Synthesis, crystal structure, infrared spectrum, and thermal properties of [Ni(1,10-phenanthroline)3](fumarate)•9H2O complex with hydrogen bonded supramolecular layers involving fumarate anions

From the aqueous-ethanolic system Ni(OH)(2)-H(2)fum-phen (H(2)fum = fumaric acid, phen = 1,10-phenanthroline), novel complex [Ni(phen)(3)](fum)center dot 9H(2)O (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 angstrom. Water molecules form hydrophilic supramolecular layers with fumarate dianions via extended network of O-H center dot center dot center dot O type hydrogen bonds with O center dot center dot center dot O distances from the range of 2.676(2)-2.916(2) angstrom; hydrophobic complex cations are embedded between these layers. Thermal study of 1 has shown that endothermic dehydration in the temperature range of 95-195 degrees C takes at least two steps of the process.