Octa­deca­bromidobis(dicarbido)deca­dysprosium, [Dy10Br18(C2)2]

Daub, K.; Meyer, G.

doi:10.1107/S1600536807066111

inorganic compounds

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Volume 64| Part 1| January 2008| Page i4

https://doi.org/10.1107/S1600536807066111

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Octadecabromidobis(dicarbido)decadysprosium, [Dy₁₀Br₁₈(C₂)₂]

Kathrin Daub ^a and Gerd Meyer ^a ^*

^aInstitut für Anorganische Chemie, Universität zu Köln, Greinstrasse 6, D-50939 Köln, Germany
^*Correspondence e-mail: gerd.meyer@uni-koeln.de

(Received 22 November 2007; accepted 7 December 2007; online 12 December 2007)

Single crystals of [Dy₁₀Br₁₈(C₂)₂] were obtained during the reaction of DyBr₃ with dysprosium metal and graphite in a sealed tantalum container. In the crystal structure, the Dy atoms form dimers of edge-sharing octahedra, each encapsulating a C₂ unit. The metal atoms are surrounded by Br atoms above the cluster edges and vertices, respectively. The dimers are connected to each other by Br atoms, leading to a three-dimensional network. [Dy₁₀Br₁₈(C₂)₂] is isotypic with its iodido analogue [Dy₁₀I₁₈(C₂)₂].

Related literature

Details of ternary and quaternary halides of the rare earth elements have been compiled by Meyer & Wickleder (2000 ). Bromides with the formula [RE₁₀Br₁₈(C₂)₂], where RE is Gd, Tb or Er, have been studied by Liess (1996 ), Mattausch et al. (2002 ) and Uhrlandt et al. (1994 ). Recently, the first dysprosium compound belonging to this structural family, [Dy₁₀I₁₈(C₂)₂], was reported by Mattausch et al. (2007 ). [Dy₁₀Br₁₈(C₂)₂] is obtained by reduction of DyBr₃ with dysprosium and graphite. For the synthesis of the starting material DyBr₃, see Meyer et al. (1987 ).

Experimental

Crystal data

[Dy₁₀Br₁₈(C₂)₂]
M_r = 3111.42
Monoclinic, P 2₁ /c
a = 9.7399 (12) Å
b = 16.3398 (15) Å
c = 13.2469 (19) Å
β = 120.869 (9)°
V = 1809.6 (4) Å³
Z = 2
Mo Kα radiation
μ = 40.24 mm⁻¹
T = 293 (2) K
0.20 × 0.20 × 0.20 mm

Data collection

Stoe IPDSII diffractometer
Absorption correction: numerical [X-RED (Stoe & Cie, 2001 ) and X-SHAPE (Stoe & Cie, 1999 )] T_min = 0.015, T_max = 0.063
23768 measured reflections
3935 independent reflections
2989 reflections with I > 2σ(I)
R_int = 0.096

Refinement

R[F² > 2σ(F²)] = 0.033
wR(F²) = 0.079
S = 1.01
3935 reflections
136 parameters
Δρ_max = 2.44 e Å⁻³
Δρ_min = −1.75 e Å⁻³

Data collection: X-AREA (Stoe & Cie, 2001); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2005 ); software used to prepare material for publication: SHELXL97.

Supporting information

Crystal structure: contains datablocks global_, I. DOI: https://doi.org/10.1107/S1600536807066111/wm2169sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536807066111/wm2169Isup2.hkl

checkCIF report

Comment top

A number of ternary and quaternary halides of the general formulae [{RE₁₀(C₂)₂}X_n] with RE = Gd, Tb, Er, Y; X = Cl, Br, I; n = 17–19 and A_x[{RE₁₀(C₂)₂}X_n] with A = K, Rb, Cs; x = 1–3; n = 18–21 have been observed and were compiled by Meyer and Wickleder (2000). Among these halides, three bromides with the formula [{RE₁₀(C₂)₂}Br₁₈], where RE is Gd, Tb, and Er, are known and were structurally studied by Lie\&s (1996), Mattausch et al. (2002) and Uhrlandt et al. (1994).

The crystal structure of the title compound is isotypic with the iodide analogue [{Dy₁₀(C₂)₂}I₁₈] studied recently by Mattausch et al. (2007). As many reduced rare earth halides, the cluster compound [{Dy₁₀(C₂)₂}Br₁₈] consists of an octahedral arrangement of dysprosium atoms stabilized by an interstitial C₂ dumbbell. The dysprosium octahedra are connected via common edges leading to the formation of dimers. The cluster cores are surrounded by bromine atoms above the cluster edges and vertices, respectively (Fig. 1). Some of the bromine atoms belong to a single dimeric unit while others connect neighbouring dimers, thus leading to a three-dimensional network (Fig. 2). Due to the slight elongation of the dysprosium octahedra established roughly parallel to the axis of the C₂ units, the Dy—Dy distances range from 3.1832 (11) to 4.0369 (9) Å. The Dy—Br distances in [{Dy₁₀(C₂)₂}Br₁₈] vary between 2.7157 (15) and 3.3231 (12) Å with the distances to the edge-bridging bromine atoms that are placed between two condensed octahedra significantly larger than those to the other ligands. The C—C bond length is 1.437 (13) Å.

Related literature top

Details of ternary and quaternary halides of the rare earth elements have been compiled by Meyer & Wickleder (2000). Bromides with the formula [RE₁₀Br₁₈(C₂)₂], where RE is Gd, Tb and Er, have been studied by Lie\&s (1996), Mattausch et al. (2002) and Uhrlandt et al. (1994). Recently, the first dysprosium compound, [Dy₁₀I₁₈(C₂)₂], belonging to this structural family, was reported by Mattausch et al. (2007). [Dy₁₀Br₁₈(C₂)₂] is obtained by reduction of DyBr₃ with dysprosium and graphite. For the synthesis of the starting material DyBr₃, see Meyer et al. (1987).

Experimental top

Black parallelepipedic crystals of [{Dy₁₀(C₂)₂}Br₁₈] were obtained by the reaction of DyBr₃ (150 mg) with dysprosium powder (85 mg, Chempur, 99,9%) and graphite (8 mg, Merck, p.a.) in a tantalum container at 1273 K. DyBr₃ had been synthesized previously according to the ammonium bromide route (Meyer et al., 1987), followed by sublimation in high vacuum for purification. Due to air and moisture sensitivity of both reagents and products, all handlings were carried out in an argon-filled glove box (M. Braun, Garching, Germany).

Structure description top

Details of ternary and quaternary halides of the rare earth elements have been compiled by Meyer & Wickleder (2000). Bromides with the formula [RE₁₀Br₁₈(C₂)₂], where RE is Gd, Tb and Er, have been studied by Lie\&s (1996), Mattausch et al. (2002) and Uhrlandt et al. (1994). Recently, the first dysprosium compound, [Dy₁₀I₁₈(C₂)₂], belonging to this structural family, was reported by Mattausch et al. (2007). [Dy₁₀Br₁₈(C₂)₂] is obtained by reduction of DyBr₃ with dysprosium and graphite. For the synthesis of the starting material DyBr₃, see Meyer et al. (1987).

Computing details top

Data collection: X-AREA (Stoe & Cie, 2001); cell refinement: X-AREA (Stoe & Cie, 2001); data reduction: X-AREA (Stoe & Cie, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2005); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).

Figures top

	Fig. 1. : The dimeric unit in [{Dy₁₀(C₂)₂}Br₁₈] with displacement ellipsoids drawn at the 90% probability level [Symmetry codes: (i) 1 - x, 1/2 + y, 1.5 - z; (ii) x, 0.5 - y, 1/2 + z].
	Fig. 2. : View of the crystal structure of [{Dy₁₀(C₂)₂}Br₁₈] emphasizing the connection between the dimers via bromine atoms.

Octadecabromidobis(dicarbido)decadysprosium top

Crystal data top

[Dy₁₀Br₁₈(C₂)₂]	F(000) = 2628
M_r = 3111.42	D_x = 5.710 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 14525 reflections
a = 9.7399 (12) Å	θ = 2.1–27.1°
b = 16.3398 (15) Å	µ = 40.24 mm⁻¹
c = 13.2469 (19) Å	T = 293 K
β = 120.869 (9)°	Parallelepiped, black
V = 1809.6 (4) Å³	0.20 × 0.20 × 0.20 mm
Z = 2

Data collection top

Stoe IPDSII diffractometer	3935 independent reflections
Radiation source: fine-focus sealed tube	2989 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.096
φ scans	θ_max = 27.3°, θ_min = 2.2°
Absorption correction: numerical [X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)]	h = −12→12
T_min = 0.015, T_max = 0.063	k = −20→20
23768 measured reflections	l = −16→16

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)] = 0.033	w = 1/[σ²(F_o²) + (0.0351P)²] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.079	(Δ/σ)_max = 0.001
S = 1.01	Δρ_max = 2.44 e Å⁻³
3935 reflections	Δρ_min = −1.75 e Å⁻³
136 parameters	Extinction correction: SHELXL97 (Sheldrick, 1997), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.00038 (3)

Crystal data top

[Dy₁₀Br₁₈(C₂)₂]	V = 1809.6 (4) Å³
M_r = 3111.42	Z = 2
Monoclinic, P2₁/c	Mo Kα radiation
a = 9.7399 (12) Å	µ = 40.24 mm⁻¹
b = 16.3398 (15) Å	T = 293 K
c = 13.2469 (19) Å	0.20 × 0.20 × 0.20 mm
β = 120.869 (9)°

Data collection top

Stoe IPDSII diffractometer	3935 independent reflections
Absorption correction: numerical [X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)]	2989 reflections with I > 2σ(I)
T_min = 0.015, T_max = 0.063	R_int = 0.096
23768 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.033	136 parameters
wR(F²) = 0.079	0 restraints
S = 1.01	Δρ_max = 2.44 e Å⁻³
3935 reflections	Δρ_min = −1.75 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
Dy1	0.72140 (7)	−0.18631 (3)	0.55464 (5)	0.01642 (12)
Dy2	0.86572 (6)	−0.05763 (3)	0.81405 (4)	0.01581 (12)
Dy3	0.49120 (6)	0.16312 (3)	0.27712 (5)	0.01646 (13)
Dy4	0.66436 (6)	0.04537 (3)	0.53869 (5)	0.01672 (12)
Dy5	0.49942 (6)	−0.05623 (3)	0.23673 (5)	0.01640 (12)
Br1	0.79002 (15)	0.17718 (7)	0.46836 (11)	0.0267 (3)
Br2	0.18295 (15)	−0.05866 (7)	0.03920 (11)	0.0261 (3)
Br3	0.81121 (14)	−0.06564 (6)	0.44345 (10)	0.0199 (2)
Br4	0.19236 (15)	0.18349 (7)	0.05984 (11)	0.0270 (3)
Br5	0.60176 (17)	−0.19122 (6)	0.14246 (12)	0.0282 (3)
Br6	0.59583 (16)	0.06929 (7)	0.14910 (12)	0.0273 (3)
Br7	1.01722 (16)	−0.18152 (7)	0.75532 (12)	0.0274 (3)
Br8	0.97720 (15)	0.06689 (7)	0.73923 (11)	0.0265 (3)
Br9	0.58632 (14)	0.19733 (6)	0.66855 (10)	0.0198 (2)
C1	0.6314 (13)	−0.0891 (5)	0.6212 (9)	0.0118 (18)*
C2	0.4262 (13)	0.0309 (6)	0.3277 (9)	0.0144 (19)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Dy1	0.0185 (3)	0.0131 (2)	0.0193 (3)	0.00139 (17)	0.0109 (2)	−0.00086 (17)
Dy2	0.0133 (3)	0.0157 (2)	0.0161 (3)	−0.00058 (17)	0.0058 (2)	0.00070 (17)
Dy3	0.0170 (3)	0.0136 (2)	0.0190 (3)	−0.00068 (17)	0.0094 (2)	0.00148 (17)
Dy4	0.0136 (3)	0.0162 (2)	0.0177 (3)	−0.00185 (17)	0.0061 (2)	0.00218 (17)
Dy5	0.0162 (3)	0.0138 (2)	0.0191 (3)	0.00202 (17)	0.0089 (2)	−0.00146 (17)
Br1	0.0196 (6)	0.0273 (5)	0.0261 (6)	−0.0087 (4)	0.0066 (5)	0.0045 (4)
Br2	0.0170 (6)	0.0321 (6)	0.0209 (6)	0.0031 (4)	0.0037 (5)	−0.0070 (5)
Br3	0.0161 (6)	0.0213 (5)	0.0235 (6)	0.0005 (4)	0.0110 (5)	0.0020 (4)
Br4	0.0214 (7)	0.0287 (5)	0.0247 (6)	−0.0059 (4)	0.0073 (5)	0.0103 (4)
Br5	0.0435 (8)	0.0148 (5)	0.0400 (7)	0.0018 (4)	0.0313 (7)	−0.0017 (4)
Br6	0.0361 (7)	0.0225 (5)	0.0354 (7)	−0.0012 (5)	0.0271 (6)	0.0002 (5)
Br7	0.0191 (6)	0.0298 (5)	0.0281 (7)	0.0066 (4)	0.0083 (5)	−0.0031 (4)
Br8	0.0182 (6)	0.0291 (5)	0.0248 (6)	−0.0074 (4)	0.0057 (5)	0.0056 (4)
Br9	0.0189 (6)	0.0163 (4)	0.0235 (6)	−0.0005 (4)	0.0104 (5)	−0.0009 (4)

Geometric parameters (Å, º) top

Dy1—C1	2.205 (9)	Dy4—C2	2.568 (11)
Dy1—Br7	2.7413 (15)	Dy4—C1ⁱⁱ	2.652 (10)
Dy1—Br5ⁱ	2.8473 (12)	Dy4—C2ⁱⁱ	2.659 (10)
Dy1—Br3	2.8539 (12)	Dy4—Br8	2.8564 (14)
Dy1—Br9ⁱⁱ	2.9434 (14)	Dy4—Br1	2.8591 (12)
Dy1—Br4ⁱⁱⁱ	2.9730 (12)	Dy4—Br3	2.9630 (12)
Dy1—Dy2	3.6399 (8)	Dy4—Dy4ⁱⁱ	3.1832 (11)
Dy1—Dy3ⁱⁱ	3.7595 (9)	Dy4—Br9	3.3231 (12)
Dy1—Dy4	3.8163 (7)	Dy5—C2	2.207 (10)
Dy2—C1	2.453 (10)	Dy5—Br6	2.7485 (12)
Dy2—C2ⁱⁱ	2.515 (11)	Dy5—Br2	2.8413 (14)
Dy2—Br8	2.7213 (12)	Dy5—Br3	2.8655 (14)
Dy2—Br7	2.8388 (13)	Dy5—Br9ⁱⁱ	2.9432 (12)
Dy2—Br4ⁱⁱ	2.8827 (12)	Dy5—Br5	2.9488 (12)
Dy2—Br2ⁱⁱ	2.9258 (13)	Dy5—Dy2ⁱⁱ	3.7560 (8)
Dy2—Br2^iv	2.9978 (14)	Br2—Dy2ⁱⁱ	2.9258 (13)
Dy2—Dy3ⁱⁱ	3.4938 (8)	Br2—Dy2^vii	2.9978 (14)
Dy2—Dy4	3.5558 (9)	Br4—Dy2ⁱⁱ	2.8827 (12)
Dy2—Dy5ⁱⁱ	3.7560 (8)	Br4—Dy1^v	2.9730 (12)
Dy3—C2	2.439 (9)	Br5—Dy1^viii	2.8473 (12)
Dy3—C1ⁱⁱ	2.520 (10)	Br5—Dy3ⁱⁱⁱ	2.9340 (12)
Dy3—Br1	2.7157 (15)	Br9—Dy5ⁱⁱ	2.9432 (12)
Dy3—Br6	2.8354 (13)	Br9—Dy1ⁱⁱ	2.9434 (14)
Dy3—Br4	2.8759 (14)	Br9—Dy3^ix	3.0812 (12)
Dy3—Br5^v	2.9340 (12)	C1—C2ⁱⁱ	1.437 (13)
Dy3—Br9^vi	3.0812 (12)	C1—Dy3ⁱⁱ	2.520 (10)
Dy3—Dy2ⁱⁱ	3.4938 (8)	C1—Dy4ⁱⁱ	2.652 (10)
Dy3—Dy4	3.5434 (8)	C2—C1ⁱⁱ	1.437 (13)
Dy3—Dy5	3.6309 (7)	C2—Dy2ⁱⁱ	2.515 (11)
Dy3—Dy1ⁱⁱ	3.7595 (8)	C2—Dy4ⁱⁱ	2.659 (10)
Dy4—C1	2.547 (9)

C1—Dy1—Br7	91.6 (3)	C2—Dy4—C2ⁱⁱ	105.0 (3)
C1—Dy1—Br5ⁱ	90.7 (2)	C1ⁱⁱ—Dy4—C2ⁱⁱ	93.6 (3)
Br7—Dy1—Br5ⁱ	94.05 (4)	C1—Dy4—Br8	90.9 (2)
C1—Dy1—Br3	89.9 (2)	C2—Dy4—Br8	163.8 (2)
Br7—Dy1—Br3	91.88 (4)	C1ⁱⁱ—Dy4—Br8	155.9 (2)
Br5ⁱ—Dy1—Br3	174.01 (4)	C2ⁱⁱ—Dy4—Br8	89.9 (2)
C1—Dy1—Br9ⁱⁱ	92.1 (3)	C1—Dy4—Br1	163.6 (2)
Br7—Dy1—Br9ⁱⁱ	176.15 (4)	C2—Dy4—Br1	90.8 (2)
Br5ⁱ—Dy1—Br9ⁱⁱ	87.03 (4)	C1ⁱⁱ—Dy4—Br1	90.5 (2)
Br3—Dy1—Br9ⁱⁱ	87.00 (4)	C2ⁱⁱ—Dy4—Br1	156.1 (2)
C1—Dy1—Br4ⁱⁱⁱ	173.6 (3)	Br8—Dy4—Br1	77.27 (4)
Br7—Dy1—Br4ⁱⁱⁱ	94.80 (4)	C1—Dy4—Br3	81.3 (2)
Br5ⁱ—Dy1—Br4ⁱⁱⁱ	89.28 (4)	C2—Dy4—Br3	81.0 (2)
Br3—Dy1—Br4ⁱⁱⁱ	89.40 (4)	C1ⁱⁱ—Dy4—Br3	112.9 (2)
Br9ⁱⁱ—Dy1—Br4ⁱⁱⁱ	81.51 (4)	C2ⁱⁱ—Dy4—Br3	113.2 (2)
C1—Dy1—Dy2	41.1 (3)	Br8—Dy4—Br3	87.35 (4)
Br7—Dy1—Dy2	50.46 (3)	Br1—Dy4—Br3	86.65 (4)
Br5ⁱ—Dy1—Dy2	93.50 (3)	C1—Dy4—Dy4ⁱⁱ	53.8 (2)
Br3—Dy1—Dy2	90.92 (3)	C2—Dy4—Dy4ⁱⁱ	53.8 (2)
Br9ⁱⁱ—Dy1—Dy2	133.21 (3)	C1ⁱⁱ—Dy4—Dy4ⁱⁱ	50.8 (2)
Br4ⁱⁱⁱ—Dy1—Dy2	145.25 (3)	C2ⁱⁱ—Dy4—Dy4ⁱⁱ	51.2 (2)
C1—Dy1—Dy3ⁱⁱ	40.3 (2)	Br8—Dy4—Dy4ⁱⁱ	140.68 (4)
Br7—Dy1—Dy3ⁱⁱ	92.68 (3)	Br1—Dy4—Dy4ⁱⁱ	140.71 (4)
Br5ⁱ—Dy1—Dy3ⁱⁱ	50.45 (2)	Br3—Dy4—Dy4ⁱⁱ	101.73 (3)
Br3—Dy1—Dy3ⁱⁱ	130.11 (3)	C1—Dy4—Br9	108.0 (2)
Br9ⁱⁱ—Dy1—Dy3ⁱⁱ	90.85 (3)	C2—Dy4—Br9	108.3 (2)
Br4ⁱⁱⁱ—Dy1—Dy3ⁱⁱ	139.48 (3)	C1ⁱⁱ—Dy4—Br9	76.7 (2)
Dy2—Dy1—Dy3ⁱⁱ	56.324 (16)	C2ⁱⁱ—Dy4—Br9	76.3 (2)
C1—Dy1—Dy4	39.8 (2)	Br8—Dy4—Br9	81.07 (4)
Br7—Dy1—Dy4	94.36 (3)	Br1—Dy4—Br9	81.70 (4)
Br5ⁱ—Dy1—Dy4	129.89 (3)	Br3—Dy4—Br9	165.10 (3)
Br3—Dy1—Dy4	50.25 (2)	Dy4ⁱⁱ—Dy4—Br9	93.17 (3)
Br9ⁱⁱ—Dy1—Dy4	87.75 (2)	C1—Dy4—Dy3	141.9 (2)
Br4ⁱⁱⁱ—Dy1—Dy4	138.84 (3)	C2—Dy4—Dy3	43.5 (2)
Dy2—Dy1—Dy4	56.906 (14)	C1ⁱⁱ—Dy4—Dy3	45.2 (2)
Dy3ⁱⁱ—Dy1—Dy4	79.866 (14)	C2ⁱⁱ—Dy4—Dy3	138.7 (2)
C1—Dy2—C2ⁱⁱ	33.6 (3)	Br8—Dy4—Dy3	126.02 (3)
C1—Dy2—Br8	96.3 (2)	Br1—Dy4—Dy3	48.77 (3)
C2ⁱⁱ—Dy2—Br8	96.2 (2)	Br3—Dy4—Dy3	90.43 (3)
C1—Dy2—Br7	84.4 (2)	Dy4ⁱⁱ—Dy4—Dy3	92.44 (2)
C2ⁱⁱ—Dy2—Br7	117.8 (2)	Br9—Dy4—Dy3	88.85 (3)
Br8—Dy2—Br7	94.17 (4)	C1—Dy4—Dy2	43.6 (2)
C1—Dy2—Br4ⁱⁱ	95.7 (2)	C2—Dy4—Dy2	142.0 (2)
C2ⁱⁱ—Dy2—Br4ⁱⁱ	94.2 (2)	C1ⁱⁱ—Dy4—Dy2	138.4 (2)
Br8—Dy2—Br4ⁱⁱ	167.98 (4)	C2ⁱⁱ—Dy4—Dy2	44.9 (2)
Br7—Dy2—Br4ⁱⁱ	86.23 (4)	Br8—Dy4—Dy2	48.74 (3)
C1—Dy2—Br2ⁱⁱ	116.5 (2)	Br1—Dy4—Dy2	126.00 (3)
C2ⁱⁱ—Dy2—Br2ⁱⁱ	82.9 (2)	Br3—Dy4—Dy2	90.82 (3)
Br8—Dy2—Br2ⁱⁱ	89.27 (4)	Dy4ⁱⁱ—Dy4—Dy2	92.53 (2)
Br7—Dy2—Br2ⁱⁱ	158.35 (4)	Br9—Dy4—Dy2	88.56 (3)
Br4ⁱⁱ—Dy2—Br2ⁱⁱ	86.07 (4)	Dy3—Dy4—Dy2	174.519 (19)
C1—Dy2—Br2^iv	165.5 (2)	C1—Dy4—Dy1	33.6 (2)
C2ⁱⁱ—Dy2—Br2^iv	159.6 (2)	C2—Dy4—Dy1	89.6 (2)
Br8—Dy2—Br2^iv	88.07 (4)	C1ⁱⁱ—Dy4—Dy1	112.27 (19)
Br7—Dy2—Br2^iv	81.56 (4)	C2ⁱⁱ—Dy4—Dy1	65.6 (2)
Br4ⁱⁱ—Dy2—Br2^iv	80.09 (4)	Br8—Dy4—Dy1	90.87 (3)
Br2ⁱⁱ—Dy2—Br2^iv	77.19 (4)	Br1—Dy4—Dy1	133.69 (3)
C1—Dy2—Dy3ⁱⁱ	46.2 (2)	Br3—Dy4—Dy1	47.77 (2)
C2ⁱⁱ—Dy2—Dy3ⁱⁱ	44.3 (2)	Dy4ⁱⁱ—Dy4—Dy1	69.484 (18)
Br8—Dy2—Dy3ⁱⁱ	139.04 (3)	Br9—Dy4—Dy1	141.07 (3)
Br7—Dy2—Dy3ⁱⁱ	96.80 (3)	Dy3—Dy4—Dy1	125.134 (19)
Br4ⁱⁱ—Dy2—Dy3ⁱⁱ	52.56 (3)	Dy2—Dy4—Dy1	59.047 (14)
Br2ⁱⁱ—Dy2—Dy3ⁱⁱ	94.50 (3)	C2—Dy5—Br6	91.4 (3)
Br2^iv—Dy2—Dy3ⁱⁱ	132.53 (3)	C2—Dy5—Br2	90.6 (3)
C1—Dy2—Dy4	45.7 (2)	Br6—Dy5—Br2	93.77 (4)
C2ⁱⁱ—Dy2—Dy4	48.3 (2)	C2—Dy5—Br3	89.6 (3)
Br8—Dy2—Dy4	52.09 (3)	Br6—Dy5—Br3	91.11 (4)
Br7—Dy2—Dy4	98.46 (3)	Br2—Dy5—Br3	175.10 (4)
Br4ⁱⁱ—Dy2—Dy4	139.75 (3)	C2—Dy5—Br9ⁱⁱ	91.8 (3)
Br2ⁱⁱ—Dy2—Dy4	100.49 (3)	Br6—Dy5—Br9ⁱⁱ	176.15 (4)
Br2^iv—Dy2—Dy4	140.15 (3)	Br2—Dy5—Br9ⁱⁱ	88.32 (4)
Dy3ⁱⁱ—Dy2—Dy4	87.228 (19)	Br3—Dy5—Br9ⁱⁱ	86.79 (3)
C1—Dy2—Dy1	36.2 (2)	C2—Dy5—Br5	171.1 (3)
C2ⁱⁱ—Dy2—Dy1	69.8 (2)	Br6—Dy5—Br5	96.68 (4)
Br8—Dy2—Dy1	96.95 (3)	Br2—Dy5—Br5	92.42 (4)
Br7—Dy2—Dy1	48.13 (3)	Br3—Dy5—Br5	86.67 (4)
Br4ⁱⁱ—Dy2—Dy1	92.26 (3)	Br9ⁱⁱ—Dy5—Br5	79.99 (3)
Br2ⁱⁱ—Dy2—Dy1	152.46 (3)	C2—Dy5—Dy3	41.0 (3)
Br2^iv—Dy2—Dy1	129.62 (3)	Br6—Dy5—Dy3	50.49 (3)
Dy3ⁱⁱ—Dy2—Dy1	63.568 (16)	Br2—Dy5—Dy3	93.10 (3)
Dy4—Dy2—Dy1	64.047 (17)	Br3—Dy5—Dy3	90.27 (2)
C1—Dy2—Dy5ⁱⁱ	68.1 (2)	Br9ⁱⁱ—Dy5—Dy3	132.68 (3)
C2ⁱⁱ—Dy2—Dy5ⁱⁱ	34.5 (2)	Br5—Dy5—Dy3	146.99 (3)
Br8—Dy2—Dy5ⁱⁱ	94.73 (3)	C2—Dy5—Dy2ⁱⁱ	40.2 (3)
Br7—Dy2—Dy5ⁱⁱ	151.85 (3)	Br6—Dy5—Dy2ⁱⁱ	92.98 (3)
Br4ⁱⁱ—Dy2—Dy5ⁱⁱ	90.45 (3)	Br2—Dy5—Dy2ⁱⁱ	50.35 (3)
Br2ⁱⁱ—Dy2—Dy5ⁱⁱ	48.39 (3)	Br3—Dy5—Dy2ⁱⁱ	129.76 (3)
Br2^iv—Dy2—Dy5ⁱⁱ	125.37 (3)	Br9ⁱⁱ—Dy5—Dy2ⁱⁱ	90.84 (3)
Dy3ⁱⁱ—Dy2—Dy5ⁱⁱ	59.980 (16)	Br5—Dy5—Dy2ⁱⁱ	142.13 (3)
Dy4—Dy2—Dy5ⁱⁱ	66.960 (16)	Dy3—Dy5—Dy2ⁱⁱ	56.425 (13)
Dy1—Dy2—Dy5ⁱⁱ	104.213 (19)	C2—Dy5—Dy4	39.8 (3)
C2—Dy3—C1ⁱⁱ	33.6 (3)	Br6—Dy5—Dy4	93.80 (3)
C2—Dy3—Br1	97.1 (3)	Br2—Dy5—Dy4	129.92 (3)
C1ⁱⁱ—Dy3—Br1	96.7 (2)	Br3—Dy5—Dy4	49.90 (3)
C2—Dy3—Br6	84.8 (2)	Br9ⁱⁱ—Dy5—Dy4	87.31 (3)
C1ⁱⁱ—Dy3—Br6	118.3 (2)	Br5—Dy5—Dy4	135.47 (3)
Br1—Dy3—Br6	93.53 (4)	Dy3—Dy5—Dy4	56.545 (13)
C2—Dy3—Br4	96.1 (3)	Dy2ⁱⁱ—Dy5—Dy4	79.862 (17)
C1ⁱⁱ—Dy3—Br4	94.4 (2)	Dy3—Br1—Dy4	78.88 (3)
Br1—Dy3—Br4	166.85 (4)	Dy5—Br2—Dy2ⁱⁱ	81.26 (3)
Br6—Dy3—Br4	87.35 (4)	Dy5—Br2—Dy2^vii	173.49 (5)
C2—Dy3—Br5^v	116.5 (2)	Dy2ⁱⁱ—Br2—Dy2^vii	102.81 (4)
C1ⁱⁱ—Dy3—Br5^v	82.9 (2)	Dy1—Br3—Dy5	94.31 (4)
Br1—Dy3—Br5^v	88.59 (4)	Dy1—Br3—Dy4	81.98 (3)
Br6—Dy3—Br5^v	158.19 (4)	Dy5—Br3—Dy4	82.40 (3)
Br4—Dy3—Br5^v	85.82 (4)	Dy3—Br4—Dy2ⁱⁱ	74.70 (3)
C2—Dy3—Br9^vi	165.0 (2)	Dy3—Br4—Dy1^v	100.81 (4)
C1ⁱⁱ—Dy3—Br9^vi	160.6 (2)	Dy2ⁱⁱ—Br4—Dy1^v	175.51 (5)
Br1—Dy3—Br9^vi	86.44 (4)	Dy1^viii—Br5—Dy3ⁱⁱⁱ	81.11 (3)
Br6—Dy3—Br9^vi	80.48 (3)	Dy1^viii—Br5—Dy5	175.47 (5)
Br4—Dy3—Br9^vi	80.76 (3)	Dy3ⁱⁱⁱ—Br5—Dy5	102.63 (4)
Br5^v—Dy3—Br9^vi	77.99 (3)	Dy5—Br6—Dy3	81.10 (3)
C2—Dy3—Dy2ⁱⁱ	46.0 (3)	Dy1—Br7—Dy2	81.41 (4)
C1ⁱⁱ—Dy3—Dy2ⁱⁱ	44.6 (2)	Dy2—Br8—Dy4	79.17 (3)
Br1—Dy3—Dy2ⁱⁱ	139.84 (3)	Dy5ⁱⁱ—Br9—Dy1ⁱⁱ	90.85 (3)
Br6—Dy3—Dy2ⁱⁱ	97.22 (3)	Dy5ⁱⁱ—Br9—Dy3^ix	99.30 (4)
Br4—Dy3—Dy2ⁱⁱ	52.74 (3)	Dy1ⁱⁱ—Br9—Dy3^ix	96.84 (4)
Br5^v—Dy3—Dy2ⁱⁱ	95.05 (3)	Dy5ⁱⁱ—Br9—Dy4	79.96 (3)
Br9^vi—Dy3—Dy2ⁱⁱ	133.46 (3)	Dy1ⁱⁱ—Br9—Dy4	79.62 (3)
C2—Dy3—Dy4	46.4 (3)	Dy3^ix—Br9—Dy4	176.35 (4)
C1ⁱⁱ—Dy3—Dy4	48.3 (2)	C2ⁱⁱ—C1—Dy1	174.9 (7)
Br1—Dy3—Dy4	52.35 (3)	C2ⁱⁱ—C1—Dy2	75.6 (6)
Br6—Dy3—Dy4	98.89 (3)	Dy1—C1—Dy2	102.7 (4)
Br4—Dy3—Dy4	140.45 (3)	C2ⁱⁱ—C1—Dy3ⁱⁱ	70.1 (5)
Br5^v—Dy3—Dy4	99.56 (3)	Dy1—C1—Dy3ⁱⁱ	105.2 (3)
Br9^vi—Dy3—Dy4	138.77 (3)	Dy2—C1—Dy3ⁱⁱ	89.3 (3)
Dy2ⁱⁱ—Dy3—Dy4	87.713 (18)	C2ⁱⁱ—C1—Dy4	78.3 (5)
C2—Dy3—Dy5	36.4 (2)	Dy1—C1—Dy4	106.6 (4)
C1ⁱⁱ—Dy3—Dy5	70.0 (2)	Dy2—C1—Dy4	90.7 (3)
Br1—Dy3—Dy5	97.29 (3)	Dy3ⁱⁱ—C1—Dy4	147.4 (4)
Br6—Dy3—Dy5	48.41 (2)	C2ⁱⁱ—C1—Dy4ⁱⁱ	70.8 (6)
Br4—Dy3—Dy5	93.11 (3)	Dy1—C1—Dy4ⁱⁱ	111.5 (4)
Br5^v—Dy3—Dy5	152.68 (3)	Dy2—C1—Dy4ⁱⁱ	145.5 (4)
Br9^vi—Dy3—Dy5	128.83 (3)	Dy3ⁱⁱ—C1—Dy4ⁱⁱ	86.4 (3)
Dy2ⁱⁱ—Dy3—Dy5	63.595 (14)	Dy4—C1—Dy4ⁱⁱ	75.5 (3)
Dy4—Dy3—Dy5	64.703 (15)	C1ⁱⁱ—C2—Dy5	175.8 (8)
C2—Dy3—Dy1ⁱⁱ	68.1 (2)	C1ⁱⁱ—C2—Dy3	76.3 (5)
C1ⁱⁱ—Dy3—Dy1ⁱⁱ	34.5 (2)	Dy5—C2—Dy3	102.7 (4)
Br1—Dy3—Dy1ⁱⁱ	95.23 (4)	C1ⁱⁱ—C2—Dy2ⁱⁱ	70.8 (6)
Br6—Dy3—Dy1ⁱⁱ	152.30 (3)	Dy5—C2—Dy2ⁱⁱ	105.2 (4)
Br4—Dy3—Dy1ⁱⁱ	89.95 (3)	Dy3—C2—Dy2ⁱⁱ	89.7 (3)
Br5^v—Dy3—Dy1ⁱⁱ	48.44 (2)	C1ⁱⁱ—C2—Dy4	77.3 (6)
Br9^vi—Dy3—Dy1ⁱⁱ	126.24 (3)	Dy5—C2—Dy4	106.8 (4)
Dy2ⁱⁱ—Dy3—Dy1ⁱⁱ	60.109 (16)	Dy3—C2—Dy4	90.0 (3)
Dy4—Dy3—Dy1ⁱⁱ	66.772 (17)	Dy2ⁱⁱ—C2—Dy4	147.2 (4)
Dy5—Dy3—Dy1ⁱⁱ	104.320 (16)	C1ⁱⁱ—C2—Dy4ⁱⁱ	69.7 (5)
C1—Dy4—C2	98.4 (3)	Dy5—C2—Dy4ⁱⁱ	111.8 (4)
C1—Dy4—C1ⁱⁱ	104.5 (3)	Dy3—C2—Dy4ⁱⁱ	145.0 (4)
C2—Dy4—C1ⁱⁱ	31.9 (3)	Dy2ⁱⁱ—C2—Dy4ⁱⁱ	86.8 (3)
C1—Dy4—C2ⁱⁱ	32.0 (3)	Dy4—C2—Dy4ⁱⁱ	75.0 (3)

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

Experimental details

Crystal data
Chemical formula	[Dy₁₀Br₁₈(C₂)₂]
M_r	3111.42
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	293
a, b, c (Å)	9.7399 (12), 16.3398 (15), 13.2469 (19)
β (°)	120.869 (9)
V (Å³)	1809.6 (4)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	40.24
Crystal size (mm)	0.20 × 0.20 × 0.20

Data collection
Diffractometer	Stoe IPDSII
Absorption correction	Numerical [X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)]
T_min, T_max	0.015, 0.063
No. of measured, independent and observed [I > 2σ(I)] reflections	23768, 3935, 2989
R_int	0.096
(sin θ/λ)_max (Å⁻¹)	0.645

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.033, 0.079, 1.01
No. of reflections	3935
No. of parameters	136
Δρ_max, Δρ_min (e Å⁻³)	2.44, −1.75

Computer programs: X-AREA (Stoe & Cie, 2001), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), DIAMOND (Brandenburg, 2005).

Acknowledgements

This work was supported by the Deutsche Forschungsgemeinschaft (DFG) (SFB 608 `Complex transition metal compounds with spin and charge degrees of freedom and disorder').

References

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