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We have recently demonstrated that a heavily boron-doped diamond (BDD) can be categorized as a material with two-dimensional (2D) misfit layer structure [1]. Boron atoms, incorporated in a diamond unit cell in definite positions, form nanosheets at boron concentration >4×1018 cm−3 and bilayers when concentration of boron atoms is ~2×1020 cm−3 along which there is a metallic conductivity. These data require a new insight on the semiconducting properties of boron-doped diamond. The emergence of a new shallow acceptor level, associated with the formation of 2D layers opens the way of the creation of new high-speed electronic devices. Metallic conductivity of the layers in the near future can solve the problem of contacts in the construction of power electronic devices. BDD periodic structure with alternating layers behaves similarly to the multilayer mirror and X-ray interferometer that paving the way to design the new X-ray optics. Designing of these devices requires more detailed studies of BDD structure. This work presents the results of BDD crystal structure investigations in a wide range of boron content by high resolution X-ray diffraction, X-ray topography and Raman spectroscopy. 1. Polyakov et al. Nanoscale Research Letters (2016) 11:11 DOI 10.1186/s11671-015- 1215-6