Short-range lattice superstructures have been studied with high-energy x-ray
diffuse scattering in underdoped, optimally doped, and overdoped (Y,Ca)Ba2Cu3O6+x. A new four-unit-cell superstructure was observed in
compounds with x∼0.95. Its temperature, doping, and material dependence
was used to attribute its origin to short-range oxygen vacancy ordering, rather
than electronic instabilities in the CuO2 layers. No significant diffuse
scattering is observed in YBa2Cu4O8. The oxygen superstructures must
be taken into account when interpreting spectral anomalies in (Y,Ca)Ba2Cu3O6+x