Ionic Liquid of Choline Chloride/Malonic Acid as a Solvent in the
Synthesis of Open-Framework Iron Oxalatophosphates
Chyi-Yang Sheu
Shang-Fan Lee
Kwang-Hwa Lii
10.1021/ic0518475.s002
https://acs.figshare.com/articles/journal_contribution/Ionic_Liquid_of_Choline_Chloride_Malonic_Acid_as_a_Solvent_in_the_Synthesis_of_Open_Framework_Iron_Oxalatophosphates/3234805
Two new iron(III) oxalatophosphates, Cs<sub>2</sub>Fe(C<sub>2</sub>O<sub>4</sub>)<sub>0.5</sub>(HPO<sub>4</sub>)<sub>2</sub> (<b>1</b>)
and CsFe(C<sub>2</sub>O<sub>4</sub>)<sub>0.5</sub>(H<sub>2</sub>PO<sub>4</sub>)(HPO<sub>4</sub>) (<b>2</b>), have been synthesized by
using a low melting point eutectic mixture of choline chloride and
malonic acid as a solvent and characterized by single-crystal X-ray
diffraction and magnetic susceptibility. Crystal data are as follows: compound <b>1</b>, monoclinic, <i>P</i>2<sub>1</sub>/<i>c </i>(No. 14), <i>a</i> = 8.5085(4) Å,
<i>b</i> = 12.7251(6) Å, <i>c</i> = 9.8961(4) Å, β = 107.117(1)°, <i>V</i> =
1024.01(8) Å<sup>3</sup>, <i>Z </i>= 4, and <i>R</i><sub>1</sub> = 0.0264; compound <b>2</b>, monoclinic,
<i>P</i>2<sub>1</sub>/<i>n </i>(No. 14), <i>a</i> = 8.0038(3) Å, <i>b</i> = 10.2923(3) Å, <i>c</i> = 11.4755(4) Å, β = 100.507(1)°, <i>V</i> = 929.47(5) Å<sup>3</sup>, <i>Z </i>= 4, and <i>R</i><sub>1</sub> =
0.0311. The structure of <b>1</b> comprises FeO<sub>6</sub> octahedra connected
by HPO<sub>4</sub><sup>2-</sup> tetrahedra and bisbidentate oxalate anions to form a
3D framework containing intersecting 12-ring channels, with the
charge-compensating Cs<sup>+</sup> cations being located at the intersections
of these channels. The structure of <b>2</b> consists of 2D layers of
octahedral FeO<sub>6</sub>, tetrahedral H<sub>2</sub>PO<sub>4</sub><sup>-</sup> and HPO<sub>4</sub><sup>2-</sup> moieties, and
bisbidentate oxalate ligands with the Cs<sup>+</sup> cations between the
layers. They are the first examples for the use of ionic liquid as a
solvent in the synthesis of metal oxalatophosphates.
2006-03-06 00:00:00
3 D framework
compound
point eutectic mixture
FeO 6 octahedra
R 1
2 D layers
HPO
bisbidentate oxalate ligands
cation
0.5
octahedral FeO 6
tetrahedral H 2 PO 4
oxalatophosphate
bisbidentate oxalate anions