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00925njm 22002777a 4500 dc Domingo de la Rubia, Estela de author García Moreno, Gregorio José author Folcia, César L. author Ortega, Josu author Etxebarria, Jesús author Coco Cea, Silverio author 2023 This work reports an uncommon modulation of columnar segregation of metal–organic triphenylene liquid crystals by blending two structurally dissimilar metallomesogens that can self-associate through complementary electron donor–acceptor interactions. The constituent molecules are cis-[PtCl2(CNR)2] (CNR = 2-(6-(4-isocyanophenoxy)hexyloxy)-3,6,7,10,11-pentakisdodecyloxytriphenylene) that displays an organic/inorganic segregated columnar mesophase and [PtCl2(Bipy)] (Bipy = didodecyl 2,2′-bipyridyl-4,4′-dicarboxylate) that shows a lamellar mesomorphism. The phase diagram of this system was constructed using polarized optical microscopy (POM), differential scanning calorimetry (DSC), and X-ray scattering data. The phase diagram corresponds to a typical binary system with an intermediate compound (in this case a supramolecular aggregate) of stoichiometry [PtCl2(CNR)2]/2[PtCl2(Bipy)], which is maintained in solution. This species shows an unusual columnar mesophase formed by the stacking of alternating organic/inorganic fragments. Quantum chemical calculations show that the columnar structure is mainly supported by complementary π electron donor–acceptor interactions between each triphenylene group of the isocyanide complex and a platinum-bipyridine molecule. This induces the elimination of the organic/inorganic columnar segregation of the isocyano parent component and constitutes an unconventional example of modulation of organic/inorganic segregation in columnar mesophases by the intercalation of metal complexes into hexaalkoxytriphenylene stacks. Crystal Growth Design 2023, vol. 23, n. 9, pp. 6812–6821 1528-7483 https://uvadoc.uva.es/handle/10324/61501 10.1021/acs.cgd.3c00660 6812 9 6821 Crystal Growth & Design 23 1528-7505 Materials science Química inorgánica Modulating organic/inorganic segregation in columnar mesophases