We have studied the geometry of the high-coverage Rh(111) + (2 x 2)-3CO str
ucture by surface x-ray diffraction. Analysis of the in-plane data set reve
als three evenly separated CO molecules per (2 x 2) unit cell. The evaluati
on of the crystal truncation rods shows that one CO molecule resides in an-
on-top site while the other two CO molecules occupy hollow sites. The inten
sity modulations of the out-of-plane fractional order rods provide geometri
cal information about distances between the C and O atoms and on the buckli
ng of the CO overlayer. [S0163-1829(99)10107-3].