Poly[μ2-aqua-μ4-[1-(4-chlorophenyl)-4,4,4-trifluorobutane-1,3-dionato]-potassium]

In the title compound, [K(C10H5ClO2F3)(H2O)]n, the two independent K+ ions are located on a twofold rotation axis. For each of the cations, the distorted cubic coordination environment is defined by two F and four O atoms of symmetry-related 1,4-chlorophenyl-4,4,4-trifluorobutane-1,3-dionate anions and by two O atoms of water molecules. The μ4-bridging character of the anion and the μ2-bridging of the water molecule lead to the formation of layers parallel to (100). The coordinating water molecules are also involved in O—H⋯O hydrogen bonds that reinforce the molecular cohesion within the layers, which are stacked along [100]. The β-diketonate anion is not planar, with an angle of 31.78 (10)° between the mean planes of the diketonate group and the chlorophenyl ring.

In the title compound, [K(C 10 H 5 ClO 2 F 3 )(H 2 O)] n , the two independent K + ions are located on a twofold rotation axis. For each of the cations, the distorted cubic coordination environment is defined by two F and four O atoms of symmetry-related 1,4-chlorophenyl-4,4,4-trifluorobutane-1,3dionate anions and by two O atoms of water molecules. The 4 -bridging character of the anion and the 2 -bridging of the water molecule lead to the formation of layers parallel to (100). The coordinating water molecules are also involved in O-HÁ Á ÁO hydrogen bonds that reinforce the molecular cohesion within the layers, which are stacked along [100]. The -diketonate anion is not planar, with an angle of 31.78 (10) between the mean planes of the diketonate group and the chlorophenyl ring. H atoms treated by a mixture of independent and constrained refinement Á max = 0.19 e Å À3 Á min = À0.20 e Å À3 Table 1 Hydrogen-bond geometry (Å , ). Data collection: SMART (Bruker, 2003); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97. supplementary materials Acta Cryst. (2013). E69, m422-m423 [doi:10.1107 The title compound contains two potassium ions, one 1,4-chlorophenyl-4,4,4-trifluoro-1,3-butanedionate anion and one coordinating water molecule in the asymmetric unit. Both potassium ions are situated on twofold rotation axes and are in the centres of distorted cubes, that are formed by two F and six O atoms. The cations are arranged in alternating chains along [010], Fig. 2, with K···K distances of 3.6379 (11) and 4.4360 (11) Å, respectively. The cations are bridged by two water molecules and one bis-monodentate CF 3 group, as well as by four oxygen atoms of two β-diketonate groups. The chains are joined into layers parallel to (100) since each diketonate coordinates potassium ions from two adjacent chains.

Related literature
The β-diketonate ligand is not planar with an angle of 31.78 (10)° between the mean planes of the diketonate group and the chlorophenyl ring. Within the layers, there are hydrogen bonds between the coordinating water molecules and adjacent diketonate O atoms (Table 1, Fig. 3). The unit cell does not contain any residual solvent acessible voids.

Experimental
Firstly, 0.5 mmol of europium(III) nitrate pentahydrate were dissolved in 20 ml of methanol followed by the addition of 0.9 ml of potassium methoxide. This solution was left to reflux at 353 K for 15 min. Secondly, 1.5 mmol of 1,14 chlorophenyl-4,4,4-trifluoro-1,3-butanedionate were dissolved in 15 ml of methanol and added to the main solution. After decanting the resulting solution, 0.5 mmol of bathophenanthroline were dissolved in 10 ml of methanol and added to the main solution. The main solution was then transferred from a volumetric balloon to a beaker covered with paraffin film and placed on a water bath at 303 K until complete evaporation was verified. Since from the evaporation process no crystals were obtained, all the material from this batch was dissolved in 25 ml of chloroform. A light orange powder was formed alongside with some transparent crystals. The powder was studied by X-ray powder diffraction and was proven to be amorphous; the transparent crystals were studied by single-crystal X-ray diffraction, and as a result, the title compound was revealed.

Refinement
All hydrogen atoms bound to carbon atoms were placed at calculated positions and were treated as riding on the parent atoms with C-H = 0.93 Å (aromatic) and with U iso (H) = 1.2 U eq (C). The H atoms belonging to the water molecule were found in a difference electron density synthesis and subsequently refined with

Computing details
Data collection: SMART (Bruker, 2003); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT (Bruker, 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).  Packing of the components in the title structure. For clarity, the Cl and H atoms were omitted. Atoms C5 to C10 defining the benzene ring were also omitted.  Packing of the components showing the hydrogen bonding interactions as dashed lines.

Poly[µ 2 -aqua-µ 4 -[1-(4-chlorophenyl)-4,4,4-trifluorobutane-1,3-dionato]-potassium]
Crystal data Refinement. Refinement of F 2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F 2 , conventional R-factors R are based on F, with F set to zero for negative F 2 . The threshold expression of F 2 > σ(F 2 ) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F 2 are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger.