In the course of our structural investigations of borates synthesized under high-pressure, high-temperature conditions, we discovered several new high-pressure modifications [1][2][3][4][5] with interesting structural features and physical properties, for example, a new non-centrosymmetric modification of bismuth triborate (d-BiB 3 O 6 ).[6] Along with the investigation of these phase transitions, we aim to synthesize borates with new compositions, whose existence is presumably based on high-pressure conditions during synthesis. Examples are the borates RE 3 B 5 O 12 (RE = Tm-Lu), [7] RE 4 B 6 O 15 (RE = Dy, Ho), [8][9][10] a-RE 2 B 4 O 9 (RE = SmHo), [11][12][13] b-RE 2 B 4 O 9 (RE = Gd, Dy), [14,15] and Pr 4 B 10 O 21 , [16] which have no corresponding ambient-pressure modifications. To our surprise, the borates RE 4 B 6 O 15 (RE = Dy, Ho) [8][9][10] revealed edge-sharing as well as corner-sharing BO 4 tetrahedra; such edge-sharing tetrahedra had been previously unknown in the varied structural chemistry of borates. Later on, we discovered a second type of structure, a-RE 2 B 4 O 9 (RE = Sm-Ho), [11][12][13] that also display this new structural feature. Herein, we report the synthesis and characterization of a new nickel borate HP-NiB 2 O 4 , in which each BO 4 tetrahedron shares a common edge with a second BO 4 tetrahedron.In the system NiO-B 2 O 3 , there is only one nickel borate, of the composition Ni 3 (BO 3 ) 2 . [17][18][19][20] This compound displays trigonally coordinated boron atoms and Ni 2+ ions with octahedral coordination. Recently, Pompetzki and Albert found a new synthetic route to pure Ni 3 (BO 3 ) 2 ; they employed the thermal decomposition of a mixture of NiCO 3 ·2 Ni(OH) 2 ·4 H 2 O and H 3 BO 3 .[21] In our own investigations of the Ni-B-O ternary system, we synthesized a second borate of the composition b-NiB 4 O 7[22] under high-pressure conditions of 7.5 GPa and at a temperature of 1000 8C; this compound has a structure analogous to the high-pressure modification b-ZnB 4 O 7 .[5] With HP-NiB 2 O 4 , we have now found a third composition in the Ni-B-O ternary system, which accentuates the performance of high-pressure synthesis in solid-state chemistry.HP-NiB 2 O 4 was synthesized in a high-pressure, hightemperature reaction at 7.5 GPa and 680 8C in a modified Walker module (multianvil assembly) starting from the oxides NiO and B 2 O 3 [Eq.(1)]. [23] NiO þ B 2 O 3 !HP-NiB 2 O 4 ð1Þ