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

Literature Information

Publication Date 2015-08-24
DOI 10.1039/C5CE01689D
Impact Factor 3.545
Authors

Jane V. Knichal, William J. Gee, Andrew D. Burrows, Paul R. Raithby, Chick C. Wilson


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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.

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CrystEngComm

CrystEngComm
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CrystEngComm is the forum for the design and understanding of crystalline materials. We welcome studies on the investigation of molecular behaviour within crystals, control of nucleation and crystal growth, engineering of crystal structures, and construction of crystalline materials with tuneable properties and functions. We publish hypothesis-driven research into… how crystal design affects thermodynamics, phase transitional behaviours, polymorphism, morphology control, solid state reactivity (crystal-crystal solution-crystal, and gas-crystal reactions), optoelectronics, ferroelectric materials, non-linear optics, molecular and bulk magnetism, conductivity and quantum computing, catalysis, absorption and desorption, and mechanical properties. Using Techniques and methods including… Single crystal and powder X-ray, electron, and neutron diffraction, solid-state spectroscopy, spectrometry, and microscopy, modelling and data mining, and empirical, semi-empirical and ab-initio theoretical evaluations. On crystalline and solid-state materials. We particularly welcome work on MOFs, coordination polymers, nanocrystals, host-guest and multi-component molecular materials. We also accept work on peptides and liquid crystals. All papers should involve the use or development of a design or optimisation strategy. Routine structural reports or crystal morphology descriptions, even when combined with an analysis of properties or potential applications, are generally considered to be outside the scope of the journal and are unlikely to be accepted.

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