The title complex [Co（TPPO）4] [Co（NCS）2TPPO]2 （TPPO=triphenylphosphine oside） was prepared by solvent evaporation method. Its crystal structure was determined by x-ray diffraction method. The crystal is rhombohedral with space group R3. The unit cell parameters are presented and the structure has been refined to a final R of 0.064.
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