Films of the pyramidic liquid crystals hexakis(nonanoyloxy)tribenzocyc
lononene and hexakis(pentadecanoyloxy)tribenzocyclononene spread at th
e air-water interface have been studied using grazing incidence X-ray
reflectrometry. Both compounds exhibit a transition from an expanded p
hase to a condensed phase. In the expanded phases as well as in the co
ndensed phase of hexakis(pentadecanoyloxy)tribenzocyclononene the mole
cules lie flat on the surface. The density and the thickness measured
in the condensed phase of hexakis(nonanoyloxy)tribenzocyclononene are
only consistent with an ''edge-on'' configuration. This latter phase i
s metastable with respect to the growth of three-dimensional domains w
hose thickness, orientation, and lattice parameters are determined and
compared to bulk lattice parameters.