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Issue 42, 2015
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A new small molecule gelator and 3D framework ligator of lead(II)

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Abstract

Reacting equimolar quantities of 5-allenyl-1,3-benzenedicarboxylic acid (H2abd) with lead(II) acetate trihydrate in N,N-dimethylformamide (DMF) under solvothermal conditions results in formation of a metallogel with a critical gelation percentage of 1% w/v. Elemental analysis performed on the gel provided a molecular composition ratio of [Pb(abd)(H2O)]n (1). Viewing the gel by scanning electron microscopy (SEM) identified an entangled network of cross-linked nano-fibres. 1H-NMR aliquots of hydrated lead(II) acetate added to a solution of H2abd in deuterated DMF allows inferences to be made about solution-state behaviour that occurs during the initial gel aggregation stage. Under non-solvothermal conditions, combining H2abd and hydrated lead(II) acetate resulted in formation of single crystals suitable for X-ray diffraction, which were identified as a 3D coordination polymer with composition [Pb(abd)(DMF)] (2). Structural features observed within this 3D coordination polymer provide the basis for assigning the molecular structure to the fibrils present within gel 1. This assertion is supported by comparable vibrational profiles taken from a sample of dried gel 1 to that of crystalline 2, and the matching of early solution-state 1H-NMR spectroscopic trends to later solid-state observations.

Graphical abstract: A new small molecule gelator and 3D framework ligator of lead(ii)

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Publication details

The article was received on 03 Aug 2015, accepted on 21 Aug 2015 and first published on 24 Aug 2015


Article type: Paper
DOI: 10.1039/C5CE01689D
Citation: CrystEngComm, 2015,17, 8139-8145
  • Open access: Creative Commons BY license
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    A new small molecule gelator and 3D framework ligator of lead(II)

    J. V. Knichal, W. J. Gee, A. D. Burrows, P. R. Raithby and C. C. Wilson, CrystEngComm, 2015, 17, 8139
    DOI: 10.1039/C5CE01689D

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