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Instruments / Technical Area	Publication Details	Published	Actions
I19-Small Molecule Single Crystal Diffraction	Evaluating iodine uptake in a crystalline sponge using dynamic X-ray crystallography William J. Gee , Lauren E> Hatcher , Christopher A. Cameron , Clare Stubbs , Mark R. Warren , Andrew D. Burrows , Paul R. Raithby Inorganic Chemistry DOI: 10.1021/acs.inorgchem.7b03218 Diamond Proposal Number(s): [13015] Show Abstract ▼ Abstract: The uptake of gaseous iodine into the crystalline sponge material [(ZnI2)3(tpt)2]·0.7triphenylene·0.3PhNO2·0.7C6H12 1 (tpt = 2,4,6-tris(4-pyridyl)-1,3,5-triazine) has been monitored by dynamic X-ray diffraction and thermogravimetric analysis. The X-ray analyses have enabled the location, quantity, uptake rate, and subsequent chemistry of the iodine upon inclusion into the pores to be determined. An uptake of 6.0 wt % (0.43 I2 per formula unit) was observed crystallographically over a period of 90 min before crystal degradation occurred. The included iodine molecules interact with the iodine atoms of the ZnI2 nodes at three different sites, forming coordinated I3– ions. The results contrast to recent observations on [(ZnI2)3(tpt)2] without the triphenylene guests which show the presence of I42– ions with low quantities of absorbed iodine.	Apr 2018
I19-Small Molecule Single Crystal Diffraction	Monitoring photo-induced population dynamics in metastable linkage isomer crystals: a crystallographic kinetic study of [Pd(Bu4dien)NO2]BPh4 Lauren E. Hatcher , Jonathan M. Skelton , Mark R. Warren , Clare Stubbs , Estelina Lora Da Silva , Paul R. Raithby Physical Chemistry Chemical Physics DOI: 10.1039/C7CP05422J Diamond Proposal Number(s): [8567, 9734, 13698] Open Access Show Abstract ▼ Abstract: We present a detailed kinetic study of photo-induced solid state linkage isomerism in the compound [Pd(Bu4dien)NO2]BPh4 (Bu4dien = N,N,N’,N’-tetrabutyldiethylenetriamine) using in-situ photocrystallographic techniques. We explore the key variables that influence the photoconversion and develop a detailed kinetic model for the excitation and decay processes and the temperature dependence of the conversion rates. We show that by varying the temperature the lifetime of the excited state can be varied over orders of magnitude, making these systems ideal test cases for the development of new time-resolved X-ray diffraction methods. The kinetic model is used to build a numerical-simulation tool, which we use to explore the practicalities of pump-probe single-crystal diffraction experiments with minute and second time-resolution.	Jan 2018

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