Inorganic-organic hybrid materials with small unit cells are difficult to characterize, but a study in Nature now shows how serial femtosecond X-ray crystallography can determine their structure
+ 1 reflections. Data collected at atomic resolution in the upcoming LCLS runs may yield further insights.Benzeneselenol , diphenyl ditelluride , silver oxide , silver powder , and thiophenol were used as received from Sigma Aldrich. Microcrystalline silver benzeneselenolate and its homologues silver benzene thiolate and silver benzenetellurolate were prepared in an approach adapted from our earlier report.
For small-scale reactions producing mithrene and thiorene, 1 equivalent of silver oxide was placed in a 1-dram glass vial with 1.5 equivalents of benzeneselenol or benzenethiol. Reactions can be run solvent-free or in 1 ml of isopropanol. We find the addition of isopropanol is useful for subsequent sample recovery. The vial was sealed and heated in an oven to 70 °C.
Product purity was assessed by taking aliquots of the crystals from a slurry and depositing them on silicon substrates until dry. Laboratory powder X-ray diffraction experiments were sufficient to match powder patterns of earlier reports and to determine whether there was any silver oxide remaining. Images of all three benzenchalcogenolate crystals were imaged using a field-emission scanning electron microscope at an accelerating voltage of 1–5 kV.
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