The structure and morphology of vinylidene chloridemethyl acrylate copolymers were studied using small-angle and wide-angle x-ray scattering. Long period increased with comonomer concentration for compressionmolded films crystallized at the same temperature. An increase in the “a” dimension of the unit cell was noted for the “as polymerized” powder as comonomer content increased. Sequence distribution information obtained from the instantaneous copolymer composition equation agreed well with the observed powder data. No such trend was observed for melt-crystallized films, possibly because of a greater restriction on crystallization and a lower level of crystallinity within these samples.