A synchrotron X-ray diffraction study of a single crystal of titanomagnetite shows that the cation distribution of Fe 2+ , Fe 3+ and Ti 4+ is of the inverse-spinel type. The valence-difference contrast (VDC) method of resonant scattering was applied at a wavelength of = 1.7441 Å (E = 7.1085 keV) within the pre-edge of the Fe K absorption spectrum, utilizing the large difference in the real part of anomalous scattering factors, between À7.45 and À6.50, for Fe 2+ and Fe 3+ , respectively. The most plausible atomic arrangement in Ti 0.31 Fe 2.69 O 4 obtained from our analysis is [Fe 3+ 1.00 ] A [Fe 3+ 0.38 Fe 2+ 1.31 Ti 4+ 0.31 ] B O 4 , where A and B in an AB 2 O 4type structure correspond to the tetrahedral and octahedral sites, respectively.This result suggests that titanomagnetite has the complete inverse-spinel structure continuously from the end-member of magnetite, even in the case of relatively high Ti content. The physical properties may be described by the Né el model, which claims that Fe 3+ preferentially occupies the tetrahedral site, within a Ti-poor half-region of the solid solution. Based on the ordering scheme the magnetic structure of titanomagnetite is considered to be analogous to that of magnetite. The combination of circularly polarized X-rays and a horizontal-type four-circle diffractometer used in this VDC technique has the advantage of increasing the experimental accuracy and freedom with the simultaneous reduction of experimental noise. research papers J. Synchrotron Rad. (2018). 25, 1694-1702 Maki Okube et al. Fe 2+ , Fe 3+ and Ti 4+ in titanomagnetite 1695 Figure 1 Crystal structure of titanomagnetite, showing A and B sites and oxygen atoms.