AbstractAn X‐ray structure analysis was performed on single crystals of the cycloalkane (CH2)36. The lattice belongs to the space groupAaand is arranged in layers. The unit cell has the dimensions α = 1,033 nm,b= 0,824 nm,c= 4,22 nm, β = 107, 1° and contains four molecules. The molecules consist of two stretched stems which are linked by sharp folds at each end. The folds have the conformation …t(g g t g g) t… lying parallel to theb‐axis. Raman measurements suggest that the stems are slightly twisted. A comparison of the homologous series (CH2)n,n= 36, 48, 60, and 72 using X‐ray powder methods showed that the (CH2)36‐structure, including the fold conformation, is also representative for the longer chai