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Optimum resolution data of X-ray powder diffraction for 7-amino desacetoxy cephalosporanic acid(7-ADCA) were collected from an X ′ Pert Pro MPD diffractometer with the setup of 0.01°/s and 0.01° per step. Indexing to the crystal system and searching space group from the diffraction data were conducted by means of the computational crystallography method. The pilot crystal models of 7-ADCA were then refined by Rietveld method to obtain the exact three-dimensional structure. The results show that the crystal structure of 7-ADCA is monoclinic, space group P2 1 with unit cell dimensions a=13.50 Å, b=6.01 Å, c =5.91 Å, α= γ =90.00°, β =101.96°, Z=2and V =469.10 Å 3 . The fraction coordinate of each atom in the unit cell is well located and reported.

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