Development of the fourth-generation synchrotron radiation sources (SRS) and X-ray free-electron lasers (XFEL) with extremely high brightness and high power calls for the use of materials that are resilient to extreme thermal and radiation loading. Diamond is the best material for the fabrication of X-ray optics elements suitable for working under these conditions. [1][2][3][4] Up to now, the synthetic single-crystal diamonds, grown by the temperature gradient method at high temperature and high pressure (HPHT), have been mainly used. However, HPHT diamonds may contain metallic impurities because they are created using catalysts. The typical catalysts being used are iron, aluminum, nickel, and cobalt. [5,6] This can lead to degradation of X-ray optics when exposed to bright XFEL and SRS beams. Single-crystal diamonds produced by low-pressure chemical vapor deposition (CVD) are more attractive for the fabrication of X-ray optics because they contain fewer metallic impurities. Nevertheless, the use of CVD single-crystal diamonds for this application has not been successful due to significant lattice stresses and the presence of defects such as dislocations and small-angle boundaries. [7,8] The requirements for the perfection of a single-crystal diamond suitable for X-ray optics are as follows: crystal lattice deformation Δd/d is %10 À7 ; no dislocations in the effective area of a crystal designed for use in SRS or XFEL optics; and the full width at half maximum (FWHM) of Bragg reflection of a double-crystal rocking curve (RC) is almost theoretical; impurity concentration is the order of 10 16 cm À3 ; transverse dimensions are up to 10 Â 10 mm 2 with thickness from 20 μm up to 5 mm. [9,10] In this work, we demonstrate the large-size diamond single crystals grown by CVD, with structural perfection not inferior to that of