMO exhibited catalytic activity for the epoxidation of <jats:italic>cis<\/jats:italic>\u2010cyclooctene with <jats:italic>tert<\/jats:italic>\u2010butylhydroperoxide (TBHP) as terminal oxidant, with quantitative yield of the epoxide being achieved within 24 h at 85 \u00b0C.<\/jats:p>","DOI":"10.1002\/ejic.202000127","type":"journal-article","created":{"date-parts":[[2020,4,16]],"date-time":"2020-04-16T06:05:49Z","timestamp":1587017149000},"page":"2408-2416","update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":2,"title":["Intercalation of (\u03b7<sup>5<\/sup>\u2010Pentamethylcyclopentadienyl)trioxomolybdenum(VI) in a Layered Double Hydroxide"],"prefix":"10.1002","volume":"2020","author":[{"ORCID":"https:\/\/orcid.org\/0000-0001-9598-1275","authenticated-orcid":false,"given":"Ana C.","family":"Gomes","sequence":"first","affiliation":[{"name":"CICECO \u2010 Aveiro Institute of Materials Department of Chemistry University of Aveiro  Campus Universit\u00e1rio de Santiago 3810\u2010193 Aveiro Portugal"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-1932-4975","authenticated-orcid":false,"given":"Patr\u00edcia","family":"Neves","sequence":"additional","affiliation":[{"name":"CICECO \u2010 Aveiro Institute of Materials Department of Chemistry University of Aveiro  Campus Universit\u00e1rio de Santiago 3810\u2010193 Aveiro Portugal"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-0221-8508","authenticated-orcid":false,"given":"Sandra","family":"Gago","sequence":"additional","affiliation":[{"name":"CICECO \u2010 Aveiro Institute of Materials Department of Chemistry University of Aveiro  Campus Universit\u00e1rio de Santiago 3810\u2010193 Aveiro Portugal"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-3495-2133","authenticated-orcid":false,"given":"Anabela A.","family":"Valente","sequence":"additional","affiliation":[{"name":"CICECO \u2010 Aveiro Institute of Materials Department of Chemistry University of Aveiro  Campus Universit\u00e1rio de Santiago 3810\u2010193 Aveiro Portugal"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-2836-7715","authenticated-orcid":false,"given":"Isabel S.","family":"Gon\u00e7alves","sequence":"additional","affiliation":[{"name":"CICECO \u2010 Aveiro Institute of Materials Department of Chemistry University of Aveiro  Campus Universit\u00e1rio de Santiago 3810\u2010193 Aveiro Portugal"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-6243-7692","authenticated-orcid":false,"given":"Martyn","family":"Pillinger","sequence":"additional","affiliation":[{"name":"CICECO \u2010 Aveiro Institute of Materials Department of Chemistry University of Aveiro  Campus Universit\u00e1rio de Santiago 3810\u2010193 Aveiro Portugal"}]}],"member":"311","published-online":{"date-parts":[[2020,5,19]]},"reference":[{"doi-asserted-by":"publisher","key":"e_1_2_6_2_1","DOI":"10.1039\/C4DT00203B"},{"doi-asserted-by":"publisher","key":"e_1_2_6_3_1","DOI":"10.1021\/cm960142l"},{"doi-asserted-by":"publisher","key":"e_1_2_6_4_1","DOI":"10.1021\/cr00034a005"},{"doi-asserted-by":"publisher","key":"e_1_2_6_5_1","DOI":"10.1039\/C5CS00758E"},{"key":"e_1_2_6_6_1","first-page":"989","volume":"18","author":"O'Hare D.","year":"1994","journal-title":"New J. 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