The efficient synthesis of all-cis -[5.5.5.5]fenestrane (2) from the r
eadily available intermediate 3 allowed the electron-diffraction analy
sis of 2. This structure analysis revealed long C-C bonds in the centr
al C(C)4 fragment and a twist-envelope conformation for the four cyclo
pentane substructures. The four bridgehead H-atoms are in a synclinal
rather than an ecliptic position with an approximate D2 Symmetry of 2.
Planarizing distortions are evident from the opposite bond angles at
the central C-atom being 116.2 +/- 0.5-degrees with the remaining four
being 103.7 +/- 0.2-degrees.