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The high-pressure behaviour of the superconductor MgB2 with a hexagonal structure has been investigated by the in situ synchrotron radiation x-ray diffraction method under pressures up to 42.2 GPa in a diamond anvil cell. An abrupt decrease of about 7％ in the unit cell volume of this material occurs in the pressure range of 26.3-30.2 GPa. A split of the Raman spectrum was also observed. The jump of the compression curve and Raman spectrum are ascribed to an isostructural transition in MgB2 at a pressure of 30.2 GPa.