Structural inhomogeneities in crystals of YBa2Cu3O75 are characterized using high resolution x-ray diffraction. Rocking curves and a high resolution specular radial scan show features indicating that the crystals are not truly "single." The high resolution radial scan of a crystal that had a superconducting transition width of only one-half Kelvin, as determined by ac susceptibility, and appeared to be free of gross defects, when examined with conventional x-ray diffraction techniques, shows a distribution in the c-axis lattice parameter. These results suggest that crystals with sharp transitions should be carefully examined for the presence of structural anomalies which might influence the superconductive properties.High temperature superconductors (HTS) still present many puzzles to researchers studying their various physical properties. Many experimental studies exploring the nature of both vortex dynamics and the mechanism of superconductivity have revealed unusual behaviors which have spawned, or apparently confirmed, many theories. The results of several studies have suggested the presence of inhomogeneities in polycrystalline samples,1 crystals2'3'4'5'6'7'8'9 and films10 of YBa2Cu3O7 (YBCO). When coupled with the behaviors mentioned above, this suggests that some, if not all, of the new phenomena may be extrinsic. Such sensitivity of superconductive properties to sample imperfections is to be expected due to the short superconducting coherence lengths of the materials, their low carrier concentrations, and the strong dependence of those carrier concentrations on the oxygen content of a sample. i1 has shown theoretically that such sample inhomogeneities can explain many of the properties of these systems and has suggested that they are responsible for the high Ta's. In this report we show that "single" crystals with various oxygen content have rocking curves with structure. Furthermore, we directly show, using high resolution x-ray diffraction, that a crystal with a sharp superconducting transition, and which appears to be homogeneous with conventional x-ray diffraction measurements, in fact contains several distinct domains with different c-lattice parameters and rocking curves with significant structure.As is well known, the superconducting properties of YBCO are strongly affected by the oxygen composition and the details of the oxygen ordering. In general, superconductivity occurs for < 0.6 with T increasing to 93 K as decreases from 0.6 to 0. Under certain processing conditions12'13'14'15'16'17'18'19 the curve of superconducting transition temperature, T, versus has several plateaus, one near ö =0 corresponding to T 90 K (the ortho-I phase) and others with lower Ta's, the most studied being the one near = 0.5 with a T of 60 K (the ortho-Il phase). These different superconducting transitions, which can be quite sharp, have been attributed to the ordering of the chain oxygens. This argument is supported by x-ray, neutron, and electron diffraction measurements.If the chains are not ordered, then T still de...