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Abstract Multiplex imaging in the second near‐infrared window (NIR‐II, 1000–1700 nm) provides exciting opportunities for more precise understanding of biological processes and more accurate diagnosis of diseases by enabling real‐time acquisition of images with improved contrast and spatial resolution in deeper tissues. Today, the number of imaging agents suitable for this modality remains very scarce. In this work, we have synthesized and fully characterized, including theoretical calculations, a series of dimeric Ln^III/Ga^IIImetallacrowns bearing Ru^IIpolypyridyl complexes,LnRu‐3(Ln=Y^III, Yb^III, Nd^III, Er^III). Relaxed structures ofYRu‐3in the ground and the excited electronic states have been calculated using dispersion‐corrected density functional theory methods. Detailed photophysical studies ofLnRu‐3have demonstrated that characteristic emission signals of Yb^III, Nd^IIIand Er^IIIin the NIR‐II range can be sensitized upon excitation in the visible range through Ru^II‐centered metal‐to‐ligand charge transfer (MLCT) states. We have also showed that these NIR‐II signals are unambiguously detected in an imaging experiment using capillaries and biological tissue‐mimicking phantoms. This work opens unprecedented perspectives for NIR‐II multiplex imaging using Ln^III‐based molecular compounds.