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Instruments / Technical Area	Publication Details	Published
I19-Small Molecule Single Crystal Diffraction	Steric and geometric tuning of π-conjugated antennae in europium(III) complexes for selective ADP recognition Samantha E. Bodman , Stephen J. Butler Chemistry – A European Journal 42 DOI: 10.1002/chem.202502251 Diamond Proposal Number(s): [26802] Open Access Show Abstract ▼ Abstract: The selective recognition of adenosine diphosphate (ADP) in water presents a significant challenge for synthetic supramolecular chemistry, driven by its biological importance in cellular energy transfer and enzymatic signaling pathways. Discriminating ADP from structurally similar anions such as ATP requires a high degree of host–guest complementarity. We recently developed [Eu.ADPGlow]−, a luminescent Eu(III) complex bearing two 6-substituted quinolyl-phenoxyacetate arms, which create a binding site at the central Eu(III) ion that accommodates ADP. Binding induces a tight interaction in water, involving both metal coordination and π–π stacking, switching the emission on with a 33-fold enhancement. Here, we examine how systematic changes in ligand geometry influence anion selectivity, by synthesizing four new Eu(III) complexes with pendant arms at the 4- or 7-positions of the quinoline scaffold. The 4-substituted systems provide a more accessible binding site and bind ADP, ATP, and AMP with limited selectivity between them, while the 7-substituted analogues impose steric hindrance at the Eu(III) center, resulting in minimal response to all tested anions. Only the 6-substituted complex [Eu.ADPGlow]− achieves optimal geometrical complementarity for ADP binding. These findings reinforce the importance of steric and geometric control in the design of selective lanthanide probes for biological anions in water.	Aug 2025
I20-Scanning-X-ray spectroscopy (XAS/XES)	Elucidating polyphosphate anion binding to lanthanide complexes using EXAFS and pulsed EPR Spectroscopy Hannah K. Pyle , Martyna Judd , Anthony Barancewicz , Alexander J. Mayer , Nicholas Cox , Simon A. Kondrat , Stephen J. Butler Inorganic Chemistry DOI: 10.1021/acs.inorgchem.4c03399 Diamond Proposal Number(s): [29024] Open Access Show Abstract ▼ Abstract: Reversible anion binding to lanthanide complexes in aqueous solution has emerged as an effective method for anion sensing. Through careful design of the organic ligand, luminescent lanthanide complexes capable of binding biologically relevant anions in a bidentate or monodentate manner can be realized. While single-crystal X-ray diffraction analyses and NMR spectroscopy have revealed the structural geometry of several host–guest complexes, the challenge remains in designing preorganized lanthanide receptors with enhanced anion selectivity for broader applications in diagnostics and bioimaging. To address this challenge, innovative and complementary methods to investigate host-anion binding geometry are becoming increasingly important. Herein, we demonstrate the combined use of Eu L3-edge extended X-ray absorption fine structure (EXAFS) and electron paramagnetic resonance (EPR) spectroscopy to elucidate the binding of nucleoside phosphates (ATP, ADP, and AMP) to a cationic lanthanide complex. We establish that ATP unequivocally binds the lanthanide center in a bidentate manner in water, while ADP adopts both bidentate and monodentate modes, and AMP binds in a monodentate manner. This interdisciplinary approach provides deeper insight into lanthanide host–guest chemistry in solution, laying the groundwork for designing emissive probes that undergo specific anion-induced structural changes and elicit desired optical responses upon binding.	Oct 2024
I19-Small Molecule Single Crystal Diffraction	Utility of tris(4-bromopyridyl) europium complexes as versatile intermediates in the divergent synthesis of emissive chiral probes Stephen J. Butler , Martina Delbianco , Nicholas H. Evans , Andrew T. Frawley , Robert Pal , David Parker , Robert S. Puckrin , Dmitry Yufit Dalton Transactions 43 (15), 5721-5730 DOI: 10.1039/c4dt00253a Diamond Proposal Number(s): [8682] Show Abstract ▼ Abstract: The synthetic utility of europium complexes with three coordinated 4-bromopyridyl groups for chromophore elaboration has been assessed in palladium-catalysed Sonogashira coupling reactions, and in copper(I) mediated click reactions of the triazide derivative, generated in situ. The crystal structure of the Eu complex of a p-OMe-phenyl substituted triazole at 100 K is reported in which the pendant triazole sensitising moieties interdigitate in the solid-state lattice. The triazole complex can be separated into Δ and Λ enantiomers by chiral HPLC but is weakly emissive in methanol (ε 5.5 mM−1 cm−1; λexc 320 nm; ϕ 0.2%), contrasting with a set of four alkynyl–aryl derivatives which are one thousand times brighter and absorb strongly with broad absorption maxima in the range 332 to 360 nm. An enantiopure europium complex gives an intense CPL signal in solution that is the strongest yet reported.	Feb 2014

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