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

Reacting equimolar quantities of 5-allenyl-1,3-benzenedicarboxylic acid (H 2 abd ) 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 )(H 2 O)] n ( 1 ). Viewing the gel by scanning electron microscopy (SEM) identified an entangled network of cross-linked nano-fibres. 1 H-NMR aliquots of hydrated lead( ii ) acetate added to a solution of H 2 abd 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 H 2 abd 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 1 H-NMR spectroscopic trends to later solid-state observations.