Naslov
In situ PXRD monitoring the mechanosynthesis of metal-organic halogen-bonded cocrystals

Autori
Lisac, Katarina ; Germann, Luzia S. ; Etter, Martin ; Dinnebier, Robert E. ; Friščić, Tomislav ; Cinčić, Dominik

Vrsta, podvrsta i kategorija rada
Sažeci sa skupova, sažetak, znanstveni

Izvornik
III. simpozij supramolekulske kemije - Knjiga sažetaka / Frkanec, Leo ; Namjesnik, Danijel ; Tomišić, Vladislav - Zagreb : Institut Ruđer Bošković, 2019, 22-22

ISBN
978-953-7941-27-7

Skup
3. simpozij supramolekulske kemije (Supramolecular Chemistry 2019)

Mjesto i datum
Zagreb, Hrvatska, 03.12.2019

Vrsta sudjelovanja
Poster

Vrsta recenzije
Domaća recenzija

Ključne riječi
in situ PXRD ; mechanosynthesis ; halogen bond ; cocrystals

Sažetak
In the last decade, in situ powder X-ray diffraction (PXRD) monitoring of mechanochemical reactions has become a prominent technique for studying the course and mechanisms of organic and metal-organic solid formation. Following our previous study on mechanochemical syntheses of metal-organic halogen-bonded cocrystals, in this work we have investigated mechanosynthesis of cocrystals containing CoCl2bzpy2 (bzpy = 2- benzoylpyridine) and a halogen bond donor, 1, 4- diiodotetra-fluorobenzene (14tfib), by in situPXRD. First, we performed experiments in solution, and have unexpectedly obtained three different products: two cocrystals with different metal-organic unit isomers, trans-(CoCl2bzpy2) (14tfib)2 and cis-(CoCl2bzpy2)(14tfib)2, and a cocrystal of 1:1 stoichiometry, cis-(CoCl2bzpy2) (14tfib). In order to determine whether single phases could be prepared, mechanosynthesis of obtained cocrystals was studied by in situPXRD using synchrotron X-ray radiation. Three different liquid-assisted grinding experiments were monitored: grinding of CoCl2bzpy2and 14tfibin the 1:2 molar ratio, one-pot grinding of CoCl2·6H2O, bzpy and 14tfibin the 1:2:2 molar ratio and grinding of CoCl2bzpy2 and 14tfibin the 1:1 molar ratio. All three monitored reactions revealed presence of a cocrystal with cis i somer as an intermediate and fast conversions to a final, thermodynamically more stable product, trans- (CoCl2bzpy2)(14tfib)2 , in less than 20 min. Single crystal X-ray diffraction experiments reveal that dominant supramolecular interactions in all obtained solids are I···Cl halogen bonds. In the trans-cocrystal halogen bonds form 2D networks while in cis- cocrystals 1D chains are formed.

Izvorni jezik
Engleski

Znanstvena područja
Kemija

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