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

Abstract

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.

Structural topologies involving energetically significant antiparallel π-stacking and unconventional N(nitrile)⋯π(fumarate) contacts in dinuclear Zn(ii) and polymeric Mn(ii) compounds: antiproliferative evaluation and theoretical studies

“…S7, ESI†). For compound 1 , the weight loss of 34.6% in the temperature range 100–215 °C can be attributed to the weight loss of the water molecules, 66 one male moiety 67 and one 3-AMpy moiety 68 (calcd = 33.15%). The weight loss of 10.21% in the temperature range of 216–350 °C is due to the decomposition of one 3-AMpy moiety (cald = 11.9%).…”

“…68 In the temperature range 351–700 °C, the weight loss of 30.25% is due to the loss of one male moiety (calcd = 28.82%). 67 For compound 2 , the weight loss of 20.82% in the temperature range 100–167 °C is due to the loss of water molecules and half of the fum moiety (calcd = 22.12%). 69,70 In the temperature range 325–450 °C, decomposition of one 3-CNpy and the other half of the fum moiety takes place with the observed weight loss of 39.23% (calcd = 38.71%).…”