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Diphenyliodonium cations were firstly introduced into halobismuthate system to synthesize two new hybrids, i. e. (DPI)4(Bi2I10) (1) and (DPI)4(Bi2Br10)·H2O (2) (DPI = diphenyliodonium). Two hybrids are isostructures containing (Bi2X10)4- halobismuthate dimmers and diphenyliodonium cations. Hypervalent I(III)⋯X interactions and CH⋯X (XI, Br) hydrogen bonds stabilize the structures and contribute to...