Bis(chlorido)(dimethyl­sulfoxide-κO)barium(II)

Gschwind, F.; Jansen, M.

doi:10.1107/S160053681204069X

metal-organic compounds

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Volume 68| Part 11| November 2012| Page m1319

doi:10.1107/S160053681204069X

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Bis(chlorido)(dimethylsulfoxide-κO)barium(II)

Fabienne Gschwind ^a ^* and Martin Jansen ^a

^aMax Planck Institute for Solid State Research, Heisenbergstrasse 1, 70569 Stuttgart, Germany
^*Correspondence e-mail: f.gschwind@fkf.mpg.de

(Received 25 September 2012; accepted 26 September 2012; online 3 October 2012)

The title compound, [BaCl₂(C₂H₆SO)], forms a Ba₆Cl₉ cluster in which the BaCl₂ units are connected via dimethylsulfoxide (DMSO) and chloride bridges. The central Cl atom of the Ba₆Cl₉ cluster is located on a threefold inversion axis and is coordinated octahedrally to six barium cations. In the crystal, the clusters are arranged in rows, which are interconnected by the DMSO molecules, forming a three-dimensional network.

Related literature

For general background to barium complexes with chloride bridges, see: Yang et al. (2006 ); Arion et al. (2001 ); Fenske et al. (1993 ). For further information on chelated barium clusters with a central chloride atom, see: Drozdov et al. (1994 ). For examples of barium–DMSO complexes, see: Harrowfield et al. (2004 ); Pi et al. (2009 ). For a description of the Cambridge Structural Database, see: Allen (2002 ).

Experimental

Crystal data

[BaCl₂(C₂H₆OS)]
M_r = 286.37
Trigonal, $[R \overline 3c ]$
a = 15.680 (7) Å
c = 33.848 (6) Å
V = 7207 (5) Å³
Z = 36
Mo Kα radiation
μ = 5.79 mm⁻¹
T = 298 K
0.18 × 0.12 × 0.10 mm

Data collection

Stoe IPDS 2 diffractometer
Absorption correction: numerical (X-SHAPE; Stoe & Cie, 2009 ) T_min = 0.422, T_max = 0.595
28344 measured reflections
1807 independent reflections
1783 reflections with I > 2σ(I)
R_int = 0.059

Refinement

R[F² > 2σ(F²)] = 0.023
wR(F²) = 0.057
S = 1.25
1807 reflections
55 parameters
H-atom parameters constrained
Δρ_max = 0.51 e Å⁻³
Δρ_min = −0.54 e Å⁻³

Data collection: X-AREA (Stoe & Cie, 2009); cell refinement: X-AREA; data reduction: X-RED32 (Stoe & Cie, 2009); 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: publCIF (Westrip, 2010 ).

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S160053681204069X/hg5254sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S160053681204069X/hg5254Isup2.hkl

checkCIF report

Comment top

The title compound crystallizes in the trigonal space group R3c and its asymmetric unit consists of one barium ion and four chloride ions (three of which are located on special positions and have partial occupancies: Cl1 1/2; Cl3 1/6; Cl4 1/3) and one DMSO solvent molecule (Fig. 1). The complete structure forms a Ba₆Cl₉ cluster (Fig. 2). Atom Cl3 occupies the center of the polyhedron located at position (0,0,0: 3); it is coordinated to six barium ions and has an octahedral configuration. Each barium ion sits on a corner of the cluster and coordinates via two O atoms of the DMSO molecule (O1 and its symmetry equivalent O1ⁱ; Ba1—O1 2.752 (3) Å, Ba1—O1ⁱ 2.830 (1) Å; symmetry code: (i) x - y + 1/3, -y + 2/3, -z + 1/6) and one chloride (Ba1—Cl1 = Cl1—Ba1ⁱ = 3.088 (1) Å) to the next BaCl cluster. The average Ba—O bond distance lies in the typical range for a Ba—O(DMSO) bond length (2.637–2.875 Å). The Ba—Cl bond distances in the title compound vary between 3.0888 (16)–3.3231 (11) Å, while a similar bridging Ba—Cl—Ba structure shows bond lengths between (3.114–3.253 Å).

The average Ba···Ba distance in the cluster is about 4.69 Å, while the distance between the two bridged barium ions is shorter at 4.3106 (19) Å.

Due to the high symmetry the Ba–DMSO bridge spreads out in all three dimensions (Fig. 3). In the z-dimension wheel-shaped structures of the rows of BaCl clusters are visible. The `DMSO-chloride' bridges are arranged around the wheels. The closest distance from the BaCl clusters is about 10.6 Å (measured between Cl3 and Cl3ⁱⁱ; symmetry code: (ii) 1/3 + y, 2/3 + x, 1/6 - z). There are no classical hydrogen bonds present but there is a small solvent accessible void of ca 63 Å³.

A literature search (Allen, 2002) revealed no similar barium-chloride clusters, but there are several examples of barium chloride bridged structures. For instance barium sulfonate complexes with layered structures (Yang et al., 2006) or chloride bridged macrocyclic barium complexes (Arion et al., 2001; Fenske et al. 1993). There exist also clusters of barium and O atoms with a bridging central chloride ion (Drozdov et al., 1994). Furthermore, there exist different examples of barium DMSO complexes (Harrowfield et al., 2004; Pi et al. 2009).

Related literature top

For general background to barium complexes with chloride bridges, see: Yang et al. (2006); Arion et al. (2001); Fenske et al. (1993). For further information on chelated barium clusters with a central chloride atom, see: Drozdov et al. (1994). For examples of barium–DMSO complexes, see: Harrowfield et al. (2004); Pi et al. (2009). For a description of the Cambridge Structural Database, see: Allen (2002).

Experimental top

The title compound was obtained incidentally as a side-product in the following reaction:

Solution A: To a solution of BaCl₂ (1 g) dissolved in methanol (10 ml) was added 1,5 g of tetraethylene glycol. Product B: Phosphomolybdic acid hydrate (0.25 g, 0.54 mmol) was dissolved in acetone (5 ml) and precipitated with an excess of cobaltocenium hexafluorophosphate (0.2 g) in acetonitrile (5 ml).

Product B was then dissolved in acetonitrile (10 ml) and precipitated with solution A. The precipitate was dissolved in hot DMSO (15 ml). After cooling the solution was layered with diethylether. A few colorless crystals the title compound appeared as a side-product after a few weeks.

Computing details top

Data collection: X-AREA (Stoe & Cie, 2009); cell refinement: X-AREA (Stoe & Cie, 2009); data reduction: X-RED32 (Stoe & Cie, 2009); 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: publCIF (Westrip, 2010).

Figures top

	Fig. 1. A view of the asymmetric unit of the title compound. Three of the four Cl atoms are located on special positions and have partial occupancies of Cl1 1/2, Cl3 1/6 and Cl4 1/3.
	Fig. 2. A view of the molecular structure of the title compound, with the atom numbering. The displacement ellipsoids are drawn at the 50% probability level. Symmetry codes: (1) -y, x - y, z (2) -x + y, -y, z (3) -x, -y, -z (4) x - y, x, -z (5) y, x + y, -z.
	Fig. 3. A view along the z-axis of the crystal packing of the title compound.

Bis(chlorido)(dimethylsulfoxide-κO)barium(II) top

Crystal data top

[BaCl₂(C₂H₆OS)]	D_x = 2.375 Mg m⁻³
M_r = 286.37	Mo Kα radiation, λ = 0.71073 Å
Trigonal, R3c	Cell parameters from 28704 reflections
Hall symbol: -R 3 2"c	θ = 1.5–57.3°
a = 15.680 (7) Å	µ = 5.79 mm⁻¹
c = 33.848 (6) Å	T = 298 K
V = 7207 (5) Å³	Bloc, colourless
Z = 36	0.18 × 0.12 × 0.10 mm
F(000) = 4752

Data collection top

Stoe IPDS 2 diffractometer	1807 independent reflections
Radiation source: fine-focus sealed tube	1783 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.059
Detector resolution: 6.67 pixels mm^-1	θ_max = 27.3°, θ_min = 2.6°
ω and ϕ scans	h = −20→19
Absorption correction: numerical (X-SHAPE; Stoe & Cie, 2009)	k = −20→20
T_min = 0.422, T_max = 0.595	l = −43→43
28344 measured reflections

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)] = 0.023	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.057	H-atom parameters constrained
S = 1.25	w = 1/[σ²(F_o²) + (0.0207P)² + 30.0844P] where P = (F_o² + 2F_c²)/3
1807 reflections	(Δ/σ)_max < 0.001
55 parameters	Δρ_max = 0.51 e Å⁻³
0 restraints	Δρ_min = −0.54 e Å⁻³

Crystal data top

[BaCl₂(C₂H₆OS)]	Z = 36
M_r = 286.37	Mo Kα radiation
Trigonal, R3c	µ = 5.79 mm⁻¹
a = 15.680 (7) Å	T = 298 K
c = 33.848 (6) Å	0.18 × 0.12 × 0.10 mm
V = 7207 (5) Å³

Data collection top

Stoe IPDS 2 diffractometer	1807 independent reflections
Absorption correction: numerical (X-SHAPE; Stoe & Cie, 2009)	1783 reflections with I > 2σ(I)
T_min = 0.422, T_max = 0.595	R_int = 0.059
28344 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.023	0 restraints
wR(F²) = 0.057	H-atom parameters constrained
S = 1.25	w = 1/[σ²(F_o²) + (0.0207P)² + 30.0844P] where P = (F_o² + 2F_c²)/3
1807 reflections	Δρ_max = 0.51 e Å⁻³
55 parameters	Δρ_min = −0.54 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
S1	0.24622 (7)	0.39751 (7)	0.00510 (3)	0.0417 (2)
O1	0.1864 (2)	0.38899 (19)	0.04210 (7)	0.0463 (6)
C2	0.2400 (4)	0.4882 (3)	−0.02432 (13)	0.0576 (10)*
H2A	0.1744	0.4620	−0.0344	0.086*
H2B	0.2855	0.5063	−0.0459	0.086*
H2C	0.2567	0.5452	−0.0085	0.086*
C1	0.3718 (4)	0.4668 (4)	0.01944 (14)	0.0614 (11)*
H1A	0.3880	0.4270	0.0359	0.092*
H1B	0.3826	0.5241	0.0339	0.092*
H1C	0.4128	0.4868	−0.0037	0.092*
Cl1	−0.03305 (8)	0.3333	0.0833	0.0548 (4)
Cl2	0.23027 (6)	0.18744 (6)	0.03813 (3)	0.03946 (18)
Cl4	0.0000	0.0000	0.10413 (4)	0.0396 (3)
Ba1	0.037103 (14)	0.191429 (13)	0.054807 (5)	0.03329 (8)
Cl3	0.0000	0.0000	0.0000	0.0356 (4)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
S1	0.0425 (4)	0.0386 (4)	0.0401 (4)	0.0172 (4)	0.0055 (3)	−0.0018 (3)
O1	0.0454 (14)	0.0441 (14)	0.0408 (13)	0.0160 (12)	0.0088 (11)	−0.0018 (11)
Cl1	0.0436 (4)	0.0669 (9)	0.0617 (8)	0.0334 (4)	−0.0147 (3)	−0.0295 (7)
Cl2	0.0385 (4)	0.0382 (4)	0.0424 (4)	0.0197 (3)	0.0019 (3)	−0.0004 (3)
Cl4	0.0412 (4)	0.0412 (4)	0.0363 (7)	0.0206 (2)	0.000	0.000
Ba1	0.03337 (11)	0.03172 (11)	0.03353 (12)	0.01533 (8)	0.00041 (7)	−0.00300 (7)
Cl3	0.0367 (5)	0.0367 (5)	0.0334 (9)	0.0183 (3)	0.000	0.000

Geometric parameters (Å, º) top

S1—O1	1.530 (3)	Cl4—Ba1^iv	3.2232 (13)
S1—C1	1.776 (5)	Cl4—Ba1ⁱⁱ	3.2232 (13)
S1—C2	1.778 (5)	Cl4—Ba1	3.2232 (13)
O1—Ba1ⁱ	2.752 (2)	Ba1—O1ⁱ	2.752 (2)
O1—Ba1	2.830 (3)	Ba1—Cl2^iv	3.1528 (16)
C2—H2A	0.9600	Ba1—Cl2^v	3.1968 (11)
C2—H2B	0.9600	Ba1—Cl3	3.3231 (11)
C2—H2C	0.9600	Ba1—Ba1ⁱ	4.3106 (16)
C1—H1A	0.9600	Ba1—Ba1^v	4.6225 (10)
C1—H1B	0.9600	Ba1—Ba1ⁱⁱⁱ	4.6225 (10)
C1—H1C	0.9600	Ba1—Ba1^iv	4.776 (2)
Cl1—Ba1	3.0888 (16)	Cl3—Ba1^v	3.3231 (11)
Cl1—Ba1ⁱ	3.0888 (16)	Cl3—Ba1^vi	3.3231 (11)
Cl2—Ba1	3.1123 (16)	Cl3—Ba1ⁱⁱⁱ	3.3231 (11)
Cl2—Ba1ⁱⁱ	3.1528 (16)	Cl3—Ba1^iv	3.3231 (11)
Cl2—Ba1ⁱⁱⁱ	3.1968 (11)	Cl3—Ba1ⁱⁱ	3.3231 (11)

O1—S1—C1	105.9 (2)	O1ⁱ—Ba1—Ba1ⁱ	40.11 (5)
O1—S1—C2	104.60 (19)	O1—Ba1—Ba1ⁱ	38.79 (5)
C1—S1—C2	98.7 (2)	Cl1—Ba1—Ba1ⁱ	45.751 (18)
S1—O1—Ba1ⁱ	146.52 (15)	Cl2—Ba1—Ba1ⁱ	95.556 (16)
S1—O1—Ba1	110.82 (13)	Cl2^iv—Ba1—Ba1ⁱ	130.725 (16)
Ba1ⁱ—O1—Ba1	101.09 (8)	Cl2^v—Ba1—Ba1ⁱ	107.06 (2)
S1—C2—H2A	109.5	Cl4—Ba1—Ba1ⁱ	119.27 (3)
S1—C2—H2B	109.5	Cl3—Ba1—Ba1ⁱ	161.700 (5)
H2A—C2—H2B	109.5	O1ⁱ—Ba1—Ba1^v	173.27 (6)
S1—C2—H2C	109.5	O1—Ba1—Ba1^v	114.60 (5)
H2A—C2—H2C	109.5	Cl1—Ba1—Ba1^v	104.838 (18)
H2B—C2—H2C	109.5	Cl2—Ba1—Ba1^v	103.16 (2)
S1—C1—H1A	109.5	Cl2^iv—Ba1—Ba1^v	43.656 (18)
S1—C1—H1B	109.5	Cl2^v—Ba1—Ba1^v	42.18 (2)
H1A—C1—H1B	109.5	Cl4—Ba1—Ba1^v	99.24 (3)
S1—C1—H1C	109.5	Cl3—Ba1—Ba1^v	45.933 (9)
H1A—C1—H1C	109.5	Ba1ⁱ—Ba1—Ba1^v	139.897 (6)
H1B—C1—H1C	109.5	O1ⁱ—Ba1—Ba1ⁱⁱⁱ	124.48 (6)
Ba1—Cl1—Ba1ⁱ	88.50 (3)	O1—Ba1—Ba1ⁱⁱⁱ	79.47 (5)
Ba1—Cl2—Ba1ⁱⁱ	99.32 (2)	Cl1—Ba1—Ba1ⁱⁱⁱ	137.642 (7)
Ba1—Cl2—Ba1ⁱⁱⁱ	94.21 (2)	Cl2—Ba1—Ba1ⁱⁱⁱ	43.606 (18)
Ba1ⁱⁱ—Cl2—Ba1ⁱⁱⁱ	93.44 (2)	Cl2^iv—Ba1—Ba1ⁱⁱⁱ	102.98 (2)
Ba1^iv—Cl4—Ba1ⁱⁱ	95.60 (3)	Cl2^v—Ba1—Ba1ⁱⁱⁱ	42.91 (2)
Ba1^iv—Cl4—Ba1	95.60 (3)	Cl4—Ba1—Ba1ⁱⁱⁱ	99.24 (3)
Ba1ⁱⁱ—Cl4—Ba1	95.60 (3)	Cl3—Ba1—Ba1ⁱⁱⁱ	45.933 (9)
O1ⁱ—Ba1—O1	69.29 (9)	Ba1ⁱ—Ba1—Ba1ⁱⁱⁱ	117.194 (11)
O1ⁱ—Ba1—Cl1	70.89 (6)	Ba1^v—Ba1—Ba1ⁱⁱⁱ	62.20 (2)
O1—Ba1—Cl1	69.92 (6)	O1ⁱ—Ba1—Ba1^iv	118.10 (6)
O1ⁱ—Ba1—Cl2	83.11 (6)	O1—Ba1—Ba1^iv	169.45 (5)
O1—Ba1—Cl2	73.36 (6)	Cl1—Ba1—Ba1^iv	118.845 (16)
Cl1—Ba1—Cl2	140.52 (2)	Cl2—Ba1—Ba1^iv	99.356 (16)
O1ⁱ—Ba1—Cl2^iv	129.87 (6)	Cl2^iv—Ba1—Ba1^iv	40.024 (16)
O1—Ba1—Cl2^iv	142.06 (6)	Cl2^v—Ba1—Ba1^iv	98.624 (16)
Cl1—Ba1—Cl2^iv	85.41 (2)	Cl4—Ba1—Ba1^iv	42.200 (17)
Cl2—Ba1—Cl2^iv	133.71 (3)	Cl3—Ba1—Ba1^iv	44.067 (9)
O1ⁱ—Ba1—Cl2^v	142.50 (6)	Ba1ⁱ—Ba1—Ba1^iv	151.522 (11)
O1—Ba1—Cl2^v	73.31 (5)	Ba1^v—Ba1—Ba1^iv	58.899 (11)
Cl1—Ba1—Cl2^v	99.01 (2)	Ba1ⁱⁱⁱ—Ba1—Ba1^iv	90.0
Cl2—Ba1—Cl2^v	83.71 (2)	Ba1^v—Cl3—Ba1	88.135 (18)
Cl2^iv—Ba1—Cl2^v	83.06 (2)	Ba1^v—Cl3—Ba1^vi	91.865 (18)
O1ⁱ—Ba1—Cl4	79.44 (6)	Ba1—Cl3—Ba1^vi	180.000 (5)
O1—Ba1—Cl4	139.76 (6)	Ba1^v—Cl3—Ba1ⁱⁱⁱ	91.865 (18)
Cl1—Ba1—Cl4	123.06 (3)	Ba1—Cl3—Ba1ⁱⁱⁱ	88.135 (18)
Cl2—Ba1—Cl4	78.438 (19)	Ba1^vi—Cl3—Ba1ⁱⁱⁱ	91.865 (18)
Cl2^iv—Ba1—Cl4	77.857 (19)	Ba1^v—Cl3—Ba1^iv	88.135 (18)
Cl2^v—Ba1—Cl4	131.44 (3)	Ba1—Cl3—Ba1^iv	91.865 (18)
O1ⁱ—Ba1—Cl3	137.07 (5)	Ba1^vi—Cl3—Ba1^iv	88.135 (18)
O1—Ba1—Cl3	125.40 (5)	Ba1ⁱⁱⁱ—Cl3—Ba1^iv	180.000 (9)
Cl1—Ba1—Cl3	149.383 (17)	Ba1^v—Cl3—Ba1ⁱⁱ	180.000 (8)
Cl2—Ba1—Cl3	67.244 (16)	Ba1—Cl3—Ba1ⁱⁱ	91.865 (18)
Cl2^iv—Ba1—Cl3	66.799 (16)	Ba1^vi—Cl3—Ba1ⁱⁱ	88.135 (18)
Cl2^v—Ba1—Cl3	66.32 (2)	Ba1ⁱⁱⁱ—Cl3—Ba1ⁱⁱ	88.135 (18)
Cl4—Ba1—Cl3	65.13 (3)	Ba1^iv—Cl3—Ba1ⁱⁱ	91.865 (18)

Symmetry codes: (i) x−y+1/3, −y+2/3, −z+1/6; (ii) −x+y, −x, z; (iii) y, −x+y, −z; (iv) −y, x−y, z; (v) x−y, x, −z; (vi) −x, −y, −z.

Experimental details

Crystal data
Chemical formula	[BaCl₂(C₂H₆OS)]
M_r	286.37
Crystal system, space group	Trigonal, R3c
Temperature (K)	298
a, c (Å)	15.680 (7), 33.848 (6)
V (Å³)	7207 (5)
Z	36
Radiation type	Mo Kα
µ (mm⁻¹)	5.79
Crystal size (mm)	0.18 × 0.12 × 0.10

Data collection
Diffractometer	Stoe IPDS 2 diffractometer
Absorption correction	Numerical (X-SHAPE; Stoe & Cie, 2009)
T_min, T_max	0.422, 0.595
No. of measured, independent and observed [I > 2σ(I)] reflections	28344, 1807, 1783
R_int	0.059
(sin θ/λ)_max (Å⁻¹)	0.645

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.023, 0.057, 1.25
No. of reflections	1807
No. of parameters	55
H-atom treatment	H-atom parameters constrained
	w = 1/[σ²(F_o²) + (0.0207P)² + 30.0844P] where P = (F_o² + 2F_c²)/3
Δρ_max, Δρ_min (e Å⁻³)	0.51, −0.54

Computer programs: X-AREA (Stoe & Cie, 2009), X-RED32 (Stoe & Cie, 2009), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 2006), publCIF (Westrip, 2010).

Acknowledgements

The authors thank Helen Stöckli-Evans for valuable help.

References

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