We report the high-pressure synthesis of novel superconductor MgB 2 and some related compounds. The superconducting transition temperature of our samples of MgB 2 is found to be 36.6 K. The MgB 2 lattice parameters determined via X-ray diffraction are in excellent agreement with results of our ab initio calculations. The TDPAC measurements of 111 Cd quadrupole frequency ν Q demonstrate a small increase in ν Q with decreasing temperature from T room to T He .The electric field gradient V zz at the B site calculated from first principles is in fair agreement with V zz obtained from 11 B NMR spectra of MgB 2 reported in the literature. It is also very close to V zz found in our 111 Cd TDPAC experiments, which suggests that the 111 Cd probe substitutes for boron in the MgB 2 lattice.