The sectorial structure of semiconductor single‐crystal diamond grown at high pressure and temperature was considered. Influence of crystal structure on shape of IR‐absorption maps and photoluminescence glow were studied. The distribution of boron impurity and its concentration in the areas which belonging to different growth sectors were measured. The analysis of the effect of the conditions of type IIb crystal growth at HPHT on their structure was performed, conditions for getting the most homogeneous samples were defined. (© 2014 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)