The title complex, which has a new-type layer structure, has been obtained, and its crystal and molecular structure has been determined by the X-ray diffraction technique. The crystallographic data are: monoclinic, space group P21?n, a=18.264(7), b=16.223(7), c=10.623(5) A, β=92.77(5)° and Z=4. The final R value was 0.059. The cobalt atoms are in an octahedral geometry, ligated by three thiocyanato(SCN) nitrogen atoms and three oxygen atoms (N-methyl-2-pyrrolidone) in a meridional configuration; these cobalt atoms are cross-linked to adjacent mercury atoms by SCN ions, forming a characteristic layer structure which consists of twenty-four-membered rings of the [Co3Hg3(SCN)6] unit. The mercury atoms are in the tetrahedral geometry, ligated by four sulfur atoms of SCN ions, three bridging and one unidentate. The complex layers in parallel are piled up in the a-axis direction, and there are no bridgings or hydrogen bondings between them.

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