The Construction of Homochiral Lanthanide Quadruple‐Stranded Helicates with Multiresponsive Sensing Properties toward Fluoride Anions

A series of unique homochiral lanthanide tetranuclear quadruple‐stranded helicates have been self‐assembled controllably by using the intrinsic advantages of chiral bridging ligands, ( S )‐H 2 L and ( R )‐H 2 L , and lanthanide ions with high coordination numbers. The self‐assembly process of these chiral helicates not only ensures the structural stability and quadruple‐stranded feature of lanthanide cluster in the solid state and solution, but also achieves effective transfer and amplification of the chirality code from the ligand to a higher supramolecular level. Moreover, through using optical rotation, circular dichroism spectra analysis, and luminescence measurements, we demonstrate that these chiral lanthanide helicates could serve as sensitive and multi‐responsive sensors to recognize and detect F − anions based on the change of chiral signal and NIR luminescence simultaneously, which represents a meaningful exploration for developing functional lanthanide‐based polynuclear clusters.