The crystalline structure of a C-60/C-70 membrane prepared by are original technique has been studied by x-ray diffraction and Raman spectroscopy. The effects of purification of the starting C-60/C-70 mixture to C-70 composition and of spatial separation of the C-60 and C-70 phases in the membrane have been revealed, The samples studied were established to have a composition gradient from C-60 to C-70. The main structure of the membrane is shown to be an fcc lattice with a = 14.308 Angstrom. (C) 1998 American Institute of Physics. [S1063-7834(98)04103-3].