RSC Sir Geoffrey Wilkinson Dalton Poster Symposium 2022

7 September 2022, London Sir Geoffrey Wilkinson Dalton Poster Symposium

Book of Abstracts

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Welcome

Welcome to the RSC Sir Geoffrey Wilkinson Dalton Poster Symposium 2022, which celebrates the breadth and strength of inorganic chemistry research by those in the early stages of their careers. As a community, we are committed to supporting early career researchers in the inorganic chemistry community, and we are delighted to see this event go from strength to strength. This year, we were delighted to receive 93 applications to take part in the symposium, and the pre-selection committee felt privileged to be given this insight into the range and depth of high-quality, innovative inorganic chemistry taking place. We are also very pleased to welcome Dr James Wilton-Ely from Imperial College London and Dr Ruth Webster from the University of Bath to the meeting today, to deliver our plenary lectures. Dr Wilton-Ely is the 2021 winner of the Dalton Community mid-career Award: Sir Geoffrey Wilkinson Award for contributions to the application of metals in biological sensing and medical imaging. Dr Webster is the winner of the 2022 Dalton Division early career award: Sir Edward Frankland Fellowship for outstanding research including mechanistic elucidation of iron- catalysed, atom-efficient transformations of main group elements. This symposium wouldn’t be taking place at all without the generous support of the Wilkinson Charitable Foundation, and the enthusiastic support of a large number of academic supervisors and their research groups. In addition, Dalton Transactions has kindly provided a poster prize, which will be selected by the participants themselves. Please do enjoy talking with your fellow delegates and judges and take some time to appreciate and learn about the very best in inorganic chemistry research.

Dr Rosa Arrigo

Professor Mike Ward Dalton Community President

Chair of the Organising Committee

Scientific Committee

Rosa Arrigo (Chair) University of Salford, UK

Ian Fairlamb University of York, UK

Anna Peacock University of Birmingham, UK

Poster presentations

P01

Isolation of monomeric copper(II) phenolateselenoether complexes and their electrocatalytic hydrogen gas evolution activity Aditya Upadhyay Indian Institute of Science Education and Research Bhopal, India

P02

Coordination chemistry of azophosphines Emma Jordan University of Birmingham, UK

P03

Synthesis and reactivity of bis(diphenylphosphino)amine-type ligand cobalt complexes Adam Carrick Durham University, UK New weakly coordinating chiral anions and their application in enantioselective catalysis Richard Collins Imperial College London, UK

P04

P05

New layered vanadium oxychalcogenides Nicola Kelly University of Oxford, UK

P06

Tuning magnetism and superconductivity in nickel- and cobalt-based chalcogenides Ludmila Babicova University of Oxford, UK Solid-state preparation of single-phase Na 3 Zr 2-x Si 2 PO 12-2x solid electrolyte for Na- ion solid-state batteries. Ademola Adetona University of Sheffield, UK Synthesis of size-controlled iron oxide nanocubes for MPI-MFH applications Stanley Harvell-Smith UCL, UK Design of aluminium precursor compounds for metal thin films deposition Shreya Mrig UCL, UK

P07

P08

P09

P10

ImPAC: immobilised phosphines for applications in catalysis Jake Backhouse Durham University, UK

P11

Insights into the formation of ruthenium hydrides via Fischer carbene intermediates Katie Grant University of Edinburgh, UK Zintl clusters, multifunctional ligands for homogeneous catalysts Oliver Townrow University of Oxford, UK Heterobimetallic complexes supported by a multidentate tripodal ligand Benedict Thompson King’s College London, UK Magnetically - triggered protein release using iron oxide core - PNIPMAM shell nanoparticles Rajat Sharma University of York, UK

P12

P13

P14

P15

Magnesium-stabilised transition metal formyl complexes: structures, bonding, and ethenediolate formation

Joseph Parr Imperial, UK

P16

Exploring the synthesis and structure of copper(II)-oxo clusters Tom Barnes University of Warwick, UK

P17

Aikinite as a potential thermoelectric material with ultra-low thermal conductivity Shriparna Mukherjee University of Reading, UK Advanced oxidation of calmagite using in situ generated hydrogen peroxide catalyzed by manganese(ii) ions and bicarbonate Ye Cao Queen Mary University of London, UK Synthesis, reactivity and decomposition of aryl phospha-enolates Stephanie Urwin University of Oxford, UK A coumarin-porphyrin break-apart probe for heme oxygenase-1 Edward Walter Imperial College London, UK Polyoxometalate stabilized gold nanoparticles in polymeric ionic liquid as a catalyst Aeshah Alrubayyi Newcastle University, UK

P18

P19

P20

P21

P22

Synthesis and structures of thiamacrocycle stabilised cations and dications of M(II) (M = Ge, Sn, Pb) Rhys King University of Southampton, UK Facile reductions of nitro-organics and hydroaminations mediated by an Fe(salen) Complex Emily Pocock University of Bath, UK Mechanistic investigations into the Pauson-Khand reaction: using descriptor- based methods and in-situ IR spectroscopy for mechanistic insight Theo Tanner University of York, UK Investigating redox activity and photosensitivity of koneramines for imaging and therapeutic applications Suchismita Ghosh Indian Institute of Technology, Kanpur, India From waste electronic equipment to homogeneous gold catalysts Sean McCarthy Imperial College London, UK A circular approach to Si-based polymers: polymerising and depolymerising using an iron β-diketiminate catalyst Mirela Johnson University of Bath, UK and Monash University, Australia From recovered metal waste to a promising catalyst for C-H functionalisation and C-N amination Khairil Jantan Imperial College London, UK

P23

P24

P25

P26

P27

P28

P29

Solvent extraction of rhodium using amines and amides Andrew Carrick University of Edinburgh, UK

P30

Selective separation of light rare-earth elements by supramolecular encapsulation and precipitation Joseph O’Connell-Danes University of Edinburgh, UK Insertion of alkynes into a Cu–Al bond and functionalisation to a copper acyl Caitilín McManus University of Oxford, UK

P31

P32

Group 13 metathesis: a route to group 13 multiple bonds Ella Rice University of Edinburgh, UK

P33

Variable and efficient synthesis of new tetra-substituted pentalenide ligands Niko Jenek University of Bath, UK Interfacial photoelectrochemistry as a promising route for organic synthesis Ayman Mohammed University of York, UK

P34

P35

BODIPY Ligands in ruthenium-based CO probes Gregor Ekart Imperial College London, UK

P36

Developing stepwise catalysis for the construction of functional fluorinated molecules via a bridging nitrogen ruthenium precursor Aidan Carr University of York, UK Crystallography as a tool in elucidating activation modes of boron Lewis acid catalysts with nitrogen-containing substrates Yara van Ingen Cardiff University, UK Fast and bright phosphorescence from linear gold complexes with diamidocarbene ligands Charlotte Riley University of Manchester, UK Targeted, stimuli-responsive nanogels for atherosclerosis imaging and therapy Yu Qin Imperial College London, UK Reeling them in: Ph 2 PSiMe 3 fosters low temperature, acid-free growth of ever larger InP nanocrystals Theodore Anthony Gazis Keele University, UK Interfacial design strategies for selective electrocatalytic CO 2 reduction through control of proton coupled electron transfer Xinlei Zhang University of York, UK Peptides for targeted delivery of Pt(IV) Pro-Drugs in the treatment of rare cancers Jevon Marsh University of Oxford, UK

P37

P38

P39

P40

P41

P42

P43

Probing the speciation and electronic structure of organozinc reagents using X-ray spectroscopy Lewis Parker University of Reading, UK Engineered supramolecular metallogels as luminescent 3D-printable materials Tomas Gudmundsson Trinity College Dublin, Ireland N-Heterocyclic carbene stabilised fluoroboranes for 18 F PET Imaging: promoter- free labelling and water stability Anna Booth University of Oxford, UK Artificial metalloenzymes Inspired by lytic polysaccharide monooxygenases Sarah Robinson University of Nottingham, UK

P44

P45

P46

P47

Tunable porous materials for targeted pest control Joshua Nicks University of Bath, UK

P48

De novo designed copper coiled-coils as MRI contrast agents Giulia Molinaro University of Birmingham, UK Coordination nanostructures for high performing solar cells Kezia Sasitharan Newcastle University, UK

P49

P50

The development of organometallic platinum(iv) complexes with tridentate ligands Yana Dikova Durham University, UK

P51

Synthesis and electrolyte design for sodium-ion batteries Darren Ould Cambridge University, UK

P52

Selective chelation of magnesium ions using phosphinate-containing ligands Christopher Hogg University of Durham, UK Histidine brace copper proteins (lytic polysaccharide monooxygenases): structure, oxygen activation and biotechnological applications Azza Hassoon University of Szeged, Hungary

P53

P54

Towards single-crystal-to-single-crystal transformations in organometallic chemistry via copper(i) complexes Chloe Johnson University of York, UK Group 9 catalysts for the preparation of N-substituted polyaminoboranes Mathew Cross The University of York, UK Development of an acyclic bifunctional chelator for imaging and therapy of prostate cancer using copper-64 Veronika Rosecker King’s College London, UK Synthesis and reactivity of phospha-stannenes and -germenes Matthew Reveley University of Oxford, UK

P55

P56

P57

P58

Using MRI as a kinetic tool Viliyana Lewis University College London, UK

P59

Local structural distortions and reduced thermal conductivity in Ge-substituted chalcopyrite Sahil Tippireddy University of Reading, UK

P60

De novo designed ruthenium coiled coil metallopeptides Joseph Phillips University of Birmingham, UK

Isolation of monomeric copper(II) phenolateselenoether complexes and their electrocatalytic hydrogen gas evolution activity Aditya Upadhyay 1 , Sangit Kumar 2 1 Indian Institute of Science Education and Research Bhopal, India, 2 Bhopal, India Characterized for the first time from copper(I) phenanthroline and various substituted ortho- bisphenylselenidephenol chelating ligands. The synthesized complexes exhibit Jahn–Teller distortion in their geometry and varied from distorted square planar to distorted octahedral by varying substituents in the bis- selenophenolate ligand. The synthesized complexes electrocatalyze the hydrogen evolution reaction (HER) with a faradaic efficiency of up to 89%, and it was observed that the distorted square pyramidal geometry is the optimum geometry for the maximum efficiency of these copper complexes. References 1. A. Upadhyay, H. Meena, R. K. Jha, Kanika, and S. Kumar, Dalton Trans. 2022, 51 , 7284–7293.

P01

Coordination chemistry of azophosphines Emma Jordan, Andrew R. Jupp University of Birmingham, UK

Azophosphines are a class of compound possessing the RN=N–PR’ 2 functionality. Although first reported in the 1970s (where R = alkyl), 1 compounds bearing the N=N–P functionality have remained relatively unexplored. More recently, Cummins and co-workers reported the 1,3-dipolar cycloaddition reactions of MesN=N–PA (Mes = mesityl and A = anthracene), with concomitant loss of anthracene. 2

Figure 1. A) Photolabile anthracene-substituted azophosphine reported by Cummins and co-workers [2]; B) Generic structure for our targeted stable azophosphines; C) Monodentate azophosphine complex; D) Bidentate azophosphine complex. Recent work in the Jupp group has focused on the synthesis and properties of novel azophosphines (where R = aryl and R’ is a non-labile aryl or alkyl group). We are currently exploring the coordination chemistry of these azophosphines when employed as ligands in transition metal complexes. 3 References 1. Kroner, J., Schneid, W., Wiberg, N., Wrackmeyer, B., Ziegleder, G., Chem. Soc. Faraday Trans ., 1978 , 74 , 1909−1919. 2. Riu, M. Y., Transue, W. J., Rall, J. M., Cummins, C. C., Am. Chem. Soc ., 2021 , 143 , 7635-7640. 3. Rong, M., Holtrop, F., Slootweg, J. C., Lammertsa, K., Chem. Rev ., 2019 , 380 , 1-16.

P02

Synthesis and reactivity of bis(diphenylphosphino)amine-type ligand cobalt complexes Adam Carrick , Dr. Andrei S. Batsanov, Dr. Dmitry Yufit, Dr. Philip W. Dyer Durham University, UK The coordination chemistry of bis (phosphino) amine-type ligands (RN(PR’ 2 ) 2 ) with cobalt(II) has been scarcely studied, 1 despite the potential application of these complexes as pre-catalysts for olefin oligomerisation (by analogy with their chromium(III) analogues). 2 Here, we show for the first time that ionic cobalt(II) complexes ( e.g. C1a , {E = CH}, X = Cl, Scheme 1 ) containing a Co 2 X 6 2– anion (X = Cl, Br, I, Scheme 1 ) are formed on reaction with RN(PPh 2 ) 2 when R does not contain a suitably positioned Lewis base. In contrast, zwitterionic cobalt(II) complexes ( e.g. C2a , X = Cl, Scheme 1 ) are afforded when R bears a suitably located donor group. Complexes C2a-c are believed to form through initial in situ formation of C1a-c {E = N}, which undergoes intramolecular complexation to afford C2a-c . Operation of this latter pathway is supported by the reaction of C1b ({E = CH}, X = Br) with pyridine, which yields C3 ( Scheme 1 ). Both C1a-c and C2a-c have multiple cobalt(II) centres and so would be difficult to use as well-defined pre-catalysts. Hence, complexes C4a-b , containing only the cationic cobalt(II) centre present in C1a-c and C2a-c , have been synthesised and reduced to form cationic cobalt(I) complexes C5a-b (the active species for olefin oligomerisation 3 ). Finally, zwitterionic cobalt-hydride complex C7 with an octahedral cationic cobalt(III) centre has been synthesised, providing a route for the selective addition of a hydride ligand to the cationic cobalt(II) of C2a .

Scheme 1. The synthesis of complexes C1a-f (where C1d-f are in situ intermediates in the synthesis of C2a-c), C2a-c, C3, C4a-b, C5a-b and C6 from compounds L1 and L2. References

1. C. Fliedel et al ., Inorg. Chem ., 2015 , 54 , 6457 – 6559. 2. S. Sa et al ., J. Mol. Catal. A: Chem ., 2013 , 378 , 17 – 21. 3. M. Gray et al ., ACS Catal ., 2020 , 10 , 4337 – 4348.

P03

New weakly coordinating chiral anions and their application in enantioselective catalysis Richard Collins and Mark Chadwick Imperial College London, UK Common organometallic catalysts are generally ionic, where the anionic-stabilisation can affect the reaction outcome. 1 The application of weakly coordinating chiral anions (WCCAs) in asymmetric counter-anion directed catalysis (ACDC) has the potential to improve current industrial procedures, reducing waste and increasing the sustainability of pharmaceutical reactions through enantioselective synthesis. We have synthesised a family of alkali metal (Na), alkali earth metal (Mg), and ammonium (Et 3 NH, s Bu 3 NH) and imidazolium salts of a new WCCA of the formula [B(C 6 F 5 )(C 6 Cl 5 ){3,5-(CF 3 ) 2 C 6 H 3 }{3,5-(Cl) 2 C 6 H 3 }] - . These have been benchmarked for their capabilities by comparing to known ACDC reactions as well as asymmetric hydrogenation reactions. 2 References

1. Riddleston, I. M. et al., Angew. Chem. Int. Ed. , 2018 , 57, 13982-140242- 2. R. J. Phipps, G. L. Hamilton, F. D. Toste, Nat. Chem. , 2012 , 4, 603-614

P04

New layered vanadium oxychalcogenides Nicola Kelly, Simon J. Clarke University of Oxford, UK

Layered cuprates such as YBa 2 Cu 3 O 7- x exhibit unconventional high-temperature superconductivity as a result of the CuO 2 square planes within their crystal structures. Recently, superconductivity has been discovered in the oxypnictides BaTi 2 Bi 2 O and BaTi 2 Sb 2 O which contain “anti-CuO 2 ” transition metal-oxide square layers, i.e. Ti 2 O [1]. Doping of these materials on the Ba site enhances T c [1], which led researchers to investigate other ways to apply chemical pressure to these systems. As such, three vanadium oxychalcogenides containing a V 2 O square net were reported, with the general formula A V 2 Ch 2 O where A is Rb or Cs and Ch is S, Se or Te, Fig. 1 [2-4]. The materials contain vanadium of intermediate valency on a single crystallographic site, producing metallic conductivity and temperature-independent paramagnetism. Here we report the synthesis and characterisation of six further compounds in this structural family, extending it to include A = K for the first time, Fig. 2 .

Fig. 1. Crystal structure of AV2Ch2O oxychalcogenides, space group P4/mmm. The V2O square net is the anti-type of the CuO2 planes in high-temperature superconductors.

Fig. 2. Lattice parameters of AV2Ch2O as a function of A and Ch ionic radii. References 1. T. Yajima. Titanium Pnictide Oxide Superconductors. Condens . Matter 2 , 4 (2017)

2. H. Lin et al . Structure and physical properties of CsV 2 Se 2- x O and V 2 Se 2 O. Phys . Rev . B 98 , 075132 (2018) 3. M. Valldor et al . Bad-Metal-Layered Sulfide Oxide CsV 2 S 2 O. Eur . J . Inorg . Chem . 2016 , 23 (2016) 4. A. Ablimit et al . Weak metal-metal transition in the vanadium oxytelluride Rb 1−δ V 2 Te 2 O. Phys . Rev . B 97 , 214517 (2018)

P05

Tuning magnetism and superconductivity in nickel- and cobalt- based chalcogenides Ludmila Babicova, Prof Simon Clarke University of Oxford, UK The discovery of high-temperature superconductivity in La(O,F)FeAs has sparked renewed interest in intermetallics bearing the square anti-fluorite layers of M 2 X 2 (M = transition metal, X = pnictide or chalcogenide), since this is where superconductivity is believed to occur.The tetragonal FeSe, composed of anti-fluorite layers of Fe 2 Se 2 , has been found to be superconducting at 8K.Upon insertion of an alkali metal into this structure, a new phase – A Fe 2 Se 2 – emerges, with an increased superconducting transition temperature of 30K. A Fe 2 Se 2 belongs to the 122 family of iron-based superconductors, adapting a versatile ThCr 2 Si 2 -type structure, which has been known to demonstrate interesting magnetic phenomena.In this research, we are exploring the magnetic regions of nickel and cobalt-based 122 phases, which adapt the ThCr 2 Si 2 -type structure. The solid solutions of KNi 2-x Co x Se 2 and RbNi 2-x Co x Se 2 are both particularly interesting in terms of the magnetic states present in the members of their respective members; KNi 2 Se 2 is superconducting, while KCo 2 Se 2 is ferromagnetic, and the middle member – KNiCoSe 2 – shows antiferromagnetic behaviour. RbNi 2 Se 2 is a new, unreported phase and is an antiferromagnet, while RbNiCoSe 2 and RbCo 2 Se 2 are both ferromagnets. Therefore, our study shows the tuning of magnetism as a function of composition across the solid solution series of KNi 2-x Co x Se 2 and RbNi 2-x Co x Se 2 . References 1. Shatruk, M. Solid State Chem. Soc. 2019 , 272 , 198-209 2. Zhou, G. et al. 2016 , Appl. Phys. Lett. 108 . 3. Neilson, J. R., McQueen, T. M., Llobet, A., Wen, J. & Suchomel, M. R. Phys. Rev. B - Condens. Matter Mater. Phys. 2013 , 87 , 1–11. 4. Lei, H. et al. 2014 , J. Phys. Condens. Matter 26 . 5. Zhang, P. & Zhai, H. F., 2017 , Condens. Matter 2 , 1–14

P06

Solid-state preparation of single-phase Na 2 Zr 2-x Si 2 PO 12-2x solid electrolyte for na-ion solid-state batteries Ademola Adetona 1,2 , Dr Ge Wang 3 , Dr. Brant Walkley 2 , Prof. Ian Reaney 2 1 University of Lagos, UK, 2 University of Sheffield, UK, 3 University of Manchester, UK Na-ion solid-state batteries are promising large-scale energy storage systems due to the ubiquity and cost of sodium compounds. Na Super-Ionic CONductor (NASICON) has been widely studied; to date, researchers have not been able to prepare a phase pure Na x+1 Zr 2 Si x P 3-x O 12 with compositions invariably containing the ZrO 2 secondary phase. Solid-state methods have been used to prepare a single-phase Na 3 Zr 2-x Si 2 PO 12-2x . Density, morphology, and electrical conductivity of the phase pure Na 3 Zr 2-x Si 2 PO 12-2x are explored and compared with Na 3 Zr 2 Si 2 PO 12 (ZrO 2 second phase). References 1. X. Zeng et al. , “Commercialization of Lithium Battery Technologies for Electric Vehicles,” Adv. Energy Mater. , vol. 9, no. 27, pp. 1–25, 2019. 2. Y. Ding, Z. P. Cano, A. Yu, J. Lu, and Z. Chen, “Automotive Li-Ion Batteries: Current Status and Future Perspectives,” Electrochem. Energy Rev. , vol. 2, no. 1, pp. 1–28, 2019. 3. T. Placke, R. Kloepsch, S. Dühnen, and M. Winter, “LiLithium-lithium metal, and alternative rechargeable battery technologies: the odyssey for high energy density,” J. Solid State Electrochem. , vol. 21, no. 7, pp. 1939–1964, 2017.

P07

Synthesis of size-controlled iron oxide nanocubes for MPI-MFH applications Stanley Harvell-Smith, Nguyen T. K. Thanh UCL, UK Magnetic particle imaging (MPI) is a new tracer-based modality which has emerged as a promising tool for many therapeutic and diagnostic applications. 1 Standardly, the tracers employed by MPI are superparamagnetic iron oxide nanoparticles (SPIONs). MPI implements a gradient field with strong gradients and weak field strengths, and the non-linear magnetic response of these SPIONs to the field is detected directly for image generation. Overall performance and imaging quality is greatly influenced by the magnetic properties of the SPION implemented. By improving the properties of SPIONs through tailoring of their physical and chemical characteristics, including the iron oxide core size and shape, it is possible to significantly improve the sensitivity and imaging resolution of MPI. These particles can also be optimised for improved performance in specific MPI applications. The application of interest here is MPI in combination with magnetic fluid hyperthermia (MFH), called MPI-MFH. This refers to MFH performed using the MPI gradient system which permits localised heat deposition to a desired region in biological tissue, mitigating some of the issues with standard MFH application paradigms. The aim is to optimise single-core superparamagnetic iron oxide nanocubes (IONCs) towards both MPI, and MPI-MFH application. Due to their lower spin disorder at the surface and smaller surface anisotropies, IONCs have a greater overall performance in terms of saturation magnetisation and magnetic susceptibility compared to equivalent spherical SPIONs. 2 The effect of changing the core size of spherical SPIONs on MPI performance and sensitivity is well-documented with monodisperse single-core SPIONs having an improved MPI performance up to a magnetic core diameter of ~ 25 nm. 3 With this in mind, an array of IONCs with sizes smaller than 25 nm were synthesised. For good MPI-MFH performance, the nanoparticle must demonstrate impressive MPI spatial resolutions, so heat can be localised more specifically using the MPI gradient field system, and heating performance, individually. Reaction parameters in a thermal decomposition process were altered to obtain decanoic acid-coated magnetite IONCs. In all syntheses, there is clear formation of majority cubic shapes with narrow size distributions. The MFH properties have been measured for the largest and smallest synthesised IONCs. The heating performance for the 7 nm IONCs was poor, with an intrinsic loss parameter (ILP) value of just 0.17 nHm 2 /kg. The ILP value was much larger for the 24 nm IONCs, at 2.71 nHm 2 /kg. The 24 nm size of our IONCs is also close to the optimal size of ~25 nm for MPI, indicating potential application in MPI, and because of the good heating properties, MPI-MFH also. References 1. Harvell-Smith, L. D. Tung, and N. T. K. Thanh, Nanoscale , Advance Article, 2022. 2. M. Bauer,S. F. Situ,M. A. Griswold,and A. C. Samia, Nanoscale , 2016, 8 , 12162-12169 3. W. Tay, D. W. Hensley, E. C. Vreeland, B. Zheng, and S. M. Conolly, Biomed. Phys. Eng. Express , 2017, 3 , 035003.

P08

Design of aluminium precursor compounds for metal thin films deposition Shreya Mrig, Caroline Knapp UCL, UK The developing field of printed electronics has expanded considerably in the last decade, with this market expected to be valued at $300 billion by 2030. This growing area of research, which includes devices such as sensors, displays, integrated circuits, etc., is seeing a push towards faster, cheaper and environmentally friendly manufacturing processes that make use of flexible and renewable substrates. Inkjet printing is a fast and low-cost method of manufacturing that has displayed prominence as an alternative to traditional manufacturing techniques. To capitalize on this technique, suitable metal inks that allow deposition of conductive metals at low temperatures are crucial. Metal-organic decomposition (MOD) inks are one such example of metal inks that have exhibited the ability to deposit metals at low temperatures. Thus, the use of the inkjet printing process with a focus on MOD inks presents extensive potential for the deposition of conductive metal features onto low-cost substrates such as paper and plastic. To date, there has been little research into aluminium MOD ink chemistry, with previous work focusing only on a few different amine-stabilised aluminium hydride compounds to deposit aluminium metal. This work presents a more synthetically driven approach to aluminium precursor development using thiourea compounds as ligands. Although, thiourea ligands are common in transition metal complexes, there is a paucity of literature surrounding aluminium-thioureide complexes. This research presents several novel tris-ligated aluminium thoureide complexes displaying octahedral geometry around the aluminium centre. Novel complexes have been fully characterised by a range of techniques including SCXRD, NMR, MS and EA. Additionally, the thermal decomposition of these novel precursors has been investigated using thermogravimetric analysis (TGA) to gauge their suitability as MOD precursors. Also, using thermal analysis data, we can analyse trends such that better performing precursors (those that decompose more cleanly and at lower temperature, whilst maintaining good stability) containing different ligand systems can be predicted and subsequently synthesised. Additionally, proof of concept depositions of aluminium films on various forms of paper have been discussed. References 1. Kamyshny and S. Magdassi, Small , 2014, 10 , 3515–3535. Dungchai, O. Chailapakul and C. S. Henry, Anal. Chem. , 2009, 81 , 5821–5826. 2. B.-J. de Gans, P. C. Duineveld and U. S. Schubert, Adv. Mater. , 2004, 16 , 203–213.S. P. Douglas, S. Mrig and C. E. Knapp, Chemistry – A European Journal , 2021, 27 , 8062–8081. 3. M. Lee, S.-Y. Choi, K. T. Kim, J.-Y. Yun, D. S. Jung, S. B. Park and J. Park, Adv. Mater. , 2011, 23 , 5524–5528. 4. S. P. Douglas and C. E. Knapp, ACS Appl. Mater. Interfaces , , DOI:10.1021/acsami.0c05429. S. I. Sullivan, J. D. Parish, P. Thongchai, G. Kociok-Köhn, M. S. Hill and A. L. Johnson, Inorg. Chem. , 2019, 58 , 2784–2797.

P09

ImPAC: immobilised phosphines for applications in catalysis Jake Backhouse 1 , Dr Stephen Bennett 2 , Dr Stephen Poulston 2 , Dr Philip Dyer 1 1 Durham University, UK, 2 Johnson Matthey PLC, UK Rhodium-catalysed hydroformylation is an important industrial reaction for the production of aldehydes used as intermediates in the synthesis of detergent alcohols and surfactants. Current hydroformylation processes suffer from costly purification steps required to separate the aldehyde products and transition metal catalyst. A possible solution is the application of transition metal complexes immobilised onto solid oxide supports, hence allowing separation via a simple filtration. One approach to this immobilisation is to use an appropriately-functionalised diphosphine ligand to tether the catalyst to an insoluble support such as silica. To this end, bidentate phosphines functionalised with an Si(OMe) 3 silica tethering group have been synthesised with varying electronic and steric properties and P^P bite angles. The P V selenide derivatives of these compounds have been prepared in order to investigate the Lewis basicity of the phosphine lone pairs via an assessment of their | 1 J SeP | coupling constants. The electronic demands of the phosphine moieties of the bidentate ligand ensembles were probed through FT-IR spectroscopic analysis of their [Mo(CO) 4 (P^P)] complexes. The phosphorus compounds were then immobilised on AEROPERL 300/30 silica and characterised by solid state MAS 29 Si and 31 P NMR spectroscopies to determine their binding mode to silica. The coordination chemistry of the compounds with Rh I precursors Rh(acac)(CO) 2 and Rh(acac)(COD) was also explored in preparation for future work to investigate silica-immobilised rhodium complexes for application as heterogenised hydroformylation catalysts.

References 1. Piras, B. Powietzka, F. Wurst, D. Neumann-Walter, H. Grützmacher, T. Otto, T. Zevaco and O. Walter, Catal. Lett., 2013, 143 , 673 – 680. 2. J. Sandee, J. N. H. Reek, P. C. J. Kamer and P. W. N. M. van Leeuwen, J. Am. Chem. Soc ., 2001, 123 , 8468 – 8476. 3. M. S. Rodrigues, R. M. B. Carrilho and M. M. Pereira, Eur. J. Inorg. Chem ., 2021, 2021 , 2294 – 2324.

P10

Insights into the formation of ruthenium hydrides via Fischer carbene intermediates Katie Grant and Guy Lloyd-Jones University of Edinburgh, UK Olefin metathesis is a key C-C bond formation reaction and is used in a variety of fields including natural product synthesis, fine chemical synthesis and API synthesis. 1 However, progress has been hampered in part due to unwanted side reactions such as isomerisation. 1 Research has shown the culprit for these side reactions is a ruthenium hydride species. 2 Once identified it was realised that if the formation of such a species could be controlled then there was scope for tandem catalytic reactions in which metathesis could be followed by isomerisation or hydrogenation. 3,4 This work focusses on elucidating the mechanism of one such synthesis developed by Nishida and co-workers. 5 In their work they developed a route based on a previously reported preparation by Grubbs and Louie in which a Grubbs metathesis catalyst was reacted with ethyl vinyl ether to form a Fischer-type carbene, 2 subsequently this was thermally decomposed to form the ruthenium hydride species of interest, RuHCl(CO)(L) 2 . Nishida’s methodology replaced the ethyl vinyl ether with vinyloxy trimethylsilane, allowing for lower reaction temperatures and greater selectivity for isomerisation. Using in situ 1 H NMR and kinetic modelling, reaction constants, key reaction parameters and intermediate species have been determined. 6 From these results a preliminary mechanism has been proposed. References 1. S. Higman, J.A.M. Lummiss, D.E. Fogg, Angew. Chem. Int. Ed ., 2016 , 55 , 3552-3565. 2. Louie, R. H. Grubbs, Organometallics, 2002 , 21 , 2153-2164. 3. E. Fogg, E. N. dos Santos, Coord. Chem. Rev. , 2004 , 248 , 2365-2379.

4. E. Sutton, B. A. Seigal, D. F. Finnegan, M. L. Snapper, J. Am. Chem. Soc., 2002 , 124 , 13390-13391. 5. Arisawa, Y. Terada, K. Takahashi, M. Nakagawa, A. Nishida, J. Org. Chem. , 2006 , 26 , 4255-4261. 6. M. Grant, G. C. Lloyd-Jones, unpublished results, 2022.

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Zintl clusters, multifunctional ligands for homogeneous catalysts Oliver Townrow 1 , Andrew S. Weller 2 , Jose M. Goicoechea 1 1 University of Oxford, UK, 2 University of York, UK Zintl clusters are attractive supports for transition metal/ligand fragments. Such complexes can be viewed as molecular models for main group - transition metal alloys (TMMGAs) which have recently received significant attention as molten-state high temperature alkane dehydrogenation catalysts. 1 However, poor solubility and low yielding synthetic protocols have precluded the use of transition metal Zintl clusters in small molecule activation and catalysis. 2 We have recently reported the synthesis and reactivity of the first catalytically active Zintl cluster: Rh(COD) Ge 9 (Hyp) 3 ( 1 ) (COD = 1,5-cyclooctadiene; Hyp = Si(SiMe 3 ) 3 ) which is soluble in aliphatic hydrocarbons and can be isolated in high yields (>92%). 3 Complex 1 catalyzes the hydrogenation of COD and cis -cyclooctene. Ligand substitution of 1 gives access to clusters of form Rh(L)Ge 9 (Hyp) 3 , which feature coordinatively unsaturated rhodium centers and are active in H–H and C–H bond activation processes. 4 1 is also shown to accommodate multiple metal fragments, acting as a platform for the synthesis of homo- and hetero-multimetallic transition metal Zintl clusters. These results highlight that the [Ge 9 (Hyp) 3 ] − cage can act as a versatile, multifunctional ligand for constructing defined molecular models of TMMGAs.

Figure 1. Rh(COD)Ge9(Hyp)3(1) as a versatile, stable platform for catalysis and derivatisation. References 1. D. C. Upham, V. Agarwal, A. Khechfe, Z. R. Snodgrass, M. J. Gordon, H. Metiu and E. W. McFarland, Science , 2017, 358 , 917–921.R. 2. J. Wilson, B. Weinert and S. Dehnen, Dalton Trans. , 2018, 47 , 14861–14869. 3. O. P. E. Townrow, C. Chung, S. A. Macgregor, A. S. Weller and J. M. Goicoechea, J.Am. Chem. Soc. ,2020, 142 , 18330– 18335. 4. O. P. E. Townrow, S. B. Duckett, A. S. Weller and J. M. Goicoechea, Chem. Sci. , 2022, 13 ,7626–7633.

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Heterobimetallic complexes supported by a multidentate tripodal ligand Benedict Thompson, Till Neumann, Rebecca A. Musgrave King's College London, UK Cooperative effects between two or more metal centres are of particular interest within the context of multiple electron transfer in small-molecule activation and catalysis. 1,2 The synthesis of bimetallic complexes pairing a first row transition metal ion (M 1 ) and a lanthanide metal ion (M 2 ) within a tripodal Schiff base ligand framework will be described (Figure 1). The structural characteristics of these complexes have been determined by single crystal X-ray diffraction and 1 H NMR spectroscopy. The optical and electrochemical properties have been probed by UV- Vis and IR spectroscopies and cyclic voltammetry respectively (with support from DFT calculations) with a view to determining the degree of interaction between (1) the two metal centres and (2) the metal centres and the ligand.

Figure 1: General structure of heterobimetallic complexes discussed. References 1. Q. Zhu, W. Fang, L. Maron and C. Zhu, Acc. Chem. Res , 2022, 11 , 1718-1730. 2. J. Campos, Nat. Rev. Chem. , 2020, 4 , 696–702.

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Magnetically - triggered protein release using iron oxide core - PNIPMAM shell nanoparticles Rajat Sharma , Victor Chechik University of York, UK Superparamagnetic iron oxide nanoparticles (IONPs) are well known for biomedical applications due to their inherent magnetic behaviour and biocompatibility 1 . IONPs can be heated by an alternating current magnetic field (ACMF) and the heat generated can be used in magnetic hyperthermia and drug delivery applications. IONPs functionalised with temperature-responsive polymers present a potential combination for drug delivery and release 2,3 . Poly(N-isopropylmethacrylamide) (PNIPMAM) is such a polymer that is soluble in water below its lower critical solution temperature (LCST ~ 45˚C) but it collapses and becomes insoluble above LCST. Here, the synthesis of Fe 3 O 4 core-PNIPMAM shell nanoparticles is reported along with their potential use as a protein carrier in-situ (Figure 1). Present study could be useful in understanding protein-IONPs interactions which is an essential criterion in designing any protein carrying cargo.

Figure 1: Schematic illustration of the protein delivery from the Fe 3 O 4 core-PNIPMAM shell nanoparticles using magnetic heating as a trigger. References 1. A. Hervault and N. T. K. Thanh, Nanoscale , 2014, 6 , 11553-11573. 2. S. Kurzhals, R. Zirbs and E. Reimhult, ACS Appl. Mater. Inter. , 2015, 7 , 19342-19352. 3. M. Walker, I. Will, A. Pratt, V. Chechik, P. Genever and D. Ungar, ACS Appl. Nano Mater ., 2020, 3 , 5008-5013

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Magnesium-stabilised transition metal formyl complexes: structures, bonding, and ethenediolate formation Joseph M. Parr and Mark R Crimmin Department of Chemistry, Imperial College London, UK. jmp20@ic.ac.uk, @josephmparr

Transition metal formyl complexes are important intermediates in the reduction of carbon monoxide (CO) and carbon dioxide (CO2). For example, transition metal formyl species have been proposed as key intermediates in the reduction of CO with H2 to form linear alkanes in the Fischer–Tropsch (F–T) process. Despite their importance, the detailed study of transition metal formyl complexes has been hampered by their low stability. Herein we report the first comprehensive series of crystallographically characterised transition metal formyl complexes. In these complexes, the formyl ligand is trapped as part of a chelating structure between a transition metal (Cr, Mn, Fe, Co, Rh, W, and Ir) and a magnesium (Mg) cation. Calculations suggest that this bonding mode results in significant oxycarbene-character of the formyl ligand. Further reaction of a heterometallic Cr–Mg formyl complex results in a rare example of C–C coupling and formation of an ethenediolate complex. DFT calculations support a key role for the formyl-intermediate in ethenediolate formation. These results show that well-defined transition metal formyl complexes are potential intermediates in the homologation of carbon monoxide.

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Exploring the synthesis and structure of copper(II)-oxo clusters Tom Barnes, Sebastian Pike University of Warwick, UK Copper(II)-oxo clusters are a relatively unexplored class of copper coordination compounds. Some Cu(II)-oxo clusters have gained research attention through their applications as models for enzyme active sites, [1] catalysts, [2] single molecule magnets, [3] and as anion encapsulating agents. [4] Cu(II) is an intriguing target for making metal- oxo clusters of different shapes and sizes due to its flexible coordination geometries and Jahn-Teller effects. [5] The synthesis of Cu(II)-oxo clusters is currently poorly understood, with synthetic routes relying on slow crystallisation processes. [6] We have explored using the controlled hydrolysis of a smaller, pre-hydrolysis , cluster (i.e. no oxide/hydroxide ligands) to optimise, and control, their synthesis. We have also used techniques such as X-ray diffraction, electrochemistry, UV-vis and X-ray photoelectron spectroscopies to explore the physical and electronic structures of these clusters. An understanding of these properties will guide potential applications, such as for use as photocatalysts or as precursors for functional materials. References 1. S. Grundner, M. A. C. Markovits, G. Li, M. Tromp, E. A. Pidko, E. J. M. Hensen, A. Jentys, M. Sanchez-Sanchez and J. A. Lercher, Nature Communications , 2015, 6 , 7546 2. H.-X. Li, Z.-G. Ren, D. Liu, Y. Chen, J.-P. Lang, Z.-P. Cheng, X.-L. Zhu and B. F. Abrahams, Chemical Communications , 2010, 46 , 8430-8432 3. S. K. Langley, L. Ungur, N. F. Chilton, B. Moubaraki, L. F. Chibotaru and K. S. Murray, Chemistry – A European Journal , 2011, 17 , 9209-9218 4. G. Mezei, P. Baran and R. G. Raptis, Angewandte Chemie International Edition , 2004, 43 , 574-577 5. A. Kondinski and K. Y. Monakhov, Chemistry – A European Journal , 2017, 23 , 7841-7852 6. T.-F. Liu, T. C. Stamatatos, K. A. Abboud and G. Christou, Dalton Transactions , 2010, 39 , 3554-3556.

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Aikinite as a potential thermoelectric material with ultra-low thermal conductivity Shriparna Mukherjee 1 , Virginia Carnevali 2 , David J Voneshen 3 , Marco Fornari 2 , Anthony V. Powell 1 , Paz Vaqueiro 1 1 University of Reading, UK, 2 Central Michigan University, USA, 3 Rutherford Appleton Laboratory, UK Intrinsically low thermal conductivity is a favorable parameter for efficient thermoelectric materials 1 . Moreover, for the widespread implementation of thermoelectric (TE) energy recovery, it is important to identify tellurium- free materials with good TE performance. In this context, sulfide minerals 2 such as tetrahedrites and colusites are attracting much interest. Here, we present work on the mineral aikinite, CuPbBiS 3 , which adopts a structure closely related to that of Bi 2 S 3 , which itself exhibits promising TE properties 3 . Aikinite samples were prepared by mechanical alloying followed by heat treatment. Rietveld refinement of powder neutron diffraction data, collected on POWGEN (SNS, ORNL), indicate that the isoelectronic Pb 2+ and Bi 3+ cations are fully ordered. Moreover, Cu + and Pb 2+ have larger atomic displacement parameters than Bi 3+ . The thermal conductivity, measured on hot-pressed pellets, exhibits a remarkably low value of ca. 0.54 W m -1 K -1 at room temperature. The calculated vibrational density of states exhibits Einstein-like phonon modes at 100 cm -1 , attributed to Cu + vibrations, and low- frequency optical phonon modes below 50 cm -1 (at ~ 4.5 meV), arising from Pb 2+ vibrations. The experimentally determined vibrational phonon density of states is in very good agreement with calculations. Inelastic neutron scattering data, collected on LET (ISIS), confirms the presence of low-energy vibrational modes (~ 4 meV), which are likely to be responsible for the ultralow thermal conductivity. The temperature dependence of the low-energy Pb 2+ vibrational mode is consistent with anharmonic behaviour, while the Cu + Einstein-like mode softens markedly with increasing temperature. The results of this work will be presented here. References

1. T. Ghosh et al ., J. Am. Chem. Soc. 144 , 23 (2022), 2. A.V. Powell, J.Appl.Phys. 126 , 100901 (2019). 3. Ohmasa and Nowacki, Zeitschrift für Kristallographie - Crystalline Materials, 132 ,71 (1970).

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Advanced oxidation of calmagite using in situ generated hydrogen peroxide catalyzed by manganese(II) ions and bicarbonate Ye Cao and Tippu Sheriff Queen Mary University of London, UK The discharge of azo dyes, that possess the stable –N=N– unit, are threatening the aquatic ecosystem since they are toxic to organisms and difficult to degrade by traditional water treatment technologies. 1 An in situ advanced oxidation process is proposed here to address the water pollution caused by azo dye discharge, which involves the formation of [Mn II T 2 ] 6- (where TH 2 = 1,2-dihydroxybenzene-3,5-disulfonate, disodium salt (Tiron), Fig. 1(a)) as the catalyst for the in situ generation of H 2 O 2 , and bicarbonate as a co-catalyst for the oxidative degradation of Calmagite (CAL, 2-hydroxy-1-(2-hydroxy-5-methylphenylazo)-4-naphthalenesulfonic acid, Fig. 1(b)), which is a typical azo dye, at room temperature. A one-eighth-lives method 2 was applied to investigate the effect of pH, buffer type and Mn 2+ concentration on the degradation of CAL. Mn(IV)=O, was found to be the main reactive species, while percarbonate () and hydroxyl radicals () were the subsidiary reactive species for CAL degradation (Fig. 2). Using HPLC/ESI-MS, the degradation intermediates of CAL were identified as 1-amino-2-naphthol- 4-sulfonate ion, 1-amino-2-naphthol-4-sulfinic ion, 1-amino-2-naphthol and 1-nitroso-2-naphthol. This work demonstrates that the in situ generation of H 2 O 2 system catalyzed by Mn 2+ can efficiently degrade CAL under ambient conditions in aqueous solution. 3 In addition, we have showed this system can be used as an anti-corrosion and anti-bacteria formulation by the consumption of dissolved O 2 and the in situ generation of H 2 O 2 . We are currently investigating the use of Cu II as the catalyst in activating the in situ generated H 2 O 2 for the degradation of more stable pollutants like 4,4'-(Hexafluoroisopropylidene)diphenol (BPAF, Fig. 1(c)). This work will include an investigation of the degradation mechanism, the degradation kinetics, the degradation pathways, the concentration variation of reactive oxidant species such as , and the influence of co-existing anions such as chloride, sulfate, and nitrate on degradation. Preliminary results are promising and will be presented in the poster.

Fig 1. The Chemical structures of (a) Tiron, (b) Calmagite and (c) BPAF

Fig 2. The in situ generation of H 2 O 2 and its use for the oxidative degradation of CAL References 1. X. Meng, B. Scheidemantle, M. Li, Y.-y. Wang, X. Zhao, M. Toro-González, P. Singh, Y. Pu, C. E. Wyman, S. Ozcan, C. M. Cai and A. J. Ragauskas, ACS Omega , 2020, 5 , 2865-2877. 2. J. Peng, X. Lu, X. Jiang, Y. Zhang, Q. Chen, B. Lai and G. Yao, Chem. Eng. J. , 2018, 354 , 740-752. 3. Y. Cao and T. S. Sheriff, Chemosphere , 2022, 286 , 131792.

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Synthesis, reactivity and decomposition of aryl phospha-enolates Stephanie Urwin, Jose M. Goicoechea University of Oxford, UK Lithium enolates are integral synthetic intermediates with wide ranging applications. A key characteristic which drives the diverse reactivity of the enolate functionality is the 1,3-delocalisation of the negative charge upon deprotonation of the β-carbon atom. Replacing this carbon with phosphorus to create a phospha-enolate, unlocks a higher potential for delocalisation through the accessible lone pair on the heteroatom. Here, we present the preparation of unsupported lithium phospha-enolates, and explore their diverse reactivity and thermal decomposition (Scheme 1). On reaction with aryl lithium reagents, the C≡P bond of tri(isopropyl)silyl phosphaethynolate is reduced, and is accompanied by a 1,2-silyl migration to form [RP=C(Si i Pr 3 )OLi] 2. Initially dimeric in both the solid and solution state, phospha-enolate aggregation can be modulated by the addition of coordinating bases such as THF or crown ethers, and in the monomeric form delocalisation of negative charge across the PCO unit increases. Silylation with Me 3 SiCl affords the corresponding silyl enol ether, which reduces the extent of delocalisation, and provides a synthetic route to the heavier potassium phospha-enolate. Salt metathesis reactivity is also seen with (IDipp)AuCl, initially forming a gold phosphide with the less bulky phospha- enolate, followed by an unexpected entropically-driven rearrangement to an unusual η 1 -phosphaalkene structure.

Scheme 1. Summary of phospha-enolate chemistry. On addition of water, the lithium phospha-enolate is protonated to RP=C(Si i Pr 3 )(OH). For the sterically smaller example (R = Mes), this phospha-enol rapidly tautomerises to the corresponding acyl phosphine MesP(H)C(Si i Pr 3 ) (O), which on heating extrudes CO. In contrast, bulkier phospha-enol (R = Mes*) is stable to rearrangement at room temperature and thermally decomposes to RH and i Pr 3 SiPCO. Evidently, the chemistry of these lithium phospha-enolates is dependent on the steric environment and directed by a freely migrating silyl group.

P19

A coumarin-porphyrin break-apart probe for heme oxygenase-1 Edward R. H. Walter 1,2 , Ying GE 2 , Saul M. Cooper 1,2 , Justin C. Mason 2 , Joseph J. Boyle 2 , Nicholas J. Long 1 1 Imperial College London, UK, 2 National Heart and Lung Institute, Imperial College London, UK Heme oxygenase-1 (HO-1) is an important enzyme in vascular biology that is primarily responsible for the regulation of cytotoxic free heme. 1 Heme catabolism is a regiospecific three-step process that requires molecular oxygen, NADPH and cytochrome p450 reductase, to form biliverdin and carbon monoxide. 2 HO-1 overexpression is commonly associated with a number of cardiovascular and neurogenerative diseases, and, therefore, has the potential to act as a diagnostic / prognostic marker in this regard. However, to-date HO-1 has been somewhat overlooked as a potential marker for vascular disease. We shall describe our recent work toward the design, synthesis, photophysical and biological characterisation of the first known chemical probe to report on HO-1 activity. 3,4 Probe Fe–L 1 was designed to utilise the regiospecific HO-1- catalysed porphyrin degradation of heme and ‘break-apart’, perturbing the efficient Fluorescence Resonance Energy Transfer (FRET) mechanism from a coumarin donor to a porphyrin accepter fluorophore ( Figure 1A ). Analysis of HO-1 activity in Escherichia coli lysates overexpressing HO-1, determined that porphyrin degradation was regiospecific at the α-position following incubation with NADPH, resulting in the formation of coumarin 1 and a 6-fold increase in fluorescence ( Figure 1C ). Through the analysis of Fe–L 2 ( Figure 1B ), it was confirmed that close structural analogues of heme are required to maintain HO‑1 activity. 3,4 It is anticipated that this proof-of-concept study will act as a foundation to develop new red-shifted probes to report on HO-1 activity in the near future.

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Figure 1. (A) HO-1 catabolism of Fe–L 1 and (B) control porphyrin Fe–L 2 . (C) The change in coumarin fluorescence at 383 nm of Fe–L 1 and Fe–L 2 in E. coli lysates with and without incubation with NADPH. 3,4 References 1. Yuan, X.; Rietzschel, N.; Kwon, H.; Nuno, A. B. W.; Hanna, D. A.; Phillips, J. D.; Raven, E. L.; Reddi, A. R.; Hamza, I. Proc. Natl. Acad. Sci. U. S. A , 2016 , 113, 5144 2. Ortiz De Montellano, P. R. Curr. Opin. Chem. Biol, 2000 , 4, 221. 3. Walter, E. R. H.; Ge, Y.; Mason, J. C.; Boyle, J. J.; Long, N. J. J. Am. Chem. Soc , 2021 , 143, 6460. 4. Boyle, J. J.; Long, N. L.; Walter, E. R. H.; Ge, Y.; Mason, J. C.; WO2022/101635 A1.

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