Flux growth and crystal structure of pyromorphite

Single crystals of pyromorphite, Pb5(PO4)3Cl, were grown by standard flux growth technique with excess lead chloride used as the flux. Pyromorphite was first prepared by heating an intimate mixture of lead hydrogen phosphate and lead chloride in the molar ratio 6:4 at 100 degrees C for 1 h. A mixture of 60 wt% of pyromorphite and 40 wt% of lead chloride was heated at 850 degrees C for 15 h and then cooled at the rate of 3.4 degrees C/h. Hexagonal prismatic crystals of length 1 mm were obtained. The chemical composition has close to the theoretical value. The crystal is hexagonal, space group P6(3)/m with a = 9.9981(8), c = 7.344(1) A and Z = 2. The structure was refined to R = 0.058 and Rw = 0.053 with 502 independent reflections. The structure is in principal the same as that of barium chlorapatite; the chlorine ions occupy the (0, 0, 0) position.