Crystal structure of hexa-aqua-dichlorido-ytterbium(III) chloride.

The crystal structure of the title compound, [YbCl2(H2O)6]Cl, was determined at 110 K. Samples were obtained from evaporated aceto-nitrile 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 anti-prism. The ytterbium complex is isotypic with the europium complex [Tambrornino et al. (2014 ▶). Acta Cryst. E70, i27].

Related literature

The ytterbium complex is isotypic with the europium complex, the redetermined structure of which was published recently (Tambrornino et al. 2014 ▸) which was in turn similar to studies of other lanthanoid chloride hydrates (Marezio et al., 1961 ▸).

Experimental

Crystal data

[YbCl2(H2O)6]Cl

M = 387.49

Monoclinic,

a = 7.8158 (11) Å

b = 6.4651 (3) Å

c = 12.7250 (18) Å

β = 131.45 (2)°

V = 481.92 (16) Å3

Z = 2

Mo Kα radiation

μ = 10.52 mm−1

T = 110 K

0.24 × 0.18 × 0.17 mm

Data collection

Oxford Diffraction Xcalibur Sapphire3 diffractometer

Absorption correction: multi-scan (CrysAlis PRO; Oxford Diffraction, 2009 ▸) T min = 0.187, T max = 0.268

12358 measured reflections

1806 independent reflections

1762 reflections with I > 2σ(I)

R int = 0.042

Refinement

R[F 2 > 2σ(F 2)] = 0.018

wR(F 2) = 0.041

S = 1.12

1806 reflections

51 parameters

H-atom parameters constrained

Δρmax = 0.91 e Å−3

Δρmin = −0.96 e Å−3

Data collection: CrysAlis CCD (Oxford Diffraction, 2009 ▸); cell refinement: CrysAlis RED (Oxford Diffraction, 2009 ▸); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS2014 (Sheldrick, 2008 ▸); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015 ▸); molecular graphics: PLATON (Spek, 2009 ▸) and ORTEP-3 for Windows (Farrugia, 2012 ▸); software used to prepare material for publication: SHELXL2014.

Crystal structure: contains datablock(s) I. DOI: 10.1107/S2056989015008488/br2249sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S2056989015008488/br2249Isup2.hkl

Click here for additional data file.

. DOI: 10.1107/S2056989015008488/br2249fig1.tif

A view of the title compound (Farrugia, 2012). Displacement ellipsoids are drawn at the 50% probability level. H atoms have been omitted for clarity.

CCDC reference: 1062504

Additional supporting information: crystallographic information; 3D view; checkCIF report

[YbCl2(H2O)6]Cl	Dx = 2.671 Mg m−3
Mr = 387.49	Melting point: 350 K
Monoclinic, P2/c	Mo Kα radiation, λ = 0.71073 Å
a = 7.8158 (11) Å	Cell parameters from 7486 reflections
b = 6.4651 (3) Å	θ = 4.9–33.8°
c = 12.7250 (18) Å	µ = 10.52 mm−1
β = 131.45 (2)°	T = 110 K
V = 481.92 (16) Å3	Block, light pink
Z = 2	0.24 × 0.18 × 0.17 mm
F(000) = 362

Oxford Diffraction Xcalibur Sapphire3 diffractometer	1806 independent reflections
Radiation source: fine-focus sealed tube	1762 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.042
Detector resolution: 16.1790 pixels mm-1	θmax = 33.7°, θmin = 4.3°
ω scans	h = −11→12
Absorption correction: multi-scan (CrysAlis PRO; Oxford Diffraction, 2009)	k = −9→9
Tmin = 0.187, Tmax = 0.268	l = −19→19
12358 measured reflections

Refinement on F2	Hydrogen site location: difference Fourier map
Least-squares matrix: full	H-atom parameters constrained
R[F2 > 2σ(F2)] = 0.018	w = 1/[σ2(Fo2) + (0.0207P)2] where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.041	(Δ/σ)max = 0.001
S = 1.12	Δρmax = 0.91 e Å−3
1806 reflections	Δρmin = −0.96 e Å−3
51 parameters	Extinction correction: SHELXL2014 (Sheldrick, 2015), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraints	Extinction coefficient: 0.0602 (13)

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 Uiso = 1.5Ueq 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.

	x	y	z	Uiso*/Ueq
Yb1	0.5000	0.65776 (2)	0.7500	0.01599 (6)
Cl1	0.32165 (12)	0.34336 (8)	0.56141 (7)	0.02594 (12)
Cl2	0.0000	−0.12652 (14)	0.2500	0.02883 (16)
O1	0.1817 (3)	0.5542 (3)	0.71889 (19)	0.0266 (3)
H1A	0.1626	0.4279	0.7416	0.040*
H1B	0.0569	0.6336	0.6823	0.040*
O2	0.7626 (3)	0.9242 (3)	0.85341 (19)	0.0276 (3)
H2A	0.7791	1.0181	0.9087	0.041*
H2B	0.8611	0.9467	0.8434	0.041*
O3	0.5420 (3)	0.8002 (3)	0.93497 (19)	0.0273 (3)
H3A	0.6709	0.8455	1.0145	0.041*
H3B	0.4315	0.8170	0.9361	0.041*

	U11	U22	U33	U12	U13	U23
Yb1	0.01594 (8)	0.01718 (8)	0.01703 (8)	0.000	0.01184 (6)	0.000
Cl1	0.0283 (3)	0.0258 (3)	0.0251 (3)	−0.00427 (18)	0.0183 (2)	−0.00488 (18)
Cl2	0.0271 (4)	0.0336 (4)	0.0299 (4)	0.000	0.0206 (4)	0.000
O1	0.0229 (8)	0.0278 (8)	0.0343 (9)	−0.0001 (6)	0.0212 (8)	0.0043 (7)
O2	0.0293 (9)	0.0262 (8)	0.0359 (9)	−0.0096 (7)	0.0253 (8)	−0.0098 (7)
O3	0.0310 (9)	0.0331 (8)	0.0246 (8)	−0.0050 (7)	0.0213 (8)	−0.0061 (7)

Yb1—O2i	2.3101 (17)	Yb1—O1i	2.3433 (16)
Yb1—O2	2.3101 (17)	Yb1—O1	2.3434 (17)
Yb1—O3i	2.3392 (17)	Yb1—Cl1i	2.7211 (7)
Yb1—O3	2.3392 (17)	Yb1—Cl1	2.7212 (7)
O2i—Yb1—O2	83.56 (10)	O1i—Yb1—Cl1i	76.75 (5)
O2i—Yb1—O3i	69.72 (6)	O1—Yb1—Cl1i	78.60 (5)
O2—Yb1—O3i	76.09 (7)	O2i—Yb1—Cl1	108.14 (6)
O2i—Yb1—O3	76.09 (7)	O2—Yb1—Cl1	143.38 (5)
O2—Yb1—O3	69.72 (6)	O3i—Yb1—Cl1	75.99 (5)
O3i—Yb1—O3	133.64 (9)	O3—Yb1—Cl1	146.11 (5)
O2i—Yb1—O1i	138.85 (6)	O1i—Yb1—Cl1	78.60 (5)
O2—Yb1—O1i	70.92 (6)	O1—Yb1—Cl1	76.75 (5)
O3i—Yb1—O1i	73.06 (7)	Cl1i—Yb1—Cl1	83.34 (3)
O3—Yb1—O1i	121.09 (7)	Yb1—O1—H1A	125.5
O2i—Yb1—O1	70.92 (6)	Yb1—O1—H1B	125.7
O2—Yb1—O1	138.85 (6)	H1A—O1—H1B	108.8
O3i—Yb1—O1	121.09 (7)	Yb1—O2—H2A	125.4
O3—Yb1—O1	73.06 (7)	Yb1—O2—H2B	125.4
O1i—Yb1—O1	146.79 (9)	H2A—O2—H2B	109.2
O2i—Yb1—Cl1i	143.38 (5)	Yb1—O3—H3A	125.4
O2—Yb1—Cl1i	108.15 (6)	Yb1—O3—H3B	125.4
O3i—Yb1—Cl1i	146.11 (5)	H3A—O3—H3B	109.2
O3—Yb1—Cl1i	75.99 (5)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1A···Cl2ii	0.91	2.37	3.2499 (19)	163
O1—H1B···Cl1iii	0.91	2.50	3.171 (2)	131
O2—H2A···Cl1iv	0.87	2.36	3.1460 (18)	150
O2—H2B···Cl2v	0.87	2.38	3.1806 (18)	154
O3—H3A···Cl2vi	0.88	2.33	3.179 (2)	163
O3—H3B···Cl1vii	0.88	2.48	3.1758 (19)	136

Table 1

Hydrogen-bond geometry (, )

DHA	DH	HA	D A	DHA
O1H1ACl2i	0.91	2.37	3.2499(19)	163
O1H1BCl1ii	0.91	2.50	3.171(2)	131
O2H2ACl1iii	0.87	2.36	3.1460(18)	150
O2H2BCl2iv	0.87	2.38	3.1806(18)	154
O3H3ACl2v	0.88	2.33	3.179(2)	163
O3H3BCl1vi	0.88	2.48	3.1758(19)	136

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) .