pathways with maxima at sites 6(c) and 9(d) (R3m notation). Best least-squares fit for Sr 2+ ions following noncentrosymmetric space group R3m; occupations of successive 6(c), 9(d), 6(c), ... sites in approximate ratios 1"1:0.65, respectively. Sr 2+ distribution at 6(c) sites is fitted to a vibrational model involving third-rank cumulants (~'ijk's). Column oxygen 0(5) occupies a 3(b) site. The refined x value in the structural formula is 0-87 (2), indicating a 37% substitution of Al (2)by Mg. The centrosymmetric spinel-block framework is retained from Na ÷/?"-alumina.Introduction. In the present study, single crystals of Sr 2+ fl"-alumina have been prepared by ion exchange from Na + ff'-alumina crystals. The ionic conductivity of Sr 2+ ff'-alumina has been reported by Dunn & Farrington (1980). It was found to resemble closely the conductivity behaviour of Ba 2+, Ca 2+ and Cd 2+ ff'-aluminas. The mean ionic distributions and shortrange order are found to be significantly different, for example, in Ba z+ /?"-alumina (Thomas, Ald6n, McIntyre & Farrington, 1984) and Ca z+ ff'-alumina (Ald+n, . The purpose here is to determine the detailed distribution of Sr 2+ ions in the conduction plane of Sr 2+ /?"-alumina, as part of a project aimed at understanding the ionic-conductivity mechanism for divalent ions in/?"-alumina. The SrZ+-ion radius (1.18 A) is intermediate between that for Ca 2+ (1.00/k) and Ba 1+ (1.35/k) (Shannon, 1976).Experimental. Single crystals of Sr 2+ fl"-alumina were prepared by ion exchange from Na + fl"-alumina crystals grown at 1963-1998 K. The exchange was performed in a Sr(NOa)2:SrC12 melt (mol ratio 47:53) at 823 K for 24 h. The remaining Na + content was shown to be <0.1%, using a 22Na radioactive isotopic form of Na + fl"-alumina to monitor the exchange (Farrington & Dunn, 1982). Intensity measurements made on a triangular platelet with well defined faces (max./min. dimensions: 0.130/ 0.048 mm respectively). Intensity data recorded using a Nonius CAD-4 automatic diffractometer, controlled by a PDP8/A computer. Integrated intensities of-h+k+l = 3n reflections measured using an 09-20 step-scan technique, 50 steps. Total of 2392 reflections of type +h,k,l measured out to sin0/2 = 0-950/k -~. Instrumental stability and crystal setting checked by monitoring the intensities of three test reflections: no significant variation throughout the data collection. The crystal could be confirmed through its systematic absences (-h+k+l 4: 3n in the hexagonal cell) to retain the R3m space-group symmetry of Na + fl"-alumina. Cell parameters determined from a least-squares fit of 25 0 angles in the range 0-20 ° measured on the diffractometer for the same crystal as was used for the data collection. Intensity data corrected for background, Lp and absorption effects (assuming composition removed, leaving 1874 for the refinements. A crude picture of the Sr 2+ distribution in the conduction plane was obtained following a refinement of the scale factor, using the positions of the Al(Mg) and O atoms taken from the ...