Crystal structure of hexaaquadichloridoytterbium(III) chloride

The crystal structure of the title compound, [YbCl2(H2O)6]Cl, was determined at 110 K. Samples were obtained from evaporated acetonitrile solutions containing the title compound, which consists of a [YbCl2(H2O)6]+ cation and a Cl− anion. The cations in the title compound sit on a twofold axis and form O—H⋯Cl hydrogen bonds with the nearby Cl− anion. The coordination geometry around the metal centre forms a distorted square antiprism. The ytterbium complex is isotypic with the europium complex [Tambrornino et al. (2014 ▸). Acta Cryst. E70, i27].


S1. Comment
Samples gathered from the mother liquor were coated with mineral oil prior to mounting to reduce sample decay. The ytterbium complex is isomorphous with a recently published redetermination of a europium complex (Tambrornino, et al. 2014) which was in turn similar to studies of other lanthanoid chloride hydrates (Marezio, et al. 1961).
Crystals of ytterbium(III) chloride hexahydrate consist of a [YbCl 2 (H 2 O) 6 ] 1+ cation and a chlorine anion. The covalent nature of the lanthanoid +3 cations are not surprising given their high charge density. An ORTEP of the title compound is shown in Fig. 1.

S2. Experimental
In 40.0 ml of acetonitrile, 0.1945 grams (0.5019 mmol) of ytterbium(III) chloride hexahydrate was added to 0.1000 grams (0.5020 mmol) of di-2-pyridyl ketone oxime (dpko) with the hopes of synthesizing a Yb-dpko complex. The mixture was heated to dissolve the solids. Upon cooling and subsequent evaporation, small colorless crystals of the title compound were isolated. The metal chloride was purchased from Strem chemicals (99.9% purity) whereas the dpko was purchased from Sigma-Aldrich (99.9%). Both were used without additional purification.

S3. Refinement
H atoms were included and were allowed to refine to ideal O-H distances based upon geometric considerations.
Thermal parameters for all H atoms were included in the refinement in riding motion approximation with U iso = 1.5U eq of the carrier atom.
supporting information

Figure 1
A view of the title compound (Farrugia, 2012). Displacement ellipsoids are drawn at the 50% probability level. H atoms have been omitted for clarity. where P = (F o 2 + 2F c 2 )/3 (Δ/σ) max = 0.001 Δρ max = 0.91 e Å −3 Δρ min = −0.96 e Å −3 Extinction correction: SHELXL2014 (Sheldrick, 2015), Fc * =kFc[1+0.001xFc 2 λ 3 /sin(2θ)] -1/4 Extinction coefficient: 0.0602 (13) Special details Experimental. Sample was covered in mineral oil prior to mounting in cryo stream. Hydrogen atoms were included and were allowed to refine to ideal O-H distances based upon geometric considerations. Thermal parameters for all H atoms were included in the refinement in riding motion approximation with U iso = 1.5U eq of the carrier atom. CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm (Oxford Diffraction (2009). Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å 2 )
x y z U iso */U eq