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Spontaneous Synthesis of [Fe II (Atrz) 3 ]SO 4 and its Analogues Through Accelerated Ageing: New Insights from Small‐Scale Reactions
Author(s) -
Lonergan Rhona F.,
Conway Georgina A.,
Doheny Patrick W.,
Shepherd Helena J.
Publication year - 2022
Publication title -
chemistry – a european journal
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.687
H-Index - 242
eISSN - 1521-3765
pISSN - 0947-6539
DOI - 10.1002/chem.202201823
Subject(s) - ligand (biochemistry) , chemistry , metal , solvent , salt (chemistry) , reaction rate , relative humidity , chemical reaction , polymer , crystal structure , crystal (programming language) , crystallography , catalysis , organic chemistry , thermodynamics , biochemistry , physics , receptor , computer science , programming language
Accelerated ageing reactions that take place between two solid materials on contact in the absence of added solvent have been used to synthesize two spin‐crossover‐active 1D coordination polymers and one of their Cu(II) analogues. The hygroscopy of the ligands and the relative humidity of the reaction chamber have been shown to be particularly important factors in the rate of reaction. Small‐scale reactions between a few individual crystals have allowed observation of deliquescence of the 4‐aminotriazole ligand at high humidity. The metal salt does not dissolve, and the ligand diffuses into the crystal of the metal salt during the reaction. In the case of the Cu analogue, the formation of the product causes the crystal of the metal salt to deform with the formation of pseudocrystals, which have a fibrous structure.