期刊
CHEMISTRY-A EUROPEAN JOURNAL
卷 22, 期 36, 页码 12767-12776出版社
WILEY-V C H VERLAG GMBH
DOI: 10.1002/chem.201601843
关键词
iron; polymorphism; single-crystal-to-single-crystal; solvatomorphs; spin crossover
资金
- ERC [StG-2010-258060]
Two polymorphs of the spin crossover (SCO) compound [Fe(1,3-bpp)(2)](ClO4)(2) (1 and 2; 1,3-bpp=2-(pyrazol-1-yl)-6-(pyrazol-3-yl)pyridine) were prepared using a novel, stepwise procedure. Crystals of 1 deposit from dry solvents, while 2 is obtained from a solid-state procedure, by sequentially removing lattice H2O molecules from the solvatomorph [Fe(1,3-bpp)(2)](ClO4)(2)center dot 2H(2)O (2 center dot 2H(2)O), using single-crystal-to-single-crystal (SCSC) transformations. Hydrate 2 center dot 2H(2)O is obtained through the same reaction as 1, now with 2.5% of water added. Compounds 2 and 2 center dot 2H(2)O are unstable in the atmosphere and absorb or lose one equivalent of water, respectively, to both yield the stable solvatomorph [Fe(1,3-bpp) 2](ClO4)(2)center dot H2O (2 center dot H2O), also following SCSC processes. The four derivatives have been characterised by single-crystal X-ray diffraction (SCXRD). Furthermore, the homogeneity of the various compounds as well as their SCSC interconversions have been confirmed by powder X-ray diffraction (PXRD). Polymorphs 1 and 2 exhibit abrupt SCO behaviour near room temperature with T-1/2 up arrow=279/316 K and T-1/2 down arrow= 276/314 K (near 40 K of shift) and different cooperativity.
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