Single crystals of dipyrrin proligands H2L3∙2HBr and H2L3′∙2HBr∙(solvent)n were prepared as follows. Dipyrrin proligand H2L3 (0.84 mmol, 1 eq) was dissolved in methanol (50 ml) by adding 48% HBr aq. (3.7 mmol, 4.4 eq). Then, diethyl ether (200 ml) was poured into the solution, giving a microcrystalline powder of H2L3∙2HBr. Its single crystals suitable for x-ray diffraction analysis were grown by vapor diffusion of diethyl ether into an ethanol solution of H2L3∙2HBr. A similar method was applied to H2L3′, and single crystals of H2L3′∙2HBr∙(solvent)n were obtained by vapor diffusion of diethyl ether into a methanol solution of H2L3′∙2HBr. Diffraction data were collected at 93 K on a Rigaku Saturn 724 (VariMax dual) diffractometer with multilayer mirror monochromated MoKα radiation using Crystal Clear (Rigaku). The structures were solved by means of the direct method using SIR92 and refined by the full-matrix least squares using SHELXL-97. Because of severe disorder, solvent molecules in the crystal structure of H2L3′∙2HBr∙(solvent)n were removed using the SQUEEZE routine of the PLATON software when necessary, after which the structures were refined again using the data generated. CCDC 1867482 [for H2L3′∙2HBr∙(solvent)n] and 1867483 (for H2L3∙2HBr) contain the supplementary crystallographic data for this paper. These data may be obtained free of charge from The Cambridge Crystallographic Data Centre via www.ccdc.cam.ac.uk/data_request/cif.

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