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Reversible single-crystal to single-crystal phase transformation between a new Werner clathrate and its apohost

Matos, Catiúcia R. M. O ; Sanii, Rana ; Wang, Shi-Qiang ; Ronconi, Célia M ; Zaworotko, Michael J

Dalton transactions : an international journal of inorganic chemistry, 2021-09, Vol.5 (37), p.12923-1293 [Periódico revisado por pares]

England: Royal Society of Chemistry

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  • Título:
    Reversible single-crystal to single-crystal phase transformation between a new Werner clathrate and its apohost
  • Autor: Matos, Catiúcia R. M. O ; Sanii, Rana ; Wang, Shi-Qiang ; Ronconi, Célia M ; Zaworotko, Michael J
  • Assuntos: Butanol ; Chemistry ; Clathrates ; Crystal structure ; Crystals ; Ligands ; Nitrobenzene ; Phase transitions ; Single crystals ; Solid state ; Synthesis ; X ray powder diffraction ; X-ray diffraction ; Xylene
  • É parte de: Dalton transactions : an international journal of inorganic chemistry, 2021-09, Vol.5 (37), p.12923-1293
  • Notas: For ESI and crystallographic data in CIF or other electronic format see DOI
    1995785-1995796
    2065192
    10.1039/d1dt01839f
    Electronic supplementary information (ESI) available: Complete synthetic protocol, compound characterisation and crystallographic details. CCDC
    and
    ObjectType-Article-1
    SourceType-Scholarly Journals-1
    ObjectType-Feature-2
    content type line 23
  • Descrição: In this work, we report the synthesis and structural characterisation of the ligand 2-(pyridin-3-yl)-benzo[ de ]isoquinoline-1,3(2 H )-dione, 5 , its isostructural Werner complexes ML 4 (NCS) 2 (L = 5 ; M = Co( ii ) and Ni( ii )), and five clathrates with three aromatic guests, ML 4 (NCS) 2 ·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 (C 3 S 3 , Cocrystal Controlled Solid-State Synthesis). The Werner complexes ML 4 (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 °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 °C for 48-96 h. The clathrates were observed to transform to the apohost ML 4 (NCS) 2 upon heating. CoL 4 (NCS) 2 ·2NB was subsequently regenerated by exposing CoL 4 (NCS) 2 to liquid NB at 60 °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 CoL 4 (NCS) 2 and its Werner clathrate CoL 4 (NCS) 2 ·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. A new Werner complex exhibits reversible transformation between apohost and host-guest phase induced by nitrobenzene.
  • Editor: England: Royal Society of Chemistry
  • Idioma: Inglês
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