[Yb(H₂O)₈][Cd₃Cl₉(H₂O)]·6H₂O

The title compound, namely octa­aqua­ytterbium(III) aqua­nona­chloro­tricadmate(II) hexa­hydrate, [Yb(H₂O)₈][Cd₃Cl₉(H₂O)]·6H₂O, was prepared by evaporation at 278 K from an aqueous solution of the ternary system YbCl₃–CdCl₂–H₂O and was characterized by elemental chemical analysis and by X-ray powder and single-crystal diffraction studies. The crystal structure can be viewed as being built from layers of double chains of CdCl₆ and CdCl₅(H₂O) octahedra separated by antiprismatic [Yb(H₂O)₈]³⁺ cations. The stabilization of the structure is ensured by O—H...O and O—H...Cl hydrogen bonds. A comparison with the structures of SrCd₂Cl₆·8H₂O and CeCd₄Cl₁₁·13H₂O is presented.

S1. Comment

Investigations of hydrated rare earth (III) chlorides are very important for understanding their physical (magnetic, optical) and structural properties. The ternary systems ACl–LnCl₃–H₂O [where A is an alkali metal and Ln a rare earth (III) metal] have previously been investigated at various temperatures (Kost et al., 1980; Shirai et al., 1981; Lazorenko et al., 1983; Shirai et al., 1986; Storozhenko et al., 1987; Bunyakina et al., 1991; Bunyakina et al., 1992). However, all synthesized compounds were only characterized by powder X-ray diffraction and no single-crystal structures have been reported. The interest of other authors in these hydrated alkali metal/rare earth (III) chlorides was mainly based on the change of the coordination number of the rare earth ions and the parameters influencing these changes (Reuter et al., 1995; Fink et al., 1990).

To the best of our knowledge, only a few examples of divalent metal halide (MX₂) rare earth (III) halide (MX₃—H₂O) systems have been investigated. In the case of the SrCl₂–CdCl₂–H₂O and CeCl₃–CdCl₂–H₂O systems, the hydrated phases SrCd₂Cl₆·8H₂O and CeCd₄Cl₁₁.13H₂O were isolated and their structures were determined (Yahyaoui et al., 2002; Yahyaoui et al., 2003). The room-temperature form of the first compound crystallizes in the P-1 triclinic system and is characterized by pseudo-monoclinic symmetry and the occurrence of twinning by twofold rotation around the c axis. SrCd₂Cl₆·8H₂O undergoes a structural phase transition at 323 K, which is related to a change to higher symmetry and the disappearance of twinning. On the other hand, CeCd₄Cl₁₁.13H₂O crystallizes in the monoclinic system with P2₁ symmetry. In comparison with SrCd₂Cl₆·8H₂O, the substitution of strontium for cerium(III) cations leads to an increase of the symmetry, a disappearance of twinning phenomena and the preservation of the cation environments.

As part of our research, we have investigated the YbCl₃–CdCl₂–H₂O system, in order to study further the influence of the substitution of strontium and cerium cations on the structural properties the double chloride salts formed in these sytems. We report here the results of a structural investigation of a new double-salt hydrate, namely YbCd₃Cl₉.15H₂O. In contrast to CeCd₄Cl₁₁.13H₂O, the structural arrangement of YbCd₃Cl₉.15H₂O at room temperature is bidimensional (Fig. 1), with an increase in the unit-cell volume. Two types of octahedra are present around the cadmium cations; atoms Cd2 and Cd3 are each coordinated to six Cl atoms, while atom Cd1 is surrounded by five Cl atoms and one O atom (Table 2). Six of these octahedra share edges, thus generating short double chains that are themselves connected through atom Cl5 to form layers parallel to the (−1 1 1) plane (Figs. 1 and 2). These layers of double octahedral chains around Cd atoms have not been previously observed in complex hydrated cadmium chlorides, and the structural arrangement in YbCd₃Cl₉.15H₂O differs from the infinite double chains of CdCl₆ octahedra found in SrCd₂Cl₆·8H₂O and CeCd₄Cl₁₁.13H₂. The average Cd1—Cl, Cd2—Cl and Cd3—Cl distances in YbCd₃Cl₉.15H₂O are 2.626, 2.633 and 2.622 Å, respectively, and the Cd1—O distance is 2.322 (3) Å [cf. Cd—O = 2.374 (17) Å in CeCd₄Cl₁₁.13H₂O].

Three types of water molecules are present in the crystal structure of (I); the first type corresponds to six water molecules not coordinated to cations (atoms O10W–O15W), the second corresponds to the H₂O molecule (O9W) bonded to atom Cd1 and the last category contains the remaining water molecules coordinating the ytterbium ions (atoms O1W–O8W). The ytterbium coordination sphere consists of eight water molecules at the corners of a distorted square antiprism, with an average Yb—O distance equal to 2.312 Å (Figs. 1 and 2, and Table 2). These square antiprisms are intercalated between the layers of cadmium octahedra. Compound (I) is the first known example of a complex hydrated cadmium chloride showing such a coordination environment, it having previously been observed only in (CH₃NH₃)₃PrCl₆·2H₂O (Runge et al., 1990) and (CH₃NH₃)₈[NdCl₆][NdCl₄(H₂O) ₂]₂Cl₃ (Runge et al., 1991). The coordination number of the rare-earth(III) ion decreases from nine in CeCd₄Cl₁₁.13H₂O to eight in YbCd₃Cl₉.15H₂O, in conjunction with a decrease of the rare-earth(III)–oxygen distance (cf. <Ce—O> = 2.542 Å).

A comparison can be made between the structures of YbCd₃Cl₉.15H₂O and SrCd₂Cl₆·8H₂O. The triclinic Sr compound was found to be twinned with a pseudo-monoclinic face-centered unit cell related to the triclinic unit-cell by the 100/001/1–4-1 transformation matrix. In SrCd₂Cl₆·8H₂O, pairs of Cd, Cl and O atoms are related by a c/2 pseudo-translation, whereas in YbCd₃Cl₉.15H₂O, similar atoms are related by a true b/2 translation. The twin rotation axis parallel to c in the Sr compound is replaced by a real 2₁ axis parallel to b in the Yb compound.

A projection view of the title compound, illustrating the hydrogen bonding, is depicted in Fig. 1. The hydrogen bonds are of two types, namely O—H^···Cl and O—H^···O (Table 3). The O—H^···Cl bonds appear between layers of cadmium octahedra and water molecules, with distances ranging from 3.130 (3) to 3.346 (4) Å. Atoms Cl6, Cl7 and Cl9 atoms are each bonded to one Cd atom and establish the most hydrogen bonds; atom Cl9 forms four hydrogen bonds, and atoms Cl6 and Cl7 are involved in three hydrogen bonds. Atoms Cl1, Cl2, Cl5 and Cl8 atoms each bridge two Cd atoms and participate in fewer hydrogen bonds, i.e. one for atom Cl2 and two for atoms Cl1, Cl and Cl8. Atoms Cl3 and Cl4 are each bonded to three cd atoms and, whereas atom Cl3 is not involved in any hydrogen bonds, atom Cl4 can be considered to be engaged in a weak hydrogen bond with one water molecule (O6W). O—H···O hydrogen bonds connect the water molecules surrounding the ytterbium ions to water molecules not coordinated to cations, and only atoms O1W and O5W are not involved in any hydrogen bonds. The associated O···O distances vary from 2.681 (4) to 3.202 (5) Å.

S2. Experimental

Colorless single crystals of YbCd₃Cl₉.15H₂O were grown from a heated mixture (T= 363 K) of ytterbium oxide Yb₂O₃(0.9852 g) and cadmium chloride CdCl₂·H₂O (1.14 g) in HCl solution (18 M) in a 1:4 molar ratio. This solution was allowed to evaporate slowly to dryness at 278 K and twinned needle shaped crystals were obtained. Susequently, several recrystallizations in acetone and methanol were performed, yielding colorless, transparent and parallelepiped-shaped single crystals. The hydrated double salt was characterized by X-ray powder diffraction, elemental chemical analysis and thermogravimetric studies in order to determine the water content. The formula was confirmed by density measurement and the refinement of the crystal structure.

S3. Refinement

All H atoms were found in difference Fourier maps but were introduced into the refinement as fixed contributors with U_iso values fixed at 0.06 Ų. The maximum electron-density residual peak is located 0.93 Šfrom the Yb atom and the largest hole is 0.90 Šfrom the same atom.

Computing details

Data collection: IPDS Software (Stoe & Cie, 1996); cell refinement: IPDS Software; data reduction: X-RED (Stoe & Cie, 1996); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXL97.

Figures

	Fig. 1. : A projection of the structure of YbCd3Cl9.15H2O on to the (001) plane. Hydrogen bonds are shown as dashed lines (blue for O—H···O bonds and purple for O—H···Cl bonds in the online version of the journal).
	Fig. 2. : A polyhedral representation of YbCd3Cl9.15H2O projected on to the (001) plane.

(I)

Crystal data

[Yb(H2O)8][Cd3Cl9(H2O)]·6H2O	F(000) = 2068
Mr = 1099.53	Dx = 2.641 Mg m^−3 Dm = 2.611 Mg m^−3 Dm measured by picnometry
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
a = 12.2692 (12) Å	Cell parameters from 8000 reflections
b = 20.057 (2) Å	θ = 2.7–28.1°
c = 12.2820 (13) Å	µ = 6.55 mm^−1
β = 113.803 (11)°	T = 293 K
V = 2765.3 (5) Å^3	Prism, colorless
Z = 4	0.30 × 0.15 × 0.11 mm

Data collection

Stoe IPDS image-plate diffractometer	5551 reflections with I > 2σ(I)
ϕ scans	Rint = 0.037
Absorption correction: multi-scan Symmetry-related measurements (Blessing R.H., 1995)	θmax = 26.4°, θmin = 2.7°
Tmin = 0.234, Tmax = 0.487	h = −15→15
22337 measured reflections	k = −25→25
5583 independent reflections	l = −15→15

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	H-atom parameters not refined
R[F^2 > 2σ(F^2)] = 0.027	w = 1/[σ^2(Fo^2) + (0.0237P)^2 + 7.9527P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.064	(Δ/σ)max = 0.001
S = 1.29	Δρmax = 1.30 e Å^−3
5583 reflections	Δρmin = −1.37 e Å^−3
254 parameters

Special details

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
O1W	0.5288 (2)	0.13359 (14)	0.1917 (3)	0.0190 (6)
O2W	0.5499 (3)	0.03709 (16)	0.3597 (3)	0.0274 (7)
O3W	0.3997 (3)	0.03810 (16)	0.0328 (3)	0.0246 (7)
O4W	0.3919 (3)	−0.04907 (15)	0.2016 (3)	0.0232 (7)
O5W	0.1831 (3)	0.03346 (19)	0.0766 (3)	0.0295 (8)
O6W	0.2808 (3)	0.03299 (15)	0.3214 (3)	0.0202 (6)
O7W	0.2810 (3)	0.15819 (15)	0.0994 (3)	0.0266 (7)
O8W	0.4082 (3)	0.14753 (14)	0.3451 (3)	0.0180 (6)
O9W	0.1145 (4)	−0.1289 (2)	−0.0251 (3)	0.0392 (9)
O10W	0.5397 (3)	−0.11698 (15)	0.1160 (3)	0.0202 (6)
O11W	0.2595 (3)	−0.12971 (15)	−0.7199 (3)	0.0231 (6)
O12W	0.0543 (3)	0.18712 (16)	−0.0416 (3)	0.0243 (7)
O13W	0.3495 (3)	0.08114 (15)	0.5457 (3)	0.0204 (6)
O14W	0.2460 (3)	0.24517 (16)	0.3246 (3)	0.0230 (6)
O15W	0.6441 (3)	0.1617 (2)	0.4794 (3)	0.0327 (8)
Cl1	0.25058 (8)	−0.06585 (4)	−0.16893 (8)	0.01562 (19)
Cl2	0.17734 (8)	−0.22504 (5)	−0.35945 (8)	0.01651 (18)
Cl3	0.11762 (8)	−0.05316 (5)	−0.50273 (8)	0.01420 (17)
Cl4	−0.04803 (8)	−0.11968 (4)	−0.34331 (8)	0.01398 (17)
Cl5	0.35158 (8)	−0.22862 (5)	−0.02754 (8)	0.01664 (18)
Cl6	0.02429 (9)	−0.27641 (5)	−0.14161 (10)	0.0231 (2)
Cl7	0.05083 (9)	−0.21747 (5)	−0.68159 (8)	0.01752 (19)
Cl8	−0.18369 (8)	−0.10367 (5)	−0.68271 (8)	0.01576 (18)
Cl9	−0.01707 (8)	0.03583 (5)	−0.17868 (8)	0.01748 (19)
Cd1	0.14417 (2)	−0.183803 (14)	−0.17724 (3)	0.01466 (7)
Cd2	−0.01025 (2)	−0.170568 (14)	−0.52435 (2)	0.01333 (7)
Cd3	0.06851 (2)	−0.005187 (14)	−0.32702 (2)	0.01304 (7)
Yb1	0.377998 (14)	0.065643 (8)	0.203399 (14)	0.01206 (6)
H11	0.5248	0.1787	0.1889	0.060*
H12	0.5971	0.1226	0.1839	0.060*
H21	0.6150	0.0622	0.3939	0.060*
H22	0.5788	−0.0056	0.3820	0.060*
H31	0.4087	0.0045	−0.0070	0.060*
H32	0.3994	0.0764	−0.0144	0.060*
H41	0.3472	−0.0794	0.2286	0.060*
H42	0.4385	−0.0753	0.1773	0.060*
H51	0.1415	0.0425	0.0012	0.060*
H52	0.1356	0.0139	0.0948	0.060*
H61	0.2092	0.0096	0.2920	0.060*
H62	0.2842	0.0469	0.3822	0.060*
H71	0.1992	0.1640	0.0410	0.060*
H72	0.3190	0.1994	0.0993	0.060*
H81	0.3649	0.1804	0.3372	0.060*
H82	0.4861	0.1642	0.4036	0.060*
H91	0.0568	−0.1433	0.0034	0.060*
H92	0.1280	−0.0880	−0.0049	0.060*
H101	0.4894	−0.1477	0.0679	0.060*
H102	0.5998	−0.1461	0.1834	0.060*
H111	0.1947	−0.1164	−0.7395	0.060*
H112	0.2494	−0.1678	−0.7636	0.060*
H121	0.0392	0.2298	−0.0222	0.060*
H122	0.0384	0.1956	−0.1164	0.060*
H131	0.3030	0.0907	0.5764	0.060*
H132	0.3858	0.1235	0.5426	0.060*
H141	0.2464	0.2473	0.3902	0.060*
H142	0.1598	0.2430	0.2797	0.060*
H151	0.6875	0.1607	0.5590	0.060*
H152	0.6902	0.1771	0.4494	0.060*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
O1W	0.0157 (13)	0.0135 (13)	0.0332 (16)	−0.0019 (11)	0.0153 (13)	−0.0007 (12)
O2W	0.0203 (15)	0.0168 (15)	0.0301 (17)	0.0001 (12)	−0.0055 (13)	0.0030 (13)
O3W	0.0404 (19)	0.0203 (15)	0.0212 (15)	−0.0089 (14)	0.0211 (14)	−0.0063 (12)
O4W	0.0306 (17)	0.0133 (14)	0.0355 (18)	−0.0002 (12)	0.0236 (15)	−0.0023 (12)
O5W	0.0182 (15)	0.045 (2)	0.0198 (15)	−0.0136 (14)	0.0018 (12)	0.0079 (14)
O6W	0.0200 (14)	0.0256 (16)	0.0195 (14)	−0.0091 (12)	0.0126 (12)	−0.0053 (12)
O7W	0.0181 (15)	0.0162 (15)	0.0348 (18)	0.0013 (12)	−0.0005 (13)	0.0086 (13)
O8W	0.0163 (13)	0.0170 (14)	0.0213 (14)	−0.0008 (11)	0.0081 (11)	−0.0058 (11)
O9W	0.051 (2)	0.042 (2)	0.041 (2)	−0.0133 (18)	0.0355 (19)	−0.0143 (17)
O10W	0.0206 (14)	0.0186 (14)	0.0220 (14)	−0.0004 (12)	0.0091 (12)	−0.0009 (12)
O11W	0.0198 (15)	0.0202 (15)	0.0325 (17)	−0.0041 (12)	0.0137 (13)	−0.0003 (13)
O12W	0.0239 (16)	0.0252 (16)	0.0197 (15)	0.0047 (13)	0.0048 (13)	0.0001 (12)
O13W	0.0207 (15)	0.0201 (15)	0.0244 (15)	0.0022 (12)	0.0131 (12)	0.0000 (12)
O14W	0.0222 (15)	0.0270 (16)	0.0227 (15)	0.0014 (13)	0.0120 (13)	−0.0011 (12)
O15W	0.0174 (15)	0.054 (2)	0.0254 (17)	−0.0083 (15)	0.0072 (13)	−0.0013 (16)
Cl1	0.0125 (4)	0.0137 (4)	0.0184 (4)	0.0011 (3)	0.0039 (4)	−0.0002 (3)
Cl2	0.0156 (4)	0.0187 (4)	0.0157 (4)	0.0038 (4)	0.0068 (3)	0.0008 (3)
Cl3	0.0131 (4)	0.0150 (4)	0.0148 (4)	0.0004 (3)	0.0060 (3)	−0.0006 (3)
Cl4	0.0129 (4)	0.0131 (4)	0.0167 (4)	−0.0005 (3)	0.0068 (3)	−0.0011 (3)
Cl5	0.0144 (4)	0.0163 (4)	0.0188 (4)	0.0035 (3)	0.0063 (4)	0.0019 (3)
Cl6	0.0194 (5)	0.0206 (5)	0.0309 (5)	−0.0004 (4)	0.0118 (4)	0.0075 (4)
Cl7	0.0223 (5)	0.0154 (4)	0.0191 (4)	0.0013 (4)	0.0126 (4)	0.0000 (3)
Cl8	0.0131 (4)	0.0149 (4)	0.0178 (4)	−0.0007 (3)	0.0046 (3)	0.0013 (3)
Cl9	0.0154 (4)	0.0220 (5)	0.0166 (4)	−0.0016 (4)	0.0082 (4)	−0.0036 (4)
Cd1	0.01379 (14)	0.01606 (14)	0.01483 (14)	0.00063 (10)	0.00649 (11)	0.00156 (10)
Cd2	0.01360 (14)	0.01250 (14)	0.01439 (14)	0.00098 (10)	0.00616 (11)	−0.00054 (10)
Cd3	0.01390 (14)	0.01207 (14)	0.01372 (14)	0.00078 (10)	0.00618 (11)	0.00028 (10)
Yb1	0.01166 (9)	0.01163 (9)	0.01377 (9)	−0.00127 (6)	0.00605 (7)	−0.00058 (6)

Geometric parameters (Å, º)

O1W—Yb1	2.349 (3)	O11W—H112	0.912
O1W—H11	0.906	O12W—H121	0.927
O1W—H12	0.908	O12W—H122	0.876
O2W—Yb1	2.279 (3)	O13W—H131	0.824
O2W—H21	0.893	O13W—H132	0.967
O2W—H22	0.925	O14W—H141	0.805
O3W—Yb1	2.283 (3)	O14W—H142	0.976
O3W—H31	0.866	O15W—H151	0.905
O3W—H32	0.962	O15W—H152	0.849
O4W—Yb1	2.308 (3)	Cl1—Cd3	2.596 (1)
O4W—H41	0.964	Cl1—Cd1	2.684 (1)
O4W—H42	0.911	Cl2—Cd1	2.568 (1)
O5W—Yb1	2.356 (3)	Cl2—Cd2	2.613 (1)
O5W—H51	0.877	Cl3—Cd3	2.645 (1)
O5W—H52	0.806	Cl3—Cd3^i	2.665 (1)
O6W—Yb1	2.312 (3)	Cl3—Cd2	2.782 (1)
O6W—H61	0.931	Cl4—Cd2	2.652 (1)
O6W—H62	0.782	Cl4—Cd3	2.670 (1)
O7W—Yb1	2.295 (3)	Cl4—Cd1	2.737 (1)
O7W—H71	0.977	Cl5—Cd1	2.624 (1)
O7W—H72	0.949	Cl5—Cd2^ii	2.629 (1)
O8W—Yb1	2.311 (3)	Cl6—Cd1	2.515 (1)
O8W—H81	0.828	Cl7—Cd2	2.519 (1)
O8W—H82	0.993	Cl8—Cd3^i	2.577 (1)
O9W—Cd1	2.320 (3)	Cl8—Cd2	2.602 (1)
O9W—H91	0.952	Cl9—Cd3	2.577 (1)
O9W—H92	0.855	Cd2—Cl5^iii	2.629 (1)
O10W—H101	0.902	Cd3—Cl8^i	2.577 (1)
O10W—H102	1.038	Cd3—Cl3^i	2.665 (1)
O11W—H111	0.779
Yb1—O1W—H11	123.4	Cl7—Cd2—Cl8	91.50 (3)
Yb1—O1W—H12	130.5	Cl7—Cd2—Cl2	89.80 (3)
H11—O1W—H12	106.0	Cl8—Cd2—Cl2	173.50 (3)
Yb1—O2W—H21	127.1	Cl7—Cd2—Cl5^iii	95.22 (3)
Yb1—O2W—H22	126.6	Cl8—Cd2—Cl5^iii	93.30 (3)
H21—O2W—H22	102.7	Cl2—Cd2—Cl5^iii	92.92 (3)
Yb1—O3W—H31	142.7	Cl7—Cd2—Cl4	173.40 (3)
Yb1—O3W—H32	112.8	Cl8—Cd2—Cl4	93.51 (3)
H31—O3W—H32	104.5	Cl2—Cd2—Cl4	84.74 (3)
Yb1—O4W—H41	124.8	Cl5^iii—Cd2—Cl4	88.77 (3)
Yb1—O4W—H42	129.6	Cl7—Cd2—Cl3	93.35 (3)
H41—O4W—H42	105.5	Cl8—Cd2—Cl3	83.94 (3)
Yb1—O5W—H51	130.1	Cl2—Cd2—Cl3	89.63 (3)
Yb1—O5W—H52	127.2	Cl5^iii—Cd2—Cl3	171.06 (3)
H51—O5W—H52	102.4	Cl4—Cd2—Cl3	82.93 (3)
Yb1—O6W—H61	123.0	Cl8^i—Cd3—Cl9	93.96 (3)
Yb1—O6W—H62	130.9	Cl8^i—Cd3—Cl1	94.14 (3)
H61—O6W—H62	103.2	Cl9—Cd3—Cl1	95.39 (3)
Yb1—O7W—H71	130.8	Cl8^i—Cd3—Cl3	92.57 (3)
Yb1—O7W—H72	124.1	Cl9—Cd3—Cl3	170.01 (3)
H71—O7W—H72	104.8	Cl1—Cd3—Cl3	91.67 (3)
Yb1—O8W—H81	125.3	Cl8^i—Cd3—Cl3^i	86.82 (3)
Yb1—O8W—H82	126.8	Cl9—Cd3—Cl3^i	87.13 (3)
H81—O8W—H82	101.6	Cl1—Cd3—Cl3^i	177.23 (3)
Cd1—O9W—H91	122.3	Cl3—Cd3—Cl3^i	85.69 (3)
Cd1—O9W—H92	127.9	Cl8^i—Cd3—Cl4	177.83 (3)
H91—O9W—H92	105.7	Cl9—Cd3—Cl4	88.21 (3)
H101—O10W—H102	102.5	Cl1—Cd3—Cl4	85.76 (3)
H111—O11W—H112	103.1	Cl3—Cd3—Cl4	85.27 (3)
H121—O12W—H122	96.2	Cl3^i—Cd3—Cl4	93.18 (3)
H131—O13W—H132	103.2	O2W—Yb1—O3W	107.51 (13)
H141—O14W—H142	97.8	O2W—Yb1—O7W	140.16 (11)
H151—O15W—H152	105.7	O3W—Yb1—O7W	84.91 (13)
Cd3—Cl1—Cd1	97.25 (3)	O2W—Yb1—O4W	73.18 (12)
Cd1—Cl2—Cd2	98.10 (3)	O3W—Yb1—O4W	73.35 (11)
Cd3—Cl3—Cd3^i	94.31 (3)	O7W—Yb1—O4W	145.56 (12)
Cd3—Cl3—Cd2	94.61 (3)	O2W—Yb1—O8W	74.44 (11)
Cd3^i—Cl3—Cd2	91.44 (3)	O3W—Yb1—O8W	145.07 (11)
Cd2—Cl4—Cd3	97.14 (3)	O7W—Yb1—O8W	74.57 (12)
Cd2—Cl4—Cd1	93.12 (3)	O4W—Yb1—O8W	136.53 (11)
Cd3—Cl4—Cd1	94.25 (3)	O2W—Yb1—O6W	86.40 (12)
Cd1—Cl5—Cd2^ii	135.32 (4)	O3W—Yb1—O6W	141.90 (11)
Cd3^i—Cl8—Cd2	97.73 (3)	O7W—Yb1—O6W	107.17 (12)
O9W—Cd1—Cl6	85.25 (10)	O4W—Yb1—O6W	77.45 (11)
O9W—Cd1—Cl2	170.47 (10)	O8W—Yb1—O6W	72.31 (10)
Cl6—Cd1—Cl2	102.90 (4)	O2W—Yb1—O1W	73.32 (11)
O9W—Cd1—Cl5	91.21 (11)	O3W—Yb1—O1W	72.43 (11)
Cl6—Cd1—Cl5	95.45 (3)	O7W—Yb1—O1W	74.99 (11)
Cl2—Cd1—Cl5	92.88 (3)	O4W—Yb1—O1W	120.97 (10)
O9W—Cd1—Cl1	77.50 (10)	O8W—Yb1—O1W	75.08 (10)
Cl6—Cd1—Cl1	162.57 (4)	O6W—Yb1—O1W	145.18 (10)
Cl2—Cd1—Cl1	94.09 (3)	O2W—Yb1—O5W	146.63 (12)
Cl5—Cd1—Cl1	87.48 (3)	O3W—Yb1—O5W	77.89 (12)
O9W—Cd1—Cl4	90.53 (11)	O7W—Yb1—O5W	72.17 (12)
Cl6—Cd1—Cl4	95.06 (3)	O4W—Yb1—O5W	77.29 (12)
Cl2—Cd1—Cl4	83.91 (3)	O8W—Yb1—O5W	120.26 (12)
Cl5—Cd1—Cl4	169.45 (3)	O6W—Yb1—O5W	72.20 (11)
Cl1—Cd1—Cl4	82.75 (3)	O1W—Yb1—O5W	137.12 (11)

Symmetry codes: (i) −x, −y, −z−1; (ii) x+1/2, −y−1/2, z+1/2; (iii) x−1/2, −y−1/2, z−1/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H11···Cl7^iv	0.906	2.267	3.130 (3)	159.06
O10W—H101···Cl5	0.902	2.296	3.188 (3)	170.04
O1W—H12···Cl1^v	0.908	2.258	3.141 (3)	163.75
O2W—H21···O15W	0.893	2.215	2.893 (5)	132.35
O2W—H22···O13W^vi	0.925	1.800	2.709 (4)	168.50
O3W—H31···Cl1	0.866	2.568	3.190 (3)	129.51
O3W—H32···O10W^v	0.962	1.880	2.738 (4)	147.26
O4W—H41···O11W^vii	0.964	1.768	2.730 (4)	175.63
O4W—H42···O10W	0.911	1.887	2.791 (4)	170.75
O5W—H51···Cl9	0.877	2.284	3.106 (3)	156.20
O5W—H52···Cl9^viii	0.806	2.320	3.117 (3)	170.52
O6W—H61···Cl9^viii	0.931	2.382	3.297 (3)	167.40
O6W—H62···O13W	0.782	1.962	2.713 (4)	160.81
O7W—H71···O12W	0.977	1.717	2.681 (4)	167.92
O7W—H72···Cl7^iv	0.949	2.247	3.133 (3)	154.94
O8W—H81···O14W	0.828	1.912	2.731 (4)	169.56
O8W—H82···O15W	0.993	1.781	2.706 (4)	153.50
O9W—H91···O12W^viii	0.952	1.834	2.773 (5)	167.99
O9W—H92···O5W	0.855	2.617	3.469 (5)	174.64
O10W—H102···Cl8^ix	1.038	2.638	3.306 (3)	121.91
O11W—H111···Cl9^i	0.779	2.570	3.309 (3)	159.25
O11W—H112···O14W^x	0.912	1.911	2.808 (5)	167.82
O12W—H121···O15W^xi	0.927	2.525	3.202 (5)	130.11
O12W—H121···Cl6^viii	0.927	2.606	3.310 (3)	133.02
O12W—H122···Cl7^i	0.876	2.314	3.171 (3)	166.07
O13W—H131···Cl8^viii	0.824	2.336	3.153 (3)	171.11
O13W—H132···O8W	0.967	2.595	3.130 (4)	115.11
O13W—H132···Cl6^xii	0.967	2.376	3.236 (3)	148.02
O14W—H141···Cl5^xii	0.805	2.482	3.214 (3)	151.84
O14W—H142···Cl6^viii	0.976	2.310	3.229 (3)	156.50
O15W—H151···O11W^v	0.905	1.918	2.778 (5)	157.89
O15W—H152···Cl2^v	0.849	2.497	3.346 (4)	178.58

Symmetry codes: (i) −x, −y, −z−1; (iv) −x+1/2, y+1/2, −z−1/2; (v) −x+1, −y, −z; (vi) −x+1, −y, −z+1; (vii) x, y, z+1; (viii) −x, −y, −z; (ix) x+1, y, z+1; (x) −x+1/2, y−1/2, −z−1/2; (xi) x−1/2, −y+1/2, z−1/2; (xii) −x+1/2, y+1/2, −z+1/2.