The preparation of amylopection tris(phenylcarbamate) (ATP) chiral stationary phases(CSPs) coated on a small-particle (5μm, 120Å) spherical silica support, according to a process that is reported, is presented. A new chiral tetrahedral cluster (μ3-Se)RuCoW(CO)8C5H4C(O)CH32which was synthesized by the thermal reaction of the precursor (μ3-Se)RuCo2(CO)91with the functionally substituted cyclopentadienyl tricarbonyl metal complex anions [W(CO)3C5H4C(O)CH3]−is resolved on the amylopectin tris (phenylcarbamate) chiral stationary phases.