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Based on the results from previous high‐pressure experiments on the gadolinite‐type mineral datolite, CaBSiO 4 (OH), the behavior of the isostructural borates  β ‐HfB 2 O 5  and  β ‐ZrB 2 O 5  have been studied by synchrotron‐based in situ high‐pressure single‐crystal X‐ray diffraction experiments. On compression to 120 GPa, both borate layer‐structures are preserved. Additionally, at ≈114 GPa, the formation of a second phase can be observed in both compounds. The new high‐pressure modification  γ ‐ZrB 2 O 5  features a rearrangement of the corner‐sharing BO 4  tetrahedra, while still maintaining the four‐ and eight‐membered rings. The new phase  γ ‐HfB 2 O 5  contains ten‐membered rings including the rare structural motif of edge‐sharing BO 4  tetrahedra with exceptionally short B−O and B⋅⋅⋅B distances. For both structures, unusually high coordination numbers are found for the transition metal cations, with ninefold coordinated Hf 4+ , and tenfold coordinated Zr 4+ , respectively. These findings remarkably show the potential of cold compression as a low‐energy pathway to discover metastable structures that exhibit new coordinations and structural motifs.

Polymorphs of the Gadolinite‐Type Borates ZrB 2 O 5 and HfB 2 O 5 Under Extreme Pressure