Na3DyCl6

Schurz, C.M.; Meyer, G.; Schleid, T.

doi:10.1107/S1600536811014498

inorganic compounds

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ISSN: 2056-9890

Volume 67| Part 5| May 2011| Page i33

doi:10.1107/S1600536811014498

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Na₃DyCl₆

Christian M. Schurz,^a Gerd Meyer ^b and Thomas Schleid ^a ^*

^aInstitut für Anorganische Chemie, Universität Stuttgart, Pfaffenwaldring 55, 70569 Stuttgart, Germany, and ^bDepartment für Chemie, Institut für Anorganische Chemie, Universität zu Köln, Greinstrasse 6, 50939 Köln, Germany
^*Correspondence e-mail: schleid@iac.uni-stuttgart.de

(Received 6 April 2011; accepted 18 April 2011; online 29 April 2011)

Single crystals of the title compound, trisodium hexachloridodysprosate, Na₃DyCl₆, were obtained as a by-product of synthesis using dysprosium(III) chloride and sodium chloride among others. The monoclinic structure with its typical β angle close to 90° [90.823 (4)°] is isotypic with the mineral cryolite (Na₃AlF₆) and the high-temperature structure of the Na₃MCl₆ series, with M = Eu–Lu, Y and Sc. The isolated, almost perfect [DyCl₆]³⁻ octahedra are interconnected via two crystallographically different Na⁺ cations: while one Na⁺ resides on centres of symmetry (as well as Dy³⁺) and also builds almost perfect, isolated [NaCl₆]⁵⁻ octahedra, the other Na⁺ is surrounded by seven chloride anions forming a distorted [NaCl₇]⁶⁻ trigonal prism with just one cap as close secondary contact.

Related literature

The first structural descriptions of the Na₃MCl₆ series (M = Eu–Lu, Y and Sc) on a single crystal in the cryolite-type structure (Hawthorne &, Ferguson, 1975 ) were given for M = Er by Meyer et al. (1987 ), for M = Ho by Böcker et al. (2001 ) and for M = Y by Liao & Dronskowski (2004 ). For the correlation between the two temperature-dependent phases, see: Meyer (1984 ); Meyer et al. (1987); Wickleder & Meyer (1995 ). For a planned synthesis of Dy₂NCl₃, compare with those for Gd₂NCl₃ (Schwanitz-Schüller & Simon, 1985 ) and Y₂NCl₃ (Meyer et al., 1989 ).

Experimental

Crystal data

Na₃DyCl₆
M_r = 444.17
Monoclinic, P 2₁ /n
a = 6.8791 (5) Å
b = 7.2816 (5) Å
c = 10.1734 (7) Å
β = 90.823 (4)°
V = 509.54 (6) Å³
Z = 2
Mo Kα radiation
μ = 8.96 mm⁻¹
T = 293 K
0.20 × 0.15 × 0.10 mm

Data collection

Nonius Kappa-CCD diffractometer
Absorption correction: numerical (X-SHAPE; Stoe & Cie 1999 ) T_min = 0.218, T_max = 0.414
12026 measured reflections
1245 independent reflections
1124 reflections with I > 2σ(I)
R_int = 0.071

Refinement

R[F² > 2σ(F²)] = 0.019
wR(F²) = 0.045
S = 1.08
1245 reflections
50 parameters
Δρ_max = 0.84 e Å⁻³
Δρ_min = −1.05 e Å⁻³

Table 1
Selected bond lengths (Å)

Na1—Cl2ⁱ	2.7358 (8)
Na1—Cl3ⁱⁱⁱ	2.7902 (8)
Na1—Cl1	2.8687 (8)
Na2—Cl1	2.8295 (19)
Na2—Cl2^vi	2.8341 (19)
Na2—Cl1^iv	2.8492 (19)
Na2—Cl3ⁱ	2.8612 (19)
Na2—Cl3^vii	3.204 (2)
Na2—Cl2^iv	3.325 (2)
Na2—Cl2	3.488 (2)
Dy—Cl2	2.6176 (8)
Dy—Cl3	2.6320 (8)
Dy—Cl1^viii	2.6447 (8)
Symmetry codes: (i) $[x+{\script{1\over 2}}, -y+{\script{1\over 2}}, z+{\script{1\over 2}}]$ ; (iii) $[x-{\script{1\over 2}}, -y+{\script{1\over 2}}, z+{\script{1\over 2}}]$ ; (iv) $[-x+{\script{1\over 2}}, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (vi) x+1, y, z; (vii) -x+1, -y, -z; (viii) -x, -y, -z.

Data collection: COLLECT (Nonius, 1998 ); cell refinement: SCALEPACK (Otwinowski & Minor, 1997 ); data reduction: SCALEPACK and DENZO (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2006 ); software used to prepare material for publication: SHELXL97.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536811014498/hp2006sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536811014498/hp2006Isup2.hkl

checkCIF report

Comment top

Trisodiumhexachlorodysprosate(III) belongs to a group of ternary chlorides Na₃MCl₆ with M = Eu – Lu, Y and Sc (Meyer et al., 1987), which crystallize in the cryolite-type structure (Hawthorne et al., 1975). The Dy³⁺ and (Na1)⁺ occupy the 2a and 2b Wyckoff positions at centres of symmetry, whereas the three crystallographically different chloride anions and (Na2)⁺ reside at the 4e position with the site symmetry 1. A l l cations have six primary contacts to Cl^-, but the [(Na2)Cl₆]^5- polyhedron can not only be described as distorted trigonal prism instead of the usual octahedra that are realised for [DyCl₆]^3- and [(Na1)Cl₆]^5-, it moreover carries a seventh capping Cl^- anion. The isolated [DyCl₆]^3- octahedra are interconnected to a three-dimensional texture via sodium cations (Fig. 1). This structure represents the high-temperature phase of the Na₃MCl₆ series with M = Eu – Lu, Y and Sc. The transition into the low-temperature phase with its trigonal structure (Meyer, 1984) depends on the radius of the actual lanthanoid(III) cation (Wickleder et al., 1995) and is estimated for M = Dy at around 290 K, hence not far below the temperature of the measurement.

Related literature top

The first structural descriptions of the Na₃MCl₆ series (Eu–Lu, Y and Sc) on a single crystal in the cryolite-type structure (Hawthorne et al., 1975) were given for M = Er by Meyer et al. (1987), for M = Ho by Böcker et al. (2001) and for M = Y by Liao et al. (2004). For the correlation between the two temperature-dependent phases, see: Meyer (1984); Meyer et al. (1987); Wickleder et al. (1995).

For related literature, see: Meyer et al. (1989); Schwanitz-Schüller & Simon (1985).

Experimental top

Colourless and transparent single crystals of Na₃DyCl₆ were obtained as by-product from the reaction of sodium azide (NaN₃), dysprosium metal (Dy) and its the corresponding trichloride (DyCl₃) in presence of sodium chloride (NaCl) as flux, originally designed to produce Dy₂NCl₃ in analogy to Gd₂NCl₃ (Schwanitz-Schüller et al., 1985) and Y₂NCl₃ (Meyer et al., 1989) instead. The reaction mixture was placed into a torch- sealed evacuated fused-silica vessel, which was heated at 1143 K for seven days, followed by cooling to room temperature within one day.

Computing details top

Data collection: COLLECT (Nonius, 1998); cell refinement: SCALEPACK (Otwinowski & Minor, 1997); data reduction: SCALEPACK and DENZO (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2006); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top

Fig. 1. Crystal structure of cryolite-type Na₃DyCl₆. Displacement ellipsoids are drawn at 90% probability level.

Trisodium hexachloridodysprosate top

Crystal data top

Na₃DyCl₆	F(000) = 402
M_r = 444.17	D_x = 2.895 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71069 Å
Hall symbol: -p2yn	Cell parameters from 8457 reflections
a = 6.8791 (5) Å	θ = 3.4–28.1°
b = 7.2816 (5) Å	µ = 8.96 mm⁻¹
c = 10.1734 (7) Å	T = 293 K
β = 90.823 (4)°	Block, colourless
V = 509.54 (6) Å³	0.20 × 0.15 × 0.10 mm
Z = 2

Data collection top

Nonius KappaCCD diffractometer	1245 independent reflections
Radiation source: fine-focus sealed tube	1124 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.071
charge cpouled device scans	θ_max = 28.1°, θ_min = 3.4°
Absorption correction: numerical (X-SHAPE; Stoe & Cie 1999)	h = −9→9
T_min = 0.218, T_max = 0.414	k = −9→9
12026 measured reflections	l = −13→13

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.019	w = 1/[σ²(F_o²) + (0.0199P)² + 0.2881P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.045	(Δ/σ)_max < 0.001
S = 1.08	Δρ_max = 0.84 e Å⁻³
1245 reflections	Δρ_min = −1.05 e Å⁻³
50 parameters	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0043 (5)

Crystal data top

Na₃DyCl₆	V = 509.54 (6) Å³
M_r = 444.17	Z = 2
Monoclinic, P2₁/n	Mo Kα radiation
a = 6.8791 (5) Å	µ = 8.96 mm⁻¹
b = 7.2816 (5) Å	T = 293 K
c = 10.1734 (7) Å	0.20 × 0.15 × 0.10 mm
β = 90.823 (4)°

Data collection top

Nonius KappaCCD diffractometer	1245 independent reflections
Absorption correction: numerical (X-SHAPE; Stoe & Cie 1999)	1124 reflections with I > 2σ(I)
T_min = 0.218, T_max = 0.414	R_int = 0.071
12026 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.019	50 parameters
wR(F²) = 0.045	0 restraints
S = 1.08	Δρ_max = 0.84 e Å⁻³
1245 reflections	Δρ_min = −1.05 e Å⁻³

Special details top

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 (Å²) top

	x	y	z	U_iso*/U_eq
Na1	0.0000	0.0000	0.5000	0.0291 (4)
Na2	0.5218 (2)	−0.0749 (2)	0.24225 (18)	0.0499 (4)
Dy	0.0000	0.0000	0.0000	0.01593 (9)
Cl1	0.13816 (12)	0.06522 (12)	0.23941 (8)	0.02834 (18)
Cl2	−0.31489 (12)	0.17894 (12)	0.06382 (9)	0.0358 (2)
Cl3	0.16836 (13)	0.30521 (11)	−0.07742 (9)	0.0358 (2)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Na1	0.0323 (11)	0.0244 (10)	0.0303 (10)	−0.0038 (7)	−0.0033 (9)	0.0027 (7)
Na2	0.0462 (9)	0.0341 (9)	0.0694 (12)	−0.0069 (7)	0.0029 (8)	0.0033 (8)
Dy	0.01762 (12)	0.01512 (12)	0.01509 (12)	−0.00060 (6)	0.00126 (7)	−0.00138 (6)
Cl1	0.0334 (4)	0.0333 (4)	0.0182 (3)	0.0032 (3)	−0.0037 (3)	−0.0035 (3)
Cl2	0.0322 (4)	0.0323 (4)	0.0431 (5)	0.0149 (3)	0.0120 (4)	0.0090 (4)
Cl3	0.0350 (4)	0.0271 (4)	0.0450 (5)	−0.0123 (3)	−0.0069 (4)	0.0122 (4)

Geometric parameters (Å, º) top

Na1—Cl2ⁱ	2.7358 (8)	Na2—Dy^iv	4.0608 (17)
Na1—Cl2ⁱⁱ	2.7358 (8)	Na2—Na1^x	4.2126 (17)
Na1—Cl3ⁱⁱⁱ	2.7902 (8)	Dy—Cl2	2.6176 (8)
Na1—Cl3^iv	2.7902 (8)	Dy—Cl2^xii	2.6176 (8)
Na1—Cl1	2.8687 (8)	Dy—Cl3	2.6320 (8)
Na1—Cl1^v	2.8687 (8)	Dy—Cl3^xii	2.6320 (8)
Na1—Na2^vi	3.9579 (18)	Dy—Cl1^xii	2.6447 (8)
Na1—Na2^vii	3.9580 (18)	Dy—Cl1	2.6447 (8)
Na1—Na2^viii	4.2126 (17)	Dy—Na2^xiii	4.0608 (17)
Na1—Na2^ix	4.2126 (17)	Dy—Na2^vi	4.0608 (17)
Na2—Cl1	2.8295 (19)	Cl1—Na2^vi	2.8492 (19)
Na2—Cl2^x	2.8341 (19)	Cl2—Na1^xiv	2.7358 (8)
Na2—Cl1^iv	2.8492 (19)	Cl2—Na2^viii	2.8342 (19)
Na2—Cl3ⁱ	2.8612 (19)	Cl2—Na2^vi	3.325 (2)
Na2—Cl3^xi	3.204 (2)	Cl2—Na2	3.488 (2)
Na2—Cl2^iv	3.325 (2)	Cl3—Na1^vi	2.7902 (8)
Na2—Cl2	3.488 (2)	Cl3—Na2^xv	2.8611 (19)
Na2—Na1^iv	3.9580 (18)	Cl3—Na2^xi	3.204 (2)

Cl2ⁱ—Na1—Cl2ⁱⁱ	180.0	Cl3^xi—Na2—Na1^iv	44.32 (3)
Cl2ⁱ—Na1—Cl3ⁱⁱⁱ	90.49 (3)	Cl2^iv—Na2—Na1^iv	88.01 (4)
Cl2ⁱⁱ—Na1—Cl3ⁱⁱⁱ	89.51 (3)	Cl1—Na2—Dy^iv	103.79 (5)
Cl2ⁱ—Na1—Cl3^iv	89.51 (3)	Cl2^x—Na2—Dy^iv	158.34 (6)
Cl2ⁱⁱ—Na1—Cl3^iv	90.49 (3)	Cl1^iv—Na2—Dy^iv	40.43 (3)
Cl3ⁱⁱⁱ—Na1—Cl3^iv	180.0	Cl3ⁱ—Na2—Dy^iv	97.19 (5)
Cl2ⁱ—Na1—Cl1	85.33 (3)	Cl3^xi—Na2—Dy^iv	88.29 (4)
Cl2ⁱⁱ—Na1—Cl1	94.67 (3)	Cl2^iv—Na2—Dy^iv	39.98 (2)
Cl3ⁱⁱⁱ—Na1—Cl1	86.30 (3)	Na1^iv—Na2—Dy^iv	78.73 (3)
Cl3^iv—Na1—Cl1	93.71 (3)	Cl1—Na2—Na1^x	132.81 (6)
Cl2ⁱ—Na1—Cl1^v	94.67 (3)	Cl2^x—Na2—Na1^x	90.06 (4)
Cl2ⁱⁱ—Na1—Cl1^v	85.33 (3)	Cl1^iv—Na2—Na1^x	112.16 (5)
Cl3ⁱⁱⁱ—Na1—Cl1^v	93.71 (3)	Cl3ⁱ—Na2—Na1^x	41.17 (3)
Cl3^iv—Na1—Cl1^v	86.29 (3)	Cl3^xi—Na2—Na1^x	82.78 (4)
Cl1—Na1—Cl1^v	180.00 (3)	Cl2^iv—Na2—Na1^x	40.45 (2)
Cl2ⁱ—Na1—Na2^vi	59.53 (3)	Na1^iv—Na2—Na1^x	120.74 (4)
Cl2ⁱⁱ—Na1—Na2^vi	120.47 (3)	Dy^iv—Na2—Na1^x	74.49 (3)
Cl3ⁱⁱⁱ—Na1—Na2^vi	53.35 (3)	Cl2—Dy—Cl2^xii	180.0
Cl3^iv—Na1—Na2^vi	126.65 (3)	Cl2—Dy—Cl3	91.33 (3)
Cl1—Na1—Na2^vi	45.99 (3)	Cl2^xii—Dy—Cl3	88.67 (3)
Cl1^v—Na1—Na2^vi	134.01 (3)	Cl2—Dy—Cl3^xii	88.67 (3)
Cl2ⁱ—Na1—Na2^vii	120.47 (3)	Cl2^xii—Dy—Cl3^xii	91.33 (3)
Cl2ⁱⁱ—Na1—Na2^vii	59.53 (3)	Cl3—Dy—Cl3^xii	180.0
Cl3ⁱⁱⁱ—Na1—Na2^vii	126.65 (3)	Cl2—Dy—Cl1^xii	91.73 (3)
Cl3^iv—Na1—Na2^vii	53.35 (3)	Cl2^xii—Dy—Cl1^xii	88.27 (3)
Cl1—Na1—Na2^vii	134.01 (3)	Cl3—Dy—Cl1^xii	91.71 (3)
Cl1^v—Na1—Na2^vii	45.99 (3)	Cl3^xii—Dy—Cl1^xii	88.29 (3)
Na2^vi—Na1—Na2^vii	180.0	Cl2—Dy—Cl1	88.28 (3)
Cl2ⁱ—Na1—Na2^viii	127.96 (3)	Cl2^xii—Dy—Cl1	91.72 (3)
Cl2ⁱⁱ—Na1—Na2^viii	52.04 (3)	Cl3—Dy—Cl1	88.29 (3)
Cl3ⁱⁱⁱ—Na1—Na2^viii	42.45 (3)	Cl3^xii—Dy—Cl1	91.71 (3)
Cl3^iv—Na1—Na2^viii	137.55 (3)	Cl1^xii—Dy—Cl1	180.00 (3)
Cl1—Na1—Na2^viii	73.28 (3)	Cl2—Dy—Na2^xiii	125.31 (3)
Cl1^v—Na1—Na2^viii	106.72 (3)	Cl2^xii—Dy—Na2^xiii	54.69 (3)
Na2^vi—Na1—Na2^viii	72.02 (3)	Cl3—Dy—Na2^xiii	115.46 (3)
Na2^vii—Na1—Na2^viii	107.98 (3)	Cl3^xii—Dy—Na2^xiii	64.54 (3)
Cl2ⁱ—Na1—Na2^ix	52.04 (3)	Cl1^xii—Dy—Na2^xiii	44.32 (3)
Cl2ⁱⁱ—Na1—Na2^ix	127.96 (3)	Cl1—Dy—Na2^xiii	135.68 (3)
Cl3ⁱⁱⁱ—Na1—Na2^ix	137.55 (3)	Cl2—Dy—Na2^vi	54.69 (3)
Cl3^iv—Na1—Na2^ix	42.45 (3)	Cl2^xii—Dy—Na2^vi	125.31 (3)
Cl1—Na1—Na2^ix	106.72 (3)	Cl3—Dy—Na2^vi	64.54 (3)
Cl1^v—Na1—Na2^ix	73.28 (3)	Cl3^xii—Dy—Na2^vi	115.46 (3)
Na2^vi—Na1—Na2^ix	107.98 (3)	Cl1^xii—Dy—Na2^vi	135.68 (3)
Na2^vii—Na1—Na2^ix	72.02 (3)	Cl1—Dy—Na2^vi	44.32 (3)
Na2^viii—Na1—Na2^ix	180.0	Na2^xiii—Dy—Na2^vi	180.0
Cl1—Na2—Cl2^x	97.84 (6)	Dy—Cl1—Na2	105.51 (5)
Cl1—Na2—Cl1^iv	88.35 (5)	Dy—Cl1—Na2^vi	95.24 (4)
Cl2^x—Na2—Cl1^iv	143.02 (7)	Na2—Cl1—Na2^vi	133.80 (6)
Cl1—Na2—Cl3ⁱ	94.53 (6)	Dy—Cl1—Na1	134.58 (3)
Cl2^x—Na2—Cl3ⁱ	79.84 (5)	Na2—Cl1—Na1	104.61 (4)
Cl1^iv—Na2—Cl3ⁱ	136.23 (7)	Na2^vi—Cl1—Na1	87.61 (4)
Cl1—Na2—Cl3^xi	144.16 (7)	Dy—Cl2—Na1^xiv	138.63 (3)
Cl2^x—Na2—Cl3^xi	74.54 (5)	Dy—Cl2—Na2^viii	99.86 (4)
Cl1^iv—Na2—Cl3^xi	79.25 (5)	Na1^xiv—Cl2—Na2^viii	121.47 (5)
Cl3ⁱ—Na2—Cl3^xi	117.64 (5)	Dy—Cl2—Na2^vi	85.33 (4)
Cl1—Na2—Cl2^iv	139.29 (7)	Na1^xiv—Cl2—Na2^vi	87.50 (4)
Cl2^x—Na2—Cl2^iv	119.28 (5)	Na2^viii—Cl2—Na2^vi	102.36 (4)
Cl1^iv—Na2—Cl2^iv	72.36 (4)	Dy—Cl3—Na1^vi	134.93 (3)
Cl3ⁱ—Na2—Cl2^iv	77.55 (4)	Dy—Cl3—Na2^xv	128.25 (5)
Cl3^xi—Na2—Cl2^iv	68.06 (4)	Na1^vi—Cl3—Na2^xv	96.38 (4)
Cl1—Na2—Na1^iv	104.40 (5)	Dy—Cl3—Na2^xi	90.78 (4)
Cl2^x—Na2—Na1^iv	97.07 (5)	Na1^vi—Cl3—Na2^xi	82.33 (4)
Cl1^iv—Na2—Na1^iv	46.40 (3)	Na2^xv—Cl3—Na2^xi	104.74 (4)
Cl3ⁱ—Na2—Na1^iv	161.07 (6)

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

Experimental details

Crystal data
Chemical formula	Na₃DyCl₆
M_r	444.17
Crystal system, space group	Monoclinic, P2₁/n
Temperature (K)	293
a, b, c (Å)	6.8791 (5), 7.2816 (5), 10.1734 (7)
β (°)	90.823 (4)
V (Å³)	509.54 (6)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	8.96
Crystal size (mm)	0.20 × 0.15 × 0.10

Data collection
Diffractometer	Nonius KappaCCD diffractometer
Absorption correction	Numerical (X-SHAPE; Stoe & Cie 1999)
T_min, T_max	0.218, 0.414
No. of measured, independent and observed [I > 2σ(I)] reflections	12026, 1245, 1124
R_int	0.071
(sin θ/λ)_max (Å⁻¹)	0.663

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.019, 0.045, 1.08
No. of reflections	1245
No. of parameters	50
Δρ_max, Δρ_min (e Å⁻³)	0.84, −1.05

Computer programs: COLLECT (Nonius, 1998), SCALEPACK (Otwinowski & Minor, 1997), SCALEPACK and DENZO (Otwinowski & Minor, 1997), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 2006).

Selected bond lengths (Å) top

Na1—Cl2ⁱ	2.7358 (8)	Na2—Cl3^vii	3.204 (2)
Na1—Cl2ⁱⁱ	2.7358 (8)	Na2—Cl2^iv	3.325 (2)
Na1—Cl3ⁱⁱⁱ	2.7902 (8)	Na2—Cl2	3.488 (2)
Na1—Cl3^iv	2.7902 (8)	Dy—Cl2	2.6176 (8)
Na1—Cl1	2.8687 (8)	Dy—Cl2^viii	2.6176 (8)
Na1—Cl1^v	2.8687 (8)	Dy—Cl3	2.6320 (8)
Na2—Cl1	2.8295 (19)	Dy—Cl3^viii	2.6320 (8)
Na2—Cl2^vi	2.8341 (19)	Dy—Cl1^viii	2.6447 (8)
Na2—Cl1^iv	2.8492 (19)	Dy—Cl1	2.6447 (8)
Na2—Cl3ⁱ	2.8612 (19)

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

Acknowledgements

This work was supported by the German Research Foundation (DFG, Frankfurt/Main) within the funding programme Open Access Publishing and the State of Baden-Württemberg (Stuttgart). The authors thank Dr Sabine Strobel for the data collection.

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