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Instruments / Technical Area	Publication Details	Published	Actions
I19-Small Molecule Single Crystal Diffraction	Cyclotriveratrylene-tethered trinuclear palladium( ii )–NHC complexes; reversal of site selectivity in Suzuki–Miyaura reactions Jonathan M. Fowler , Edward Britton , Christopher M. Pask , Charlotte E. Willans , Michaele J. Hardie Dalton Transactions 48, 14687 - 14695 DOI: 10.1039/C9DT03400E Diamond Proposal Number(s): [15059] Show Abstract ▼ Abstract: The trinuclear complexes [{PdI2(pyCl)}3(L1)] C1 and [{PdI2(pyCl)}3(L2)] C2, where pyCl = 3-chloropyridine, L1 = methyl(cyclotriguaiacylenyl)methylbenzimidazol-2-ylidene and L2 = benzyl(cyclotriguaiacylenyl)methylbenzimidazol-2-ylidene, each feature three palladium N-heterocyclic carbene (NHC) centres tethered onto a host-type cyclotriguaiacylene scaffold. Crystal structures of different solvates of complex C1 reveal different host–guest motifs including intra-cavity binding of dioxane guests concomitant with intramolecular halogen bonding interactions of C1. Mononuclear NHC analogues of C1 and C2, namely [PdI2(pyCl)(L3)] C3 and [PdI2(pyCl)(L4)] C4, where L3 = (3-chloropyridyl)-1-(2-methoxyphenyoxy)methyl-3-methylbenzimidazol-2-ylidene and L4 = (3-chloropyridyl)-1-(2-methoxyphenyoxy)methyl-3-benzylbenzimidazol-2-ylidene, were also synthesised and their crystal structures determined. Complexes C1–C4 are competent catalysts for Suzuki Miyaura cross-coupling, and interestingly exhibit a switch in the normal regioselectivity observed for reactions of 2,4-dibromopyridine with aryl boronic acids, usually C2-selective, yielding C4-arylated product preferentially over C2-arylated product.	Oct 2019
I19-Small Molecule Single Crystal Diffraction	Metallo-cryptophane cages from cis -linked and trans -linked strategies Nikki J. Cookson , Jonathan M. Fowler , David P. Martin , Julie Fisher , James J. Henkelis , Tanya K. Ronson , Flora L. Thorp-Greenwood , Charlotte E. Willans , Michaele J. Hardie Supramolecular Chemistry 113, 1 - 12 DOI: 10.1080/10610278.2017.1355055 Diamond Proposal Number(s): [10334] Show Abstract ▼ Abstract: Trigonal bipyramidal metallo-cage species [Pd3(dppp)3(L)2]∙6OTf (where dppp = bis(diphenylphosphino)propane, OTf = triflate and L is tris(iso-nicotinoyl)cyclotriguaiacylene (L1) or tris(fluoro-iso-nicotinoyl)cyclotriguaiacylene (FL1)) have been characterised in solution to exist predominantly as the anti-isomers. The crystal structure of [Pd3(dppp)3(FL1)2]∙6OTf, however, was found to be the achiral syn-isomer. The complex [Pd3Cl3(L2)2] (where L2 = tris(methylbenzimidazolyl)cyclotriguaiacylene) is a trans-linked M3L2 cage, observed by mass spectrometry and in the solid state as the anti-isomer. Ligand L2 also forms a 1:1 co-crystal with cyclotriguaiacylene.	Jul 2017

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