An ultrahigh vacuum chamber has been developed for structural analysis of adsorbed films and single‐crystal surfaces using synchrotron x‐ray diffraction. It is particularly well suited for investigations of physisorbed and other weakly bound films. The chamber is small enough to transport and mount directly on a standard four‐axis diffractometer and can also be used independently of the x‐ray diffractometer. A low‐current, pulse‐counting, low‐energy electron diffraction/Auger spectroscopy system with a position‐sensitive detector enablesinsitucharacterization of the film and substrate while the sample is located at the x‐ray scattering position. A closed‐cycle He refrigerator and electron bombardment heater provide controlled substrate temperatures from 30 to 1300 K. The chamber is also equipped with an ion sputter gun, a quadrupole mass spectrometer, and a gas handling system. Details of the design and operation of the instrument are described. To demonstrate the performance of the instrument, we present some preliminary results of a study of Xe physisorbed on the Ag(111) surface.