From the aqueous-ethanolic system Ni(OH)2—H2fum—phen (H2fum = fumaric acid, phen = 1,10-phenanthroline), novel complex [Ni(phen)3](fum)·9H2O (1) was isolated and characterized by chemical analyses and FT-IR spectroscopy. Results of single crystal X-ray structure analysis have shown that the ionic crystal structure of 1 is built of [Ni(phen)3]2+ complex cations, fumarate dianions and nine crystallographically independent water molecules of crystallization. The Ni(II) atom exhibits hexa-coordination by three phen ligands with mean Ni-N bond length of 2.090 Å. Water molecules form hydrophilic supramolecular layers with fumarate dianions via extended network of O—H···O type hydrogen bonds with O···O distances from the range of 2.676(2)—2. 916(2) Å; hydrophobic complex cations are embedded between these layers. Thermal study of 1 has shown that endothermic dehydration in the temperature range of 95—195 °C takes at least two steps of the process. Graphical Abstract Crystal structure of [Ni(phen)3]fum·9H2O (phen = 1,10-phenanthroline; H2fum = fumaric acid) which is built of supramolecular layers formed by hydrogen bonded water solvate molecules and fum dianions and between the supramolecular layers embedded [Ni(phen)3]2+ complex cations is described here.

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