期刊
DALTON TRANSACTIONS
卷 50, 期 37, 页码 12923-12930出版社
ROYAL SOC CHEMISTRY
DOI: 10.1039/d1dt01839f
关键词
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资金
- Science Foundation Ireland [16/IA/B2549]
- European Research Council [ADG 885695]
- Brazilian Federal Agency for Support and Evaluation of Graduate Education (CAPES)
- Brazilian agency National Council for Scientific and Technological Development (CMR) [313799/2017-2]
- Brazilian agency National Council for Scientific and Technological Development ( CNPq) [313799/2017-2]
- Rio de Janeiro Research Foundation (FAPERJ, Cientistas do Nosso Estado) [E-26/202.629/2019]
This work presents the synthesis and structural characterisation of a new ligand, its isostructural Werner complexes with Co(II) and Ni(II), and clathrates with various aromatic guests. The compounds were prepared through solid-state synthesis and different reaction conditions, with phase transformation observed upon heating.
In this work, we report the synthesis and structural characterisation of the ligand 2-(pyridin-3-yl)-benzo[de]isoquinoline-1,3(2H)-dione, 5, its isostructural Werner complexes ML4(NCS)(2) (L = 5; M = Co(II) and Ni(II)), and five clathrates with three aromatic guests, ML4(NCS)(2)center dot 2G (M = Co(II) and Ni(II), G = nitrobenzene (NB); M = Co, G = 1,2-dichlorobenzene (1,2-DCB); M = Co(II) and Ni(II), G = o-xylene (OX)). 5 was prepared in high yield by condensation in the solid-state ((CS3)-S-3, Cocrystal Controlled Solid-State Synthesis). The Werner complexes ML4(NCS)(2) (M = Co(II) and Ni(II)) (apohosts) were prepared by reacting M(NCS)(2) (M = Co(II) and Ni(II)) and 5 in 1-butanol at 60 degrees C for 24 h. The Werner clathrates were prepared by reacting M(NCS)(2) (M = Co(II) and Ni(II)), G and 5 in 1-butanol at 60 degrees C for 48-96 h. The clathrates were observed to transform to the apohost ML4(NCS)(2) upon heating. CoL4(NCS)(2)center dot 2NB was subsequently regenerated by exposing CoL4(NCS)(2) to liquid NB at 60 degrees C for 48 h. This phase change occurred as a single-crystal to single-crystal phase transformation and was studied by single crystal X-ray diffraction, powder X-ray diffraction and thermal analyses. Structural analyses of the apohost CoL4(NCS)(2) and its Werner clathrate CoL4(NCS)(2)center dot 2NB indicated that rotational freedom of the Co-N bonds together with torsional flexibility of the ligand between the imide bond and the pyridine moiety are key to enabling the structural switching induced by exposure to NB or its removal.
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