Crystal and molecular structure of newly synthesized 2,3,2′,3′‐Bis{8″,11″‐dioxa[4.3.3]propella(3″,4″)}biphenyl

The title compound 5 was obtained from 2,2′,3,3′‐tetramethylbiphenyl in a multi‐step reaction sequence leading to the bis(propellane). X‐ray structure analysis proved the identity of bis(propellane). In the solid state the molecule possesses roughly a twofold symmetry axis perpendicular to the biphenyl bond. The conformation of the molecule is determined by a 53.5(1)° torsional angle between the biphenyl planes. The propellane bond is parallel to the phenyl plane in both symmetric parts of the molecule, what implies a boat conformation of the fused six‐membered rings.