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The crystal structure of three C2/c clinopyroxenes with composition (Ca 0.8 Co 0.2 )CoSi 2 O 6 , (Ca 0.6 Co 0.4 ) CoSi 2 O 6  and (Ca 0.4 Co 0.6 )CoSi 2 O 6  was refined down to R4σ = 2.6% by single-crystal X-ray diffraction. The crystals were synthesized at P = 3 GPa by cooling from 1500 to 1200 °C in a piston-cylinder apparatus. At the end of the refinement cycles, electron density residuals (up to 2.1 e-) were observed close to the M2 site and related to the site splitting of Ca and Co in the M2 polyhedron in the two subsites M2 and M2′. Split refinement significantly improved the agreement factor and decreased the uncertainty in the atomic coordinates. Similar features were found in (Ca,Mg)MgSi 2 O 6  and (Ca,Fe) FeSi 2 O 6  intermediate pyroxenes.

The structure of (Ca,Co)CoSi 2 O 6 pyroxenes and the Ca-M 2+ substitution in (Ca,M 2+ )M 2+ Si 2 O 6 pyroxenes (M 2+ = Co, Fe, Mg)