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In this work we present a straightforward synthesis towards hierarchically structured, macroporous carbon\/titania monoliths with ordered mesopores derived from resorcinol\/formaldehyde monoliths and a glycolated titanium precursor. We demonstrate the influence of various reaction solvents, where diol\u2010based media and the proportion of the catalyst seem to be essential in controlling spinodal decomposition, obtaining similar monolithic structures under different synthesis conditions. Based on these observations, we further homogeneously incorporated TiO<jats:sub>2<\/jats:sub> into the carbon structure by an <jats:italic>in\u2005situ<\/jats:italic> synthesis approach, obtaining structural features similar to pure carbon materials with surface areas of about 400\u2005m<jats:sup>2<\/jats:sup>\u2009g<jats:sup>\u22121<\/jats:sup>, periodically arranged mesopores with a mean distance of 10\u201311\u2005nm and cellular macroporosity.<\/jats:p>","DOI":"10.1002\/cplu.202000740","type":"journal-article","created":{"date-parts":[[2021,2,20]],"date-time":"2021-02-20T12:45:22Z","timestamp":1613825122000},"page":"275-283","update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":3,"title":["A Facile One\u2010Pot Synthesis of Hierarchically Organized Carbon\/TiO<sub>2<\/sub> Monoliths with Ordered 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