Composite materials of quantum particles (Q‐particles) arranged in layers within crystalline powders of π‐conjugated, rodlike dicarboxylic acids are reported. The synthesis of the composites, either as three‐dimensional crystals or as thin films at the air–water interface, comprises a two‐step process: 1) The preparation of the Cd salts 6 (Cd), 8 (Cd) or Pb salts 6 (Pb), 8 (Pb) of the oligo(p‐phenyleneethynylene)dicarboxylic acids 6 (H), 8 (H), in which the metal ions are arranged in ribbons and are separated by the long axis of the organic molecules, as demonstrated by X‐ray powder diffraction analysis of the solids and grazing incidence X‐ray diffraction analysis of the films on water. 2) Topotactic solid/gas reaction of these salts with H2S to convert the metal ions into Q‐particles of CdS or PbS embedded in the organic matrix that consists of the acids 6 (H) and 8 (H). These hybrid materials have been characterized by X‐ray photoelectron spectroscopy and transmission electron microscopy.