Abstract
The synthesis of more than 10 new magnetic ionic liquids with [MnX4]2− anions, X = Cl, NCS, NCO, is presented. Detailed structural information through single-crystal X-ray diffraction is given for (DMDIm)[Mn(NCS)4], (BnEt3N)2[Mn(NCS)4], and {(Ph3P)2N}2[Mn(NCO4)]·0.6H2O, respectively. All compounds consist of discrete anions and cations with tetrahedrally coordinated Mn(II) atoms. They show paramagnetic behavior as expected for spin-only systems. Melting points are found for several systems below 100 °C classifying them as ionic liquids. Thermal properties are investigated using differential scanning calorimetry (DSC) measurements. The physicochemical properties of density, dynamic viscosity, electrolytic conductivity, and surface tension were measured temperature-dependent of selected samples. These properties are discussed in comparison to similar Co containing systems. An increasing amount of bromide impurity is found to affect the surface tension only up to 3.3%.
Highlights
We report on the synthesis, properties and physicochemical investigation of a series of Ax [MnX4 ] (A = ammonium, iminium- and imidazolium-based cation; X = Cl, NCS, NCO) complexes with comparably low melting points
Melting points were determined by differential scanning calorimetry (DSC) measurements with a DSC823e instrument (Mettler-Toledo, Columbus, OH, USA) in the range −100 to 200 ◦ C at a heating rate of 10 K min−1 (Ar atmosphere, Al crucible) or with a STA 449 F3 Jupiter device (Netzsch, Selb, Germany) in the temperature range 25 to 600 ◦ C at a heating rate of 10 K min−1 (N2 atmosphere, Al crucible), respectively
[Mn(NCS)4 ]2− -based compounds were synthesized by well-established salt metathesis reactions of ammonium, iminium- or imidazolium-based halide salts with K2 [Mn(NCS)4 ] (generated from the 2− (n = 2: x+ (I) and General synthetic approach for the synthesis of [Mn(NCS)4]2−A
Summary
For the last 20 years, the ongoing tremendous interest in ionic liquids (ILs) as salts with low melting points is based on their partly unique properties which lead to a variety of possible applications. In the last 10 years, we have reported on different classes of transition metal-containing low-melting ILs with complex anions of the 3d metals Cr, Co, and Ni, respectively, of which a series of physicochemical data is available [24,25,26,27,28,29,30,31,32,33,34]. Containing system, [Ni(bpy)3 ][Mn(NCO)4 ]·H2 O (bpy = 2,20 -bipyridine) [54], respectively In this contribution, we report on the synthesis, properties and physicochemical investigation of a series of Ax [MnX4 ] (A = ammonium-, iminium- and imidazolium-based cation; X = Cl, NCS, NCO) complexes with comparably low melting points. The crystal and molecular structures of three compounds, (DMDIm)[Mn(NCS)4 ], (BnEt3 N)2 [Mn(NCS)4 ], and {(Ph3 P) N}2 [Mn(NCO4 )]·0.6H2 O, respectively, are presented and discussed
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