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In a typical experiment, a 1:1 mixture of PgC6 (3) and pyrene (4 a) or 1-bromopyrene (4 b) was dissolved in hot acetonitrile/ water (≈5:2 by volume). The solution was sonicated for around 10 min and then left to stand overnight. Slow evaporation of the solvent resulted in the formation of large single crystals of 5 a or 5 b, respectively, that were suitable for X-ray diffraction studies. Data for both crystal structures were collected on a Bruker SMART 1000 CCD diffractometer. CCDC 282089 and 282090 contain the supplementary crystallographic data for this paper. These data can be obtained free of charge from The Cambridge Crystallographic Data Centre via www.ccdc.cam.ac.uk/data_ request/cif.
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31044438194
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note
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2 = 0.2913 for 1507 parameters and two restraints.
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31044453832
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note
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2 = 0.3222 for 1627 parameters and one restraint. The structure showed significant disorder around the 1-bromopyrene molecules and this was modeled as satisfactorily as possible. The structure of the 1-bromopyrene derivative differs from that of the pyrene derivative by one water of crystallization. See Supporting Information for details of the asymmetric unit and figures of the extended structure.
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