The crystal structure of L-alanylglycine has been determined by X-ray diffraction. L-Alanylglycine crystallizes in the space group P21 with cell dimensions a= 5.283, b= 11.810, c= 5.510/~ andfl= 101-58 ° with Z=2. This non-centrosymnaetric structure was solved by the 'quadrant permutation' method. The structure is simple but interesting in that one proceeded from the collection of data to the correct solution with scarcely any human intervention. It was refined by three-dimensional anisotropic matrix least-squares analysis (block-diagonal approximation). A final R index of 0.047 for 586 observed reflexions was obtained. The molecules are held together by hydrogen bonds forming a three-dimensional network. The planes of the carboxyl and the amide groups are nearly perpendicular. The bond lengths and angles are in close agreement with the mean values proposed by Marsh & Donohue.
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