Rhodium‐Catalyzed Enantioselective Synthesis of Highly Fluorescent and CPL‐Active Dispiroindeno[2,1‐ <i>c</i> ]fluorenes

The enantioselective synthesis of chiral [7]-helical dispirodihydro[2,1-c]indenofluorenes (DSF-IFs) was achieved for the first time in good yields with high er values (er up to 99 : 1). crucial step whole reaction sequence intramolecular [2+2+2] cycloaddition tethered triynediols indenofluorenediols, which catalyzed by a Rh/SEGPHOS® complex. Further transformations led corresponding DSF-IFs. prepared helically DSF-IFs combine circularly polarized luminescence (CPL) activity (glum=∼10−3) exceptionally fluorescence quantum (up Φlum=0.97).