| Abstract: | The crystal structure of the ambient‐pressure phase of vanadyl pyrophosphate, (VO)2P2O7, has been precisely determined at 120 K from synchrotron X‐ray diffraction data measured on a high‐quality single crystal. The structure refinement unambiguously establishes the orthorhombic space group Pca21 as the true crystallographic symmetry. Moreover, it improves the accuracy of previously published atomic coordinates by one order of magnitude, and provides reliable anisotropic displacement parameters for all atoms. Along the a axis, the structure consists of infinite two‐leg ladders of vanadyl cations, (VO)2+, which are separated by pyrophosphate anions, (P2O7)4?. Parallel to the c axis, the unit cell comprises two alternating crystallographically inequivalent chains of edge‐sharing VO5 square pyramids bridged by PO4 double tetrahedra. No structural phase transition has been observed in the temperature range between 300 and 120 K. |
