%0 Journal Article %T In situ X-ray Measurements to Probe a New Solid-State Polycondensation Mechanism for the Design of Supramolecular Organo-Bridged Silsesquioxanes %+ Laboratoire des colloïdes, verres et nanomatériaux (LCVN) %+ Institut Charles Gerhardt Montpellier - Institut de Chimie Moléculaire et des Matériaux de Montpellier (ICGM ICMMM) %+ European Synchrotron Radiation Facility (ESRF) %A Dieudonné, Philippe %A Wong Chi Man, Michel %A Pichon, Benoît P. %A Vellutini, Luc %A Bantignies, Jean-Louis %A Blanc, Christophe %A Creff, Gaëlle %A Finet, Stéphanie %A Sauvajol, Jean-Louis %A Bied, Catherine %A Moreau, Joël J.E. %< avec comité de lecture %@ 1613-6810 %J Small %I Wiley-VCH Verlag %V 5 %N 4 %P 503-510 %8 2009 %D 2009 %R 10.1002/smll.200800254 %K SAXS %K silsequioxanes %K sol–gel materials %K solid-state reactions %K reaction mechanisms %K WAXS %Z Chemical Sciences/Organic chemistryJournal articles %X A long-range ordered organic/inorganic material is synthesized from a bissilane, (EtO)3Si–(CH2)3–NHCONH–C6H4–NHCONH–(CH2)3–Si(OEt)3. This crosslinked sol–gel solid exhibits a supramolecular organization via intermolecular hydrogen bonding interactions between urea groups (–NHCONH–) and covalent siloxane bonding, Si–O–Si . Time-resolved in situ X-ray measurements (coupling small- and wide-angle X-ray scattering techniques) are performed to follow the different steps involved in the synthetic process. A new mechanism based on the crystallization of the hydrolyzed species followed by their polycondensation in solid state is proposed. %G English %L hal-00381858 %U https://hal.science/hal-00381858 %~ CNRS %~ UNIV-MONTP1 %~ UNIV-MONTP2 %~ ENSC-MONTPELLIER %~ ICG %~ LCVN %~ CHIMIE %~ UNIV-MONTPELLIER %~ UM1-UM2 %~ TEST2-HALCNRS