engleski

Attempted cocrystallisation yields hydrogen-bonded salts of β-diketones

The atempt to use liquid-assisted grinding (LAG)[1] to prepare the Co(dbm)2(tmo)2 complex from CoO, dibenzoylmethane (Hdbm) and thiomorpholine (tmo) failed. Instead, powder diffraction (PXRD) indicated that a new organic phase was obtained. The experiment was repeated without CoO and in several Hdbm to tmo stoichiometry ratios. PXRD patterns and thermal analysis confirmed that the product consists of Hdbm and tmo in a 1 : 1 stoichiometric ratio. Although the product was soluble in various organic solvents it was not possible to re-crystallise it, as pure Hdbm was repeatedly obtained. Subsequently, single crystals were obtained from a solution in liquid tmo. LAG screening of mechanochemical reactivity revealed that Hdbm also readily forms new materials with secondary amines: morpholine (mor), piperidine (pip) and 2, 6-dimethylpiperidine (26Mepip). The use of these liquids as solvents provided single crystals of (Hdbm)•(mor), (Hdbm)•(pip) and (Hdbm)•(26Mepip).

liquid assisted grinding; hydrogen bonded beta-diketonate organic salts

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