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A new oxoborate β -CaB 4 O 7  has been synthesized under high-pressure/high-temperature conditions from calcium oxide and boron oxide with a Walker-type multianvil apparatus at 7.7 GPa and 1100 °C. Single crystal X-ray structure determination of β -CaB 4 O 7  revealed: Pmn2 1 , a = 1058.4(1), b = 436.9(1), c = 419.4(1) pm, Z = 2, R1 = 0.0305, wR2 = 0.0587 (all data). The compound is isotypic to the known oxoborates SrB 4 O 7 , PbB 4 O 7 , and EuB 4 O 7  exhibiting a network structure of linked BO4 tetrahedra. As a prominent feature of the tetrahedral network an oxygen atom is coordinated to three boron atoms. The relation of the crystal structure of the high-pressure phase β -CaB 4 O 7  to the normalpressure phase α-CaB 4 O 7  as well as the relation to the isotypic phases MB 4 O 7  (M = Sr, Pb, Eu) are discussed. The results of IR-spectroscopic investigations on β -CaB 4 O 7  are also presented.

β-CaB 4 O 7 : A New Polymorph Synthesized under High-Pressure/High-Temperature Conditions