Crystal structure of catena-poly[[(3-tert-butyl­pyridine-κN)(4-tert-butyl­pyridine-κN)cadmium]-di-μ-thio­cyanato-κ2N:S;κ2S:N]

Werner, J.; Reinert, T.; Jess, I.; Näther, C.

doi:10.1107/S1600536814024647

metal-organic compounds

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ISSN: 2056-9890

Volume 70| Part 12| December 2014| Pages m403-m404

doi:10.1107/S1600536814024647

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Crystal structure of catena-poly[[(3-tert-butylpyridine-κN)(4-tert-butylpyridine-κN)cadmium]-di-μ-thiocyanato-κ²N:S;κ²S:N]

Julia Werner,^a ^* Thorben Reinert,^b Inke Jess ^a and Christian Näther ^a

^aInstitut für Anorganische Chemie, Christian-Albrechts-Universität Kiel, Max-Eyth-Strasse 2, 24118 Kiel, Germany, and ^bInstitut für Physikalische Chemie, Christian-Albrechts-Universität Kiel, Max-Eyth-Strasse 1, 24118 Kiel, Germany
^*Correspondence e-mail: jwerner@ac.uni-kiel.de

Edited by S. Parkin, University of Kentucky, USA (Received 25 October 2014; accepted 10 November 2014; online 19 November 2014)

In the crystal structure of the title compound, [Cd(NCS)₂(C₉H₁₃N)₂]_n, the Cd^II cations are coordinated in a slightly distorted octahedral geometry by one 3-tert-butylpyridine ligand, one 4-tert-butylpyridine ligand and two pairs of translationally-equivalent μ-1,3-bridging thiocyanate ligands, all of which are in general positions. These μ-1,3-bridging thiocyante anions bridge the Cd^II cations, forming chains that propagate parallel to the b axis.

Keywords: crystal structure; cadmium coordination polymer; μ-1,3-thiocyanate anions.

CCDC reference: 1033510

1. Related literature

For related crystal structures with μ-1,3-bridging thiocyanate anions, see: Banerjee et al. (2005 ); Reinert et al. (2012a ,b ); Tahli et al. (2011 ).

2. Experimental

2.1. Crystal data

[Cd(NCS)₂(C₉H₁₃N)₂]
M_r = 498.97
Monoclinic, P 2₁ /c
a = 20.0917 (8) Å
b = 5.9503 (2) Å
c = 21.0198 (9) Å
β = 115.902 (3)°
V = 2260.51 (15) Å³
Z = 4
Mo Kα radiation
μ = 1.16 mm⁻¹
T = 293 K
0.16 × 0.12 × 0.09 mm

2.2. Data collection

STOE IPDS-2 diffractometer
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008 ) T_min = 0.760, T_max = 0.895
25365 measured reflections
5407 independent reflections
4159 reflections with I > 2σ(I)
R_int = 0.044

2.3. Refinement

R[F² > 2σ(F²)] = 0.046
wR(F²) = 0.084
S = 1.14
5407 reflections
244 parameters
H-atom parameters constrained
Δρ_max = 0.41 e Å⁻³
Δρ_min = −0.50 e Å⁻³

Data collection: X-AREA (Stoe & Cie, 2008); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2011 ); software used to prepare material for publication: publCIF (Westrip, 2010 ).

Supporting information

CCDC reference: 1033510

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536814024647/pk2535sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536814024647/pk2535Isup2.hkl

checkCIF report

Synthesis and crystallization top

CdSO₄·8/3H₂O was purchased from Merck, and 4-tert-butylpyridine and Ba(NCS)₂·3H₂O were purchased from Alfa Aesar. The 4-tert-butylpyridine has a purity of only 97% and is contaminated with 3-tert-butylpyridine, which cannot be separated. Cd(NCS)₂ was synthesized by stirring 17.5 g (57.00 mmol) Ba(NCS)₂·3H₂O and 14.6 g (57.00 mmol) CdSO₄·8/3H₂O in 300 mL H₂O at RT for three hours. The white residue of BaSO₄ was filtered off and the solvent was evaporated by heating. The homogeneity of the product was investigated by X-ray powder diffraction and elemental analysis. The title compound was prepared by the reaction of (0.15 mmol) 34.3 mg Cd(NCS)₂ and (0.15 mmol) 22.2 µL 4-tert-butylpyridine in 1.0 mL H₂O at 80 °C in a closed 10 mL glass culture tube. After several days, colorless crystalline blocks were obtained.

Refinement top

Carbon-bound H atoms were positioned with idealized geometry and refined with U_iso(H) = 1.2 U_eq(C) using a riding model with C—H = 0.95 Å for aromatic and C—H = 0.99 Å for methyl H atoms.

Related literature top

For related crystal structures with µ-1,3-bridging thiocyanato anions, see: Banerjee et al. (2005); Reinert et al. (2012a,b); Tahli et al. (2011).

Computing details top

Data collection: X-AREA (Stoe & Cie, 2008); cell refinement: X-AREA (Stoe & Cie, 2008); data reduction: X-AREA (Stoe & Cie, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2011); software used to prepare material for publication: publCIF (Westrip, 2010).

Figures top

Fig. 1: Crystal structure of the title compound. Displacement ellipsoids are drawn at the 50% probability level. Symmetry code: i: (x, y+1, z); ii: (x, y-1, z).

catena-Poly[[(3-tert-butylpyridine-κN)(4-tert-butylpyridine-κN)cadmium]-di-µ-thiocyanato-κ²N:S;κ²S:N] top

Crystal data top

[Cd(NCS)₂(C₉H₁₃N)₂]	F(000) = 1016
M_r = 498.97	D_x = 1.466 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 25365 reflections
a = 20.0917 (8) Å	θ = 2.0–28.0°
b = 5.9503 (2) Å	µ = 1.16 mm⁻¹
c = 21.0198 (9) Å	T = 293 K
β = 115.902 (3)°	Block, colourless
V = 2260.51 (15) Å³	0.16 × 0.12 × 0.09 mm
Z = 4

Data collection top

STOE IPDS-2 diffractometer	5407 independent reflections
Radiation source: fine-focus sealed tube	4159 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.044
ω scans	θ_max = 28.0°, θ_min = 2.0°
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008)	h = −26→26
T_min = 0.760, T_max = 0.895	k = −7→7
25365 measured reflections	l = −27→27

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)] = 0.046	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.084	H-atom parameters constrained
S = 1.14	w = 1/[σ²(F_o²) + (0.0326P)² + 0.8678P] where P = (F_o² + 2F_c²)/3
5407 reflections	(Δ/σ)_max = 0.001
244 parameters	Δρ_max = 0.41 e Å⁻³
0 restraints	Δρ_min = −0.50 e Å⁻³

Crystal data top

[Cd(NCS)₂(C₉H₁₃N)₂]	V = 2260.51 (15) Å³
M_r = 498.97	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 20.0917 (8) Å	µ = 1.16 mm⁻¹
b = 5.9503 (2) Å	T = 293 K
c = 21.0198 (9) Å	0.16 × 0.12 × 0.09 mm
β = 115.902 (3)°

Data collection top

STOE IPDS-2 diffractometer	5407 independent reflections
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008)	4159 reflections with I > 2σ(I)
T_min = 0.760, T_max = 0.895	R_int = 0.044
25365 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.046	0 restraints
wR(F²) = 0.084	H-atom parameters constrained
S = 1.14	Δρ_max = 0.41 e Å⁻³
5407 reflections	Δρ_min = −0.50 e Å⁻³
244 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.

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 > 2sigma(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
Cd1	0.732991 (14)	0.24172 (4)	0.269228 (13)	0.04067 (8)
N1	0.67220 (19)	0.5638 (5)	0.20986 (17)	0.0535 (7)
C1	0.65872 (17)	0.7440 (6)	0.18809 (16)	0.0415 (6)
S1	0.63714 (5)	0.99805 (14)	0.15449 (5)	0.0484 (2)
N2	0.79392 (17)	−0.0756 (5)	0.32949 (17)	0.0514 (7)
C2	0.80555 (17)	−0.2557 (6)	0.35212 (16)	0.0421 (6)
S2	0.82427 (6)	−0.51157 (15)	0.38460 (5)	0.0554 (2)
N11	0.81232 (17)	0.2863 (5)	0.21360 (15)	0.0482 (7)
C11	0.8505 (3)	0.4716 (7)	0.2206 (2)	0.0724 (13)
H11	0.8473	0.5835	0.2501	0.087*
C12	0.8948 (3)	0.5105 (7)	0.1870 (2)	0.0713 (13)
H12	0.9209	0.6449	0.1950	0.086*
C13	0.9014 (2)	0.3547 (6)	0.14183 (19)	0.0443 (7)
C14	0.8606 (2)	0.1617 (7)	0.1342 (3)	0.0638 (11)
H14	0.8622	0.0474	0.1047	0.077*
C15	0.8174 (2)	0.1363 (7)	0.1698 (2)	0.0638 (11)
H15	0.7901	0.0047	0.1623	0.077*
C16	0.9479 (2)	0.3988 (7)	0.1019 (2)	0.0509 (8)
C17	0.9747 (3)	0.1778 (9)	0.0830 (3)	0.0847 (15)
H17A	1.0038	0.2105	0.0580	0.127*
H17B	0.9328	0.0882	0.0536	0.127*
H17C	1.0043	0.0967	0.1255	0.127*
C18	0.8990 (3)	0.5207 (10)	0.0334 (3)	0.0867 (16)
H18A	0.9269	0.5508	0.0072	0.130*
H18B	0.8821	0.6598	0.0444	0.130*
H18C	0.8571	0.4282	0.0056	0.130*
C19	1.0150 (3)	0.5424 (10)	0.1453 (3)	0.0862 (16)
H19A	1.0432	0.5674	0.1191	0.129*
H19B	1.0452	0.4664	0.1888	0.129*
H19C	0.9990	0.6840	0.1557	0.129*
N21	0.64660 (16)	0.2045 (5)	0.31532 (16)	0.0470 (7)
C21	0.5826 (2)	0.3142 (7)	0.2852 (2)	0.0546 (9)
H21	0.5733	0.4039	0.2459	0.066*
C22	0.5296 (2)	0.2999 (7)	0.3098 (2)	0.0629 (11)
H22	0.4855	0.3795	0.2879	0.076*
C23	0.5429 (2)	0.1660 (7)	0.3673 (2)	0.0573 (10)
H23	0.5075	0.1554	0.3846	0.069*
C24	0.60838 (19)	0.0467 (6)	0.39999 (18)	0.0454 (8)
C25	0.6582 (2)	0.0755 (6)	0.37141 (19)	0.0473 (8)
H25	0.7030	−0.0005	0.3928	0.057*
C26	0.6255 (2)	−0.0980 (7)	0.4648 (2)	0.0587 (10)
C27	0.6837 (4)	−0.2738 (12)	0.4745 (4)	0.133 (3)
H27A	0.6662	−0.3706	0.4339	0.200*
H27B	0.6933	−0.3611	0.5160	0.200*
H27C	0.7285	−0.2011	0.4797	0.200*
C28	0.6512 (6)	0.0518 (13)	0.5280 (3)	0.171 (4)
H28A	0.6627	−0.0373	0.5696	0.257*
H28B	0.6127	0.1569	0.5223	0.257*
H28C	0.6945	0.1319	0.5327	0.257*
C29	0.5577 (3)	−0.2282 (11)	0.4579 (4)	0.1055 (19)
H29A	0.5416	−0.3255	0.4175	0.158*
H29B	0.5188	−0.1249	0.4521	0.158*
H29C	0.5699	−0.3165	0.4997	0.158*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cd1	0.04773 (12)	0.03305 (11)	0.04745 (12)	0.00141 (12)	0.02654 (10)	0.00495 (11)
N1	0.064 (2)	0.0352 (15)	0.0566 (18)	0.0003 (14)	0.0216 (16)	0.0037 (14)
C1	0.0434 (15)	0.0405 (15)	0.0407 (15)	−0.0062 (17)	0.0185 (13)	−0.0032 (17)
S1	0.0550 (5)	0.0374 (4)	0.0470 (5)	0.0007 (4)	0.0167 (4)	0.0063 (4)
N2	0.0536 (18)	0.0355 (14)	0.0603 (19)	0.0036 (13)	0.0204 (15)	0.0053 (14)
C2	0.0422 (15)	0.0421 (16)	0.0425 (15)	−0.0014 (17)	0.0190 (13)	−0.0044 (17)
S2	0.0675 (6)	0.0385 (4)	0.0481 (5)	−0.0007 (4)	0.0141 (5)	0.0058 (4)
N11	0.0579 (17)	0.0447 (16)	0.0456 (15)	−0.0034 (14)	0.0260 (14)	−0.0023 (13)
C11	0.108 (4)	0.055 (2)	0.084 (3)	−0.028 (2)	0.070 (3)	−0.024 (2)
C12	0.097 (3)	0.057 (2)	0.086 (3)	−0.032 (2)	0.065 (3)	−0.021 (2)
C13	0.0418 (18)	0.0475 (18)	0.0463 (19)	0.0013 (15)	0.0218 (16)	0.0042 (15)
C14	0.069 (3)	0.055 (2)	0.090 (3)	−0.017 (2)	0.055 (3)	−0.023 (2)
C15	0.063 (2)	0.052 (2)	0.088 (3)	−0.017 (2)	0.044 (2)	−0.011 (2)
C16	0.048 (2)	0.059 (2)	0.053 (2)	0.0025 (17)	0.0279 (17)	0.0068 (17)
C17	0.087 (3)	0.081 (3)	0.115 (4)	0.013 (3)	0.071 (3)	0.004 (3)
C18	0.082 (3)	0.117 (4)	0.074 (3)	0.019 (3)	0.047 (3)	0.038 (3)
C19	0.064 (3)	0.111 (4)	0.097 (4)	−0.026 (3)	0.047 (3)	−0.013 (3)
N21	0.0460 (15)	0.0488 (17)	0.0530 (16)	0.0030 (13)	0.0278 (14)	0.0065 (13)
C21	0.052 (2)	0.060 (2)	0.054 (2)	0.0076 (17)	0.0246 (18)	0.0103 (17)
C22	0.046 (2)	0.074 (3)	0.071 (3)	0.0149 (19)	0.0288 (19)	0.013 (2)
C23	0.048 (2)	0.075 (2)	0.058 (2)	−0.0019 (19)	0.0309 (19)	−0.0028 (19)
C24	0.0450 (18)	0.055 (2)	0.0395 (17)	−0.0068 (16)	0.0220 (15)	−0.0049 (15)
C25	0.0436 (18)	0.054 (2)	0.0477 (19)	0.0038 (16)	0.0230 (16)	0.0046 (16)
C26	0.063 (2)	0.071 (3)	0.049 (2)	−0.007 (2)	0.0303 (19)	0.0052 (19)
C27	0.118 (5)	0.159 (7)	0.151 (6)	0.059 (5)	0.084 (5)	0.103 (5)
C28	0.323 (12)	0.124 (6)	0.047 (3)	−0.086 (7)	0.063 (5)	−0.013 (3)
C29	0.094 (4)	0.110 (5)	0.124 (5)	−0.012 (4)	0.058 (4)	0.038 (4)

Geometric parameters (Å, º) top

Cd1—N2	2.305 (3)	C18—H18A	0.9600
Cd1—N1	2.322 (3)	C18—H18B	0.9600
Cd1—N21	2.339 (3)	C18—H18C	0.9600
Cd1—N11	2.368 (3)	C19—H19A	0.9600
Cd1—S2ⁱ	2.7412 (10)	C19—H19B	0.9600
Cd1—S1ⁱⁱ	2.7513 (10)	C19—H19C	0.9600
N1—C1	1.151 (4)	N21—C21	1.330 (5)
C1—S1	1.644 (4)	N21—C25	1.339 (4)
S1—Cd1ⁱ	2.7513 (10)	C21—C22	1.375 (5)
N2—C2	1.154 (4)	C21—H21	0.9300
C2—S2	1.644 (4)	C22—C23	1.374 (6)
S2—Cd1ⁱⁱ	2.7412 (10)	C22—H22	0.9300
N11—C11	1.314 (5)	C23—C24	1.385 (5)
N11—C15	1.319 (5)	C23—H23	0.9300
C11—C12	1.378 (5)	C24—C25	1.384 (4)
C11—H11	0.9300	C24—C26	1.518 (5)
C12—C13	1.373 (5)	C25—H25	0.9300
C12—H12	0.9300	C26—C28	1.492 (7)
C13—C14	1.379 (5)	C26—C27	1.514 (7)
C13—C16	1.527 (5)	C26—C29	1.518 (6)
C14—C15	1.379 (5)	C27—H27A	0.9600
C14—H14	0.9300	C27—H27B	0.9600
C15—H15	0.9300	C27—H27C	0.9600
C16—C19	1.519 (6)	C28—H28A	0.9600
C16—C18	1.525 (6)	C28—H28B	0.9600
C16—C17	1.537 (6)	C28—H28C	0.9600
C17—H17A	0.9600	C29—H29A	0.9600
C17—H17B	0.9600	C29—H29B	0.9600
C17—H17C	0.9600	C29—H29C	0.9600

N2—Cd1—N1	179.28 (11)	H18A—C18—H18B	109.5
N2—Cd1—N21	90.40 (11)	C16—C18—H18C	109.5
N1—Cd1—N21	89.39 (11)	H18A—C18—H18C	109.5
N2—Cd1—N11	93.03 (11)	H18B—C18—H18C	109.5
N1—Cd1—N11	87.23 (11)	C16—C19—H19A	109.5
N21—Cd1—N11	175.34 (11)	C16—C19—H19B	109.5
N2—Cd1—S2ⁱ	87.88 (8)	H19A—C19—H19B	109.5
N1—Cd1—S2ⁱ	91.43 (8)	C16—C19—H19C	109.5
N21—Cd1—S2ⁱ	90.86 (8)	H19A—C19—H19C	109.5
N11—Cd1—S2ⁱ	92.42 (8)	H19B—C19—H19C	109.5
N2—Cd1—S1ⁱⁱ	92.89 (8)	C21—N21—C25	117.4 (3)
N1—Cd1—S1ⁱⁱ	87.79 (8)	C21—N21—Cd1	119.6 (2)
N21—Cd1—S1ⁱⁱ	87.21 (8)	C25—N21—Cd1	123.0 (2)
N11—Cd1—S1ⁱⁱ	89.46 (8)	N21—C21—C22	122.5 (4)
S2ⁱ—Cd1—S1ⁱⁱ	177.92 (3)	N21—C21—H21	118.8
C1—N1—Cd1	163.7 (3)	C22—C21—H21	118.8
N1—C1—S1	178.0 (3)	C23—C22—C21	118.8 (4)
C1—S1—Cd1ⁱ	98.96 (11)	C23—C22—H22	120.6
C2—N2—Cd1	161.9 (3)	C21—C22—H22	120.6
N2—C2—S2	178.6 (3)	C22—C23—C24	120.7 (3)
C2—S2—Cd1ⁱⁱ	100.68 (11)	C22—C23—H23	119.6
C11—N11—C15	115.2 (3)	C24—C23—H23	119.6
C11—N11—Cd1	121.6 (2)	C25—C24—C23	115.6 (3)
C15—N11—Cd1	122.9 (2)	C25—C24—C26	122.4 (3)
N11—C11—C12	124.1 (4)	C23—C24—C26	122.0 (3)
N11—C11—H11	118.0	N21—C25—C24	124.9 (3)
C12—C11—H11	118.0	N21—C25—H25	117.5
C13—C12—C11	121.3 (4)	C24—C25—H25	117.5
C13—C12—H12	119.3	C28—C26—C27	110.3 (6)
C11—C12—H12	119.3	C28—C26—C24	108.3 (4)
C12—C13—C14	114.3 (3)	C27—C26—C24	111.8 (3)
C12—C13—C16	122.0 (3)	C28—C26—C29	109.6 (5)
C14—C13—C16	123.6 (3)	C27—C26—C29	105.6 (5)
C13—C14—C15	120.7 (4)	C24—C26—C29	111.2 (4)
C13—C14—H14	119.6	C26—C27—H27A	109.5
C15—C14—H14	119.6	C26—C27—H27B	109.5
N11—C15—C14	124.3 (4)	H27A—C27—H27B	109.5
N11—C15—H15	117.8	C26—C27—H27C	109.5
C14—C15—H15	117.8	H27A—C27—H27C	109.5
C19—C16—C18	109.7 (4)	H27B—C27—H27C	109.5
C19—C16—C13	111.2 (3)	C26—C28—H28A	109.5
C18—C16—C13	107.7 (3)	C26—C28—H28B	109.5
C19—C16—C17	108.5 (4)	H28A—C28—H28B	109.5
C18—C16—C17	108.5 (4)	C26—C28—H28C	109.5
C13—C16—C17	111.3 (3)	H28A—C28—H28C	109.5
C16—C17—H17A	109.5	H28B—C28—H28C	109.5
C16—C17—H17B	109.5	C26—C29—H29A	109.5
H17A—C17—H17B	109.5	C26—C29—H29B	109.5
C16—C17—H17C	109.5	H29A—C29—H29B	109.5
H17A—C17—H17C	109.5	C26—C29—H29C	109.5
H17B—C17—H17C	109.5	H29A—C29—H29C	109.5
C16—C18—H18A	109.5	H29B—C29—H29C	109.5
C16—C18—H18B	109.5

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

Experimental details

Crystal data
Chemical formula	[Cd(NCS)₂(C₉H₁₃N)₂]
M_r	498.97
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	293
a, b, c (Å)	20.0917 (8), 5.9503 (2), 21.0198 (9)
β (°)	115.902 (3)
V (Å³)	2260.51 (15)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	1.16
Crystal size (mm)	0.16 × 0.12 × 0.09

Data collection
Diffractometer	STOE IPDS2 diffractometer
Absorption correction	Numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008)
T_min, T_max	0.760, 0.895
No. of measured, independent and observed [I > 2σ(I)] reflections	25365, 5407, 4159
R_int	0.044
(sin θ/λ)_max (Å⁻¹)	0.661

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.046, 0.084, 1.14
No. of reflections	5407
No. of parameters	244
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.41, −0.50

Computer programs: X-AREA (Stoe & Cie, 2008), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2011), publCIF (Westrip, 2010).

Acknowledgements

We gratefully acknowledge financial support by the DFG (project No. NA 720/5–1) and the State of Schleswig–Holstein. We thank Professor Dr Wolfgang Bensch for access to his experimental facilities.

References

Banerjee, S., Wu, B., Lassahn, P.-G., Janiak, C. & Ghosh, A. (2005). Inorg. Chim. Acta, 358, 535–544. Web of Science CSD CrossRef CAS Google Scholar
Brandenburg, K. (2011). DIAMOND. Crystal Impact GbR, Bonn, Germany. Google Scholar
Reinert, T., Jess, I. & Näther, C. (2012a). Acta Cryst. E68, m1372. CSD CrossRef IUCr Journals Google Scholar
Reinert, T., Jess, I. & Näther, C. (2012b). Acta Cryst. E68, m1333. CSD CrossRef IUCr Journals Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Stoe & Cie (2008). X-AREA, X-RED32 and X-SHAPE. Stoe & Cie, Darmstadt, Germany. Google Scholar
Tahli, A., Maclaren, J. K., Boldog, I. & Janiak, C. (2011). Inorg. Chim. Acta, 374, 506–513. Web of Science CSD CrossRef CAS Google Scholar
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920–925. Web of Science CrossRef CAS IUCr Journals Google Scholar

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Volume 70| Part 12| December 2014| Pages m403-m404

doi:10.1107/S1600536814024647

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