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Single crystal synchrotron X-ray diffraction as a function of temperature andpressure has revealed a complex biphase mixture in superconducting FeSe. Basedon our experimental results we construct a phase diagram where structuralbehavior and superconducting properties of FeSe are found to be correlated. Weshow that below 6 GPa, where pressure promotes the superconducting criticaltemperature, the FeSe structure is composed of 2D layers of edge-shared FeSe4tetrahedra, while above 6 GPa the superconductivity is strongly suppressed onformation of a new orthorhombic polymorph characterized by a 3D network of facesharing FeSe6 octahedra. Therefore changes in topology and connectivity of theFeSe structure are found to be detrimental for superconductivity to exist. Thispreviously controversial crystal structure of the high pressure polymorph ofFeSe was also unambiguously determined. High pressure FeSe adopts anorthorhombic MnP-type structure (Pnma) which corresponds to a slightlydistorted hexagonal NiAs-type arrangement (P63/mmc). The structuraltransformation from the low- to high-pressure FeSe polymorph is first order innature and is manifested as antiparallel displacements within the Fe and Sesublattices.

Complex biphase nature of the superconducting dome of the FeSe phase diagram