engleski

Cocrystal Formation Precedes the Mechanochemically Acetate-Assisted C−H Activation with [Cp*RhCl2]2

Thisworkreportstheexperimentallystudiedmechanochem ica lformationof rhodacyclesby ballmillingpyridine- andquinoline- derivedsubstratesand[Cp*RhCl2]2inthe presenceof NaOAc.Ex-situanalysisof the mechanochem- icalreactionsusingpowderX-raydiffraction(PXRD), solid- stateUV-visspectroscopyandATR- FTIRspectroscopyre- vealedtheformationof unexpectedcocrystalsbetweenthesubstratesandthe rhodiumdimerpriorto the CH activationstep.Thissequenceof eventsdiffersfromthegenerallyacceptedstepsin solutionin whichcleavageof [Cp*RhCl2]2isinitiatedby acetateions.Additionally, the mechanochemicalapproachenabledthe synthesisof the six-memberedrhoda-cycle[Cp*Rh(2- benzilpyridine)Cl], a metalcomplexrepeatedlyreportedas inaccessiblein solution.Altogether, the resultsofthisinvestigationclarifysomeof the fundamentalaspectsofmechanochemicalcyclometallatio ns.

mechanochemistry, C-H activation

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