Additionally, we obtained SC-XRD data for the [2]staffane byproduct -SF5-BCP-BCP-Cl (3) -to compare alongside 2 as well as the previously published structure of its SF5-Ph-Ph-Cl congener (5). In this case, both transannular C•••C distances in the bicyclopentane rings of 3 (1.835(4) Å and 1.839(4) Å) are notably longer than that of 2. Alternatively, the conduit C-C bonds connecting the ring structures in 3 and 5 are similar in length; this makes the composite effect of replacing both Ph rings in the biphenyl array with BCP rings a ~27% reduction in distance between the terminal carbon atoms. Also, similar to 2 vs. 4, the C-Cl bond in 3 is longer than in 5, and average S-Feq distances are ~1.58-1.60 Å in each case. However, the S-Fax bond in 3 is ~2% longer than in 5.