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Single crystals of the high-temperature form I of [Co(NCS) 2 (DMAP) 2 ] (DMAP = 4-di-methyl-amino-pyridine, C 7 H 10 N 2 ) were obtained accidentally by the reaction of Co(NCS) 2 with DMAP at slightly elevated temperatures under kinetic control. This modification crystallizes in the monoclinic space group P 2 1 / m and is isotypic with the corresponding Zn compound. The asymmetric unit consists of one crystallographically independent Co cation and two crystallographically independent thio-cyanate anions that are located on a crystallographic mirror plane and one DMAP ligand (general position). In its crystal structure the discrete complexes are linked by C-H⋯S hydrogen bonds into a three-dimensional network. For comparison, the crystal structure of the known low-temperature form II, which is already thermodynamically stable at room temperature, was redetermined at the same temperature. In this polymorph the complexes are connected by C-H⋯S and C-H⋯N hydrogen bonds into a three-dimensional network. At 100 K the density of the high-temperature form I (ρ = 1.462 g cm -3 ) is higher than that of the low-temperature form II (ρ = 1.457 g cm -3 ), which is in contrast to the values determined by XRPD at room temperature. Therefore, these two forms represent an exception to the Kitaigorodskii density rule, for which extensive inter-molecular hydrogen bonding in form II might be responsible.

Comparison of the crystal structures of the low- and high-temperature forms of bis[4-(dimethylamino)pyridine]dithiocyanatocobalt(II)