Crystal structure of poly[[μ-4-(hy­droxy­meth­yl)pyridine-κ2N:O][4-(hy­droxy­meth­yl)pyridine-κN](μ-thio­cyanato-κ2N:S)(thio­cyanato-κN)cadmium]

Werner, J.; Jess, I.; Näther, C.

doi:10.1107/S2056989015008890

metal-organic compounds

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ISSN: 2056-9890

Volume 71| Part 6| June 2015| Pages m129-m130

doi:10.1107/S2056989015008890

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Crystal structure of poly[[μ-4-(hydroxymethyl)pyridine-κ²N:O][4-(hydroxymethyl)pyridine-κN](μ-thiocyanato-κ²N:S)(thiocyanato-κN)cadmium]

Julia Werner,^a ^* Inke Jess ^a and Christian Näther ^a

^aInstitut für Anorganische Chemie, Christian-Albrechts-Universität Kiel, Max-Eyth-Strasse 2, 24118 Kiel, Germany
^*Correspondence e-mail: jwerner@ac.uni-kiel.de

Edited by M. Weil, Vienna University of Technology, Austria (Received 4 May 2015; accepted 7 May 2015; online 13 May 2015)

The crystal structure of the title compound, [Cd(NCS)₂(C₆H₇NO)₂]_n is made up of Cd²⁺ cations that are coordinated by three thiocyanate ligands and three 4-(hydroxymethyl)pyridine ligands within distorted N₄OS octahedra. The asymmetric unit consists of one Cd²⁺ cation, two thiocyanate anions and two 4-(hydroxymethyl)pyridine ligands in general positions. Two Cd²⁺ cations are linked by two μ-1,3 N- and S-bonding thioycanate anions into dimers which are further linked into branched chains along [100] by two μ-1,6 N- and O-bonding 4-(hydroxymethyl)pyridine ligands. One additional N-bonded 4-(hydroxymethyl)pyridine ligand and one additional N-bonded thiocyanate anion are only terminally bonded to the metal cation. Interchain O—H⋯S hydrogen bonds between the hydroxy H atoms and one of the thiocyanate S atoms connect the chains into a three-dimensional network.

Keywords: crystal structure; coordination polymer; cadmium; octahedral coordination; hydrogen bonding.

CCDC reference: 1063786

1. Related literature

For similar structures with thiocyanate anions in bridging coordination to cadmium, see: Banerjee et al. (2005 ); Tahli et al. (2011 ).

2. Experimental

2.1. Crystal data

[Cd(NCS)₂(C₆H₇NO)₂]
M_r = 446.81
Monoclinic, P 2₁ /c
a = 10.9124 (3) Å
b = 20.3261 (6) Å
c = 7.9722 (2) Å
β = 105.965 (2)°
V = 1700.08 (8) Å³
Z = 4
Mo Kα radiation
μ = 1.54 mm⁻¹
T = 200 K
0.47 × 0.33 × 0.20 mm

2.2. Data collection

Stoe IPDS-2 diffractometer
Absorption correction: numerical (X-SHAPE and X-RED 32; Stoe, 2008 ) T_min = 0.526, T_max = 0.672
25370 measured reflections
3597 independent reflections
3259 reflections with I > 2σ(I)
R_int = 0.063

2.3. Refinement

R[F² > 2σ(F²)] = 0.025
wR(F²) = 0.058
S = 1.12
3597 reflections
245 parameters
H-atom parameters constrained
Δρ_max = 0.39 e Å⁻³
Δρ_min = −0.44 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O11—H11O⋯S1ⁱ	0.84	2.49	3.330 (2)	174
O21—H21O⋯S1ⁱⁱ	0.84	2.42	3.2410 (18)	164
Symmetry codes: (i) $[x-1, -y+{\script{3\over 2}}, z-{\script{1\over 2}}]$ ; (ii) $[-x+2, y-{\script{1\over 2}}, -z+{\script{3\over 2}}]$ .

Data collection: X-AREA (Stoe, 2008); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL2013 (Sheldrick, 2015 ); molecular graphics: XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999 ); software used to prepare material for publication: publCIF (Westrip, 2010 ).

Supporting information

CCDC reference: 1063786

Crystal structure: contains datablocks I, global. DOI: 10.1107/S2056989015008890/wm5156sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S2056989015008890/wm5156Isup2.hkl

checkCIF report

Synthesis and crystallization top

CdSO₄·3/8H₂O was purchased from Merck and 4-(hydroxymethyl)pyridine and Ba(NCS)₂·3H₂O were purchased from Alfa Aesar. Cd(NCS)₂ was synthesized by stirring 17.5 g (57.0 mmol) Ba(NCS)₂·3H₂O and 14.6 g (57.0 mmol) CdSO₄·3/8H₂O in 300 ml water at RT for three hours. The white residue of BaSO₄ was filtered off and dried at 353 K. The homogeneity of the product was checked by X-ray powder diffraction and elemental analysis. The title compound was prepared by the reaction of 34.3 mg (0.15 mmol) Cd(NCS)₂ and 32.7 mg (0.30 mmol) 4-(hydroxymethyl)pyridine in 1.5 ml methanol at RT. After one week suitable crystals of the title compound were obtained.

Refinement top

The carbon-bound hydrogen atoms were positioned with idealized geometry and were refined with U_iso(H) = 1.2U_eq(C) using a riding model with C—H = 0.95 Å for aromatic and C—H = 0.99 Å for methylene H atoms. The oxygen-bound hydrogen atoms were located in a difference map. For the non-coordinating hydroxyl group the H atom was positioned with idealized geometry allowed to rotate but not to tip, and for the coordinating hydroxyl group its bond length was set to an ideal value of 0.84 Å. Finally, these H atoms were refined with U_iso(H) = 1.5U_eq(O) using a riding model. The pyridine ring of one of the 4-(hydroxymethyl)pyridine ligands is disordered and was refined using a split model in two orientations with an occupancy ratio of 0.46:0.54.

Related literature top

For similar structures with thiocyanate anions in bridging coordination to cadmium, see: Banerjee et al. (2005); Tahli et al. (2011).

Computing details top

Data collection: X-AREA (Stoe, 2008); cell refinement: X-AREA (Stoe, 2008); data reduction: X-AREA (Stoe, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2013 (Sheldrick, 2015); molecular graphics: XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999); software used to prepare material for publication: publCIF (Westrip, 2010).

Figures top

	Fig. 1. Part of the crystal structure of the title compound with labelling and displacement ellipsoids drawn at the 50% probability level. [Symmetry codes: (i) -x + 1, -y + 1, -z + 1; (ii) -x + 2, -y + 1, -z + 1.]
	Fig. 2. Crystal structure of the title compound in a view approximately along [001]. Intermolecular O—H···S hydrogen bonding is shown as dashed lines; the disordered pyridine rings are omitted for clarity.

Poly[[µ-4-(hydroxymethyl)pyridine-κ²N:O][4-\ (hydroxymethyl)pyridine-κN](µ-thiocyanato-κ²N:S)\ (thiocyanato-κN)cadmium] top

Crystal data top

[Cd(NCS)₂(C₆H₇NO)₂]	F(000) = 888
M_r = 446.81	D_x = 1.746 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
a = 10.9124 (3) Å	θ = 1.9–26.7°
b = 20.3261 (6) Å	µ = 1.54 mm⁻¹
c = 7.9722 (2) Å	T = 200 K
β = 105.965 (2)°	Block, colorless
V = 1700.08 (8) Å³	0.47 × 0.33 × 0.20 mm
Z = 4

Data collection top

Stoe IPDS-2 diffractometer	3259 reflections with I > 2σ(I)
ω scans	R_int = 0.063
Absorption correction: numerical (X-SHAPE and X-RED 32; Stoe, 2008)	θ_max = 26.7°, θ_min = 1.9°
T_min = 0.526, T_max = 0.672	h = −13→13
25370 measured reflections	k = −25→25
3597 independent reflections	l = −10→10

Refinement top

Refinement on F²	0 restraints
Least-squares matrix: full	Hydrogen site location: mixed
R[F² > 2σ(F²)] = 0.025	H-atom parameters constrained
wR(F²) = 0.058	w = 1/[σ²(F_o²) + (0.0217P)² + 1.0598P] where P = (F_o² + 2F_c²)/3
S = 1.12	(Δ/σ)_max = 0.003
3597 reflections	Δρ_max = 0.39 e Å⁻³
245 parameters	Δρ_min = −0.44 e Å⁻³

Crystal data top

[Cd(NCS)₂(C₆H₇NO)₂]	V = 1700.08 (8) Å³
M_r = 446.81	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 10.9124 (3) Å	µ = 1.54 mm⁻¹
b = 20.3261 (6) Å	T = 200 K
c = 7.9722 (2) Å	0.47 × 0.33 × 0.20 mm
β = 105.965 (2)°

Data collection top

Stoe IPDS-2 diffractometer	3597 independent reflections
Absorption correction: numerical (X-SHAPE and X-RED 32; Stoe, 2008)	3259 reflections with I > 2σ(I)
T_min = 0.526, T_max = 0.672	R_int = 0.063
25370 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.025	0 restraints
wR(F²) = 0.058	H-atom parameters constrained
S = 1.12	Δρ_max = 0.39 e Å⁻³
3597 reflections	Δρ_min = −0.44 e Å⁻³
245 parameters

Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Cd1	0.70099 (2)	0.59480 (2)	0.62587 (2)	0.02720 (6)
N1	0.8330 (2)	0.65716 (10)	0.8375 (3)	0.0371 (5)
C1	0.9127 (2)	0.68944 (11)	0.9253 (3)	0.0274 (5)
S1	1.02442 (6)	0.73463 (3)	1.05226 (9)	0.03659 (15)
N2	0.4160 (2)	0.45729 (11)	0.6240 (3)	0.0390 (5)
C2	0.4891 (2)	0.49106 (11)	0.7172 (3)	0.0291 (5)
S2	0.59224 (7)	0.53855 (3)	0.85273 (8)	0.04034 (16)
N11	0.5601 (2)	0.68370 (10)	0.5577 (3)	0.0338 (5)
C11	0.4387 (3)	0.67718 (14)	0.4676 (4)	0.0477 (7)
H11	0.4082	0.6342	0.4318	0.057*
C12	0.3544 (3)	0.72883 (15)	0.4229 (4)	0.0515 (8)
H12	0.2685	0.7212	0.3582	0.062*
C13	0.3958 (3)	0.79188 (13)	0.4729 (4)	0.0396 (6)
C14	0.5211 (3)	0.79861 (14)	0.5691 (5)	0.0587 (9)
H14	0.5536	0.8409	0.6090	0.070*
C15	0.5992 (3)	0.74464 (13)	0.6074 (5)	0.0521 (8)
H15	0.6855	0.7509	0.6726	0.062*
C16	0.3100 (3)	0.85176 (15)	0.4315 (5)	0.0578 (9)
H16A	0.2975	0.8690	0.5418	0.069*
H16B	0.3538	0.8863	0.3821	0.069*
O11	0.1919 (2)	0.84038 (11)	0.3164 (3)	0.0560 (6)
H11O	0.1440	0.8225	0.3695	0.084*
N21	0.8576 (2)	0.51330 (10)	0.6674 (3)	0.0331 (5)
C21	0.9847 (8)	0.5311 (4)	0.7358 (11)	0.0369 (17)	0.46
H21	1.0044	0.5753	0.7720	0.044*	0.46
C22	1.0837 (8)	0.4867 (4)	0.7529 (10)	0.0371 (17)	0.46
H22	1.1695	0.5001	0.8019	0.045*	0.46
C23	1.0562 (2)	0.42284 (12)	0.6982 (3)	0.0315 (5)
C24	0.9315 (9)	0.4061 (4)	0.6329 (12)	0.0421 (19)	0.46
H24	0.9090	0.3620	0.5981	0.050*	0.46
C25	0.8377 (10)	0.4528 (5)	0.6170 (13)	0.040 (2)	0.46
H25	0.7521	0.4396	0.5653	0.048*	0.46
C21'	0.9611 (8)	0.5162 (4)	0.7970 (9)	0.0456 (18)	0.54
H21'	0.9666	0.5494	0.8825	0.055*	0.54
C22'	1.0627 (8)	0.4740 (4)	0.8169 (9)	0.0435 (17)	0.54
H22'	1.1371	0.4797	0.9113	0.052*	0.54
C24'	0.9438 (7)	0.4180 (3)	0.5626 (9)	0.0372 (15)	0.54
H24'	0.9342	0.3840	0.4781	0.045*	0.54
C25'	0.8466 (9)	0.4627 (4)	0.5515 (10)	0.0365 (17)	0.54
H25'	0.7697	0.4581	0.4606	0.044*	0.54
C26	1.1645 (3)	0.37527 (14)	0.7161 (4)	0.0394 (6)
H26A	1.2445	0.3965	0.7837	0.047*
H26B	1.1497	0.3364	0.7828	0.047*
O21	1.17960 (17)	0.35385 (8)	0.5527 (2)	0.0352 (4)
H21O	1.1185	0.3283	0.5100	0.053*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cd1	0.02612 (10)	0.02547 (9)	0.02941 (10)	−0.00284 (6)	0.00661 (7)	−0.00213 (6)
N1	0.0362 (12)	0.0363 (11)	0.0353 (11)	−0.0040 (10)	0.0041 (10)	−0.0081 (9)
C1	0.0310 (12)	0.0257 (10)	0.0268 (11)	0.0038 (9)	0.0101 (10)	0.0012 (9)
S1	0.0352 (3)	0.0342 (3)	0.0357 (3)	−0.0051 (3)	0.0018 (3)	−0.0052 (3)
N2	0.0413 (13)	0.0408 (11)	0.0337 (11)	−0.0132 (10)	0.0081 (10)	−0.0055 (9)
C2	0.0319 (13)	0.0285 (11)	0.0298 (12)	0.0006 (10)	0.0135 (10)	0.0028 (9)
S2	0.0436 (4)	0.0491 (4)	0.0293 (3)	−0.0211 (3)	0.0117 (3)	−0.0072 (3)
N11	0.0285 (11)	0.0324 (10)	0.0381 (11)	−0.0011 (8)	0.0052 (9)	−0.0008 (9)
C11	0.0339 (15)	0.0357 (14)	0.0641 (19)	0.0000 (11)	−0.0025 (13)	−0.0130 (13)
C12	0.0317 (15)	0.0474 (16)	0.064 (2)	0.0022 (12)	−0.0054 (14)	−0.0131 (14)
C13	0.0342 (14)	0.0353 (13)	0.0474 (15)	0.0020 (11)	0.0083 (12)	0.0023 (11)
C14	0.0390 (17)	0.0307 (13)	0.093 (3)	−0.0030 (12)	−0.0039 (17)	−0.0012 (15)
C15	0.0320 (15)	0.0327 (13)	0.080 (2)	−0.0039 (11)	−0.0046 (15)	−0.0001 (14)
C16	0.0403 (17)	0.0426 (16)	0.082 (2)	0.0062 (13)	0.0033 (16)	0.0040 (16)
O11	0.0403 (12)	0.0575 (13)	0.0648 (14)	0.0061 (10)	0.0053 (10)	0.0117 (11)
N21	0.0369 (12)	0.0297 (10)	0.0348 (11)	0.0041 (9)	0.0132 (9)	0.0021 (8)
C21	0.032 (4)	0.033 (3)	0.043 (5)	−0.002 (3)	0.005 (3)	−0.012 (3)
C22	0.031 (3)	0.048 (4)	0.032 (5)	0.006 (3)	0.008 (3)	−0.009 (3)
C23	0.0361 (13)	0.0318 (11)	0.0301 (12)	0.0034 (10)	0.0150 (10)	0.0053 (9)
C24	0.044 (4)	0.026 (3)	0.057 (6)	−0.002 (3)	0.014 (4)	−0.003 (4)
C25	0.029 (4)	0.029 (4)	0.063 (7)	−0.004 (3)	0.016 (5)	0.000 (4)
C21'	0.051 (5)	0.050 (4)	0.032 (4)	0.014 (3)	0.005 (3)	−0.009 (3)
C22'	0.044 (4)	0.052 (4)	0.028 (4)	0.012 (3)	0.001 (3)	−0.009 (3)
C24'	0.041 (3)	0.031 (3)	0.038 (4)	0.004 (2)	0.009 (3)	−0.005 (3)
C25'	0.035 (4)	0.031 (3)	0.041 (4)	−0.001 (3)	0.005 (3)	−0.003 (3)
C26	0.0435 (15)	0.0432 (14)	0.0353 (14)	0.0099 (12)	0.0170 (12)	0.0054 (11)
O21	0.0388 (10)	0.0305 (8)	0.0427 (10)	−0.0039 (7)	0.0217 (8)	−0.0027 (7)

Geometric parameters (Å, º) top

Cd1—N1	2.279 (2)	N21—C25	1.294 (11)
Cd1—N2ⁱ	2.306 (2)	N21—C21'	1.305 (8)
Cd1—N11	2.337 (2)	N21—C25'	1.366 (9)
Cd1—N21	2.337 (2)	N21—C21	1.392 (9)
Cd1—O21ⁱⁱ	2.4153 (17)	C21—C22	1.385 (12)
Cd1—S2	2.6771 (7)	C21—H21	0.9500
N1—C1	1.158 (3)	C22—C23	1.376 (9)
C1—S1	1.636 (2)	C22—H22	0.9500
N2—C2	1.155 (3)	C23—C24	1.360 (9)
N2—Cd1ⁱ	2.306 (2)	C23—C22'	1.395 (8)
C2—S2	1.643 (2)	C23—C24'	1.398 (8)
N11—C11	1.329 (3)	C23—C26	1.503 (4)
N11—C15	1.334 (3)	C24—C25	1.376 (14)
C11—C12	1.376 (4)	C24—H24	0.9500
C11—H11	0.9500	C25—H25	0.9500
C12—C13	1.381 (4)	C21'—C22'	1.376 (11)
C12—H12	0.9500	C21'—H21'	0.9500
C13—C14	1.379 (4)	C22'—H22'	0.9500
C13—C16	1.516 (4)	C24'—C25'	1.381 (12)
C14—C15	1.371 (4)	C24'—H24'	0.9500
C14—H14	0.9500	C25'—H25'	0.9500
C15—H15	0.9500	C26—O21	1.426 (3)
C16—O11	1.380 (4)	C26—H26A	0.9900
C16—H16A	0.9900	C26—H26B	0.9900
C16—H16B	0.9900	O21—Cd1ⁱⁱ	2.4152 (17)
O11—H11O	0.8400	O21—H21O	0.8400

N1—Cd1—N2ⁱ	169.07 (8)	C21'—N21—C25'	117.8 (5)
N1—Cd1—N11	89.06 (7)	C25—N21—C21	115.7 (6)
N2ⁱ—Cd1—N11	88.96 (8)	C25—N21—Cd1	125.2 (5)
N1—Cd1—N21	90.03 (8)	C21'—N21—Cd1	121.3 (4)
N2ⁱ—Cd1—N21	90.36 (8)	C25'—N21—Cd1	120.8 (4)
N11—Cd1—N21	171.60 (7)	C21—N21—Cd1	118.8 (4)
N1—Cd1—O21ⁱⁱ	82.07 (7)	C22—C21—N21	122.3 (7)
N2ⁱ—Cd1—O21ⁱⁱ	87.11 (7)	C22—C21—H21	118.8
N11—Cd1—O21ⁱⁱ	87.47 (7)	N21—C21—H21	118.8
N21—Cd1—O21ⁱⁱ	84.13 (7)	C23—C22—C21	119.2 (7)
N1—Cd1—S2	92.58 (6)	C23—C22—H22	120.4
N2ⁱ—Cd1—S2	98.31 (6)	C21—C22—H22	120.4
N11—Cd1—S2	95.85 (6)	C24—C23—C22	117.8 (5)
N21—Cd1—S2	92.54 (5)	C22'—C23—C24'	116.6 (5)
O21ⁱⁱ—Cd1—S2	173.68 (5)	C24—C23—C26	123.6 (4)
C1—N1—Cd1	168.3 (2)	C22—C23—C26	118.7 (4)
N1—C1—S1	179.0 (2)	C22'—C23—C26	121.5 (4)
C2—N2—Cd1ⁱ	161.6 (2)	C24'—C23—C26	121.9 (4)
N2—C2—S2	179.0 (2)	C23—C24—C25	120.2 (8)
C2—S2—Cd1	99.07 (9)	C23—C24—H24	119.9
C11—N11—C15	116.3 (2)	C25—C24—H24	119.9
C11—N11—Cd1	122.87 (17)	N21—C25—C24	124.8 (9)
C15—N11—Cd1	120.82 (17)	N21—C25—H25	117.6
N11—C11—C12	124.0 (3)	C24—C25—H25	117.6
N11—C11—H11	118.0	N21—C21'—C22'	123.9 (7)
C12—C11—H11	118.0	N21—C21'—H21'	118.1
C11—C12—C13	119.4 (3)	C22'—C21'—H21'	118.1
C11—C12—H12	120.3	C21'—C22'—C23	119.8 (6)
C13—C12—H12	120.3	C21'—C22'—H22'	120.1
C14—C13—C12	116.6 (3)	C23—C22'—H22'	120.1
C14—C13—C16	120.0 (3)	C25'—C24'—C23	119.9 (6)
C12—C13—C16	123.3 (3)	C25'—C24'—H24'	120.0
C15—C14—C13	120.4 (3)	C23—C24'—H24'	120.0
C15—C14—H14	119.8	N21—C25'—C24'	121.9 (7)
C13—C14—H14	119.8	N21—C25'—H25'	119.0
N11—C15—C14	123.2 (3)	C24'—C25'—H25'	119.0
N11—C15—H15	118.4	O21—C26—C23	113.3 (2)
C14—C15—H15	118.4	O21—C26—H26A	108.9
O11—C16—C13	114.7 (3)	C23—C26—H26A	108.9
O11—C16—H16A	108.6	O21—C26—H26B	108.9
C13—C16—H16A	108.6	C23—C26—H26B	108.9
O11—C16—H16B	108.6	H26A—C26—H26B	107.7
C13—C16—H16B	108.6	C26—O21—Cd1ⁱⁱ	128.55 (16)
H16A—C16—H16B	107.6	C26—O21—H21O	106.3
C16—O11—H11O	109.5	Cd1ⁱⁱ—O21—H21O	121.7

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O11—H11O···S1ⁱⁱⁱ	0.84	2.49	3.330 (2)	174
O21—H21O···S1^iv	0.84	2.42	3.2410 (18)	164

Symmetry codes: (iii) x−1, −y+3/2, z−1/2; (iv) −x+2, y−1/2, −z+3/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O11—H11O···S1ⁱ	0.84	2.49	3.330 (2)	173.5
O21—H21O···S1ⁱⁱ	0.84	2.42	3.2410 (18)	164.4

Symmetry codes: (i) x−1, −y+3/2, z−1/2; (ii) −x+2, y−1/2, −z+3/2.

Acknowledgements

We gratefully acknowledge financial support by the State of Schleswig–Holstein. We thank Professor Dr Wolfgang Bensch for access to his experimental facilities.

References

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Volume 71| Part 6| June 2015| Pages m129-m130

doi:10.1107/S2056989015008890

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