Single-crystal x-ray diffraction and diffuse x-ray scattering measurements were performed on a crystal of the commensurate intergrowth compound of bis(methylthio)ethylenedithiotetrathiafulvalene (Cz TET-TTF) and golddi-iode. The first subsystem comprises of stacks along aq of planar Cq TET-TTF groups on a monoclinic lattice, with lattice parameters aq --7.540(2) A, bz --22.450(2) A. , cz --11. 674(1) A. , Pz --100.14(1)' and space group P2&/c. The second subsystem comprises of chains of AuI& parallel to az, but with a different periodicity az --4a&. Long-range order is only obtained along the chains, as concluded from the observation of diffuse planes of scattered x-ray intensity perpendicular to the stacking axis. Within these planes, there are intensity concentrations which occur as broad spots, the centers of which correspond to a reciprocal lattice b& --b&, c& -c, and a2 --5a& +~c&, which makes this a commensurate intergrowth compound.The spacegroup of the second subsystem is again P2q/c.
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