The polyoctahedral silsesquioxane (POSS) 1,3,5,7,9,11,13,15‐octaphenylpentacyclo[9.5.1.1 3,9 .1 5,15 .1 7,13 ]octasiloxane (octaphenyl‐POSS)

Solvent‐free single crystals of 1,3,5,7,9,11,13,15‐octaphenylpentacyclo[9.5.1.1 3,9 .1 5,15 .1 7,13 ]octasiloxane (abbreviated as octaphenyl‐POSS), C 48 H 40 O 12 Si 8 , were obtained by dehydration/condensation of the tetrol Si 4 O 4 (Ph) 4 (OH) 4 . The powder pattern generated from the single‐crystal data matches well with the experimentally measured powder pattern of commercial octaphenyl‐POSS. The geometry of the centrosymmetric molecule in the crystal was compared with that in the gas phase, and had shorter Si—O bond lengths and a broader range of Si—O—Si bond angles. The average Si—O bond length [1.621 (3) Å], and Si—O—Si and O—Si—O bond angles [149 (5) and 109 (1)°, respectively] were within the same range measured previously for octaphenyl‐POSS solvates.