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Model intensity profiles have been obtained for biscarbonyl[ 14]annulene by convoluting the Mo Ka spectral distribution with two functions derived from experimental measurements at 16(1) K, up to 26Mo = 110°, of a spherical crystal mounted on a four-circle diffractometer equipped with the Samson low-temperature apparatus. The process includes accurate measurement of the inherent background, treatment of the profiles by numerical Fourier methods, and least-squares fitting. Owing to the instrumental configuration of the diffractometer used in this investigation, the first step of the process has required a careful determination of the X dependence of the background, besides the usual 26 dependence. Truncation losses for the crystal under study, evaluated for several scan ranges, are far larger than usually assumed or predicted.

Experimental Determination of Scan-truncation Losses from Low-temperature (16 K) Single-crystal X-ray Measurements