Phosphorus: New <i>in situ</i> powder data from large-volume apparatus

Abstract

Improved X-ray powder diffraction data for orthorhombic phosphorus, S.G. C mca (64) obtained in situ at synthesis conditions of 1.2 GPa and 1100 K, are described. Representative, as synthesized, data include 2.552 X , 3.320 4 , 2.595 3 , 5.191 2 , 1.630 2 , for least-squares unit-cell a =3.3182(6) Å, b =10.3744(18) Å and c =4.3227(9) Å. As an illustration of the quality of the data, the structure was solved from powder XRD and Rietveld refined to give a =3.3199(2) Å, b = 10.3678(4) Å, c =4.3154(2)Å, and V =148.535(12) Å 3 with the P atom on 8 f (1/2, y,z ) with y =0.1044(22) and z =0.9179(7).