Three two-dimensional (2D) and 3D supramolecular coordination architectures based on ternary M(II)-dicyanamide-2-hydroxypyridine systems, [Co(hmpH)2(dca)2] (1), [Cu(hmpH)2(dca)2] (2), and [Mn(hepH)2(dca)2] (3) (dca = dicyanamide, hmpH = 2-(hydroxymethyl)pyridine, hepH = 2-(hydroxyethyl)pyridine), have been synthesized. 1 is a mononuclear Co(II) complex. The mononuclear units are interlinked into a 2D (4,4) hydrogen-bonded layer via O–H？N hydrogen bonds between the hydroxyl groups and the noncoordinating nitrile ends. These 2D layers are further extended into a 3D supramolecular architecture via the interlayer pyridyl-pyridyl stacking interaction. 2 has a 1D coordination chain structure formed by the double 1,5-dca bridged dinuclear [Cu2( 1,5-dca)2(hmpH)2] unit and the 1,3-dca bridges via weak Cu–N coordination, and these 1D coordination chains are further extended into 2D hydrogen-bonded layers via strong O–H？N hydrogen-bonding interaction between the hydroxyl groups and the noncoordinating nitrile ends. 3 is a 2D (4,4) coordination network made of 1D [Mn(hepH)( 1,5-dca)] helical chain units and interchain double ( 1,5-dca) bridges. Pairs of [Mn(hepH)( 1,5-dca)] helical chains are interlinked by the double ( 1,5-dca) bridges into a racemic coordination layer structure, which is further extended into a 3D hydrogen-bonded network. Magnetic studies reveal that weak antiferromagnetic exchange occurs in 3. 1. Introduction Since the pioneering reports of Robson and coworkers in 1990 [1, 2], this realm of crystal engineering is growing interest, and great efforts have been devoted to the assembly of supramolecular systems of organic molecular solids and coordination polymers through hydrogen bonds and or coordination bonds, with the resultant crystalline materials having a wide range of potential applications, such as electronic, magnetic, optical, absorbent, and catalytic materials [3–29]. In recent years, much attention has been devoted to dicyanamide-anion- (dca-) bridged coordination polymers [30–42] for the large variety of magnetic properties, especially the α-M(dca)2 series of compounds, which have isomorphous rutile-like structure, display ferromagnetism (Co, Ni) [43–46], spin-canted antiferromagnetism (Cr, Mn, Fe) [47, 48], and paramagnetism (Cu) [45, 46]. Of further importance, from a structural perspective, when auxiliary L ligands are introduced to the ternary -dca-L systems, different coordination architectures, such as mononuclear and dinuclear compounds [49], 1D chains [50–58], 2D (4,4) or (6,3) [59–63] sheets, and 3D network topologies [64–67],
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