Bis(μ-2-{[2-(1,3-benzothia­zol-2-yl)hydrazinyl­idene]meth­yl}-6-meth­oxy­phenolato)bis­[dinitratodysprosium(III)] methanol disolvate

Xu, X.; Ding, S.; Shen, S.; Tang, J.; Liu, Z.

doi:10.1107/S1600536811019118

Volume 67
Part 6
Pages m796-m797
June 2011

Received 23 March 2011
Accepted 19 May 2011
Online 25 May 2011

Key indicators
Single-crystal X-ray study
T = 159 K
Mean (C-C) = 0.007 Å
R = 0.025
wR = 0.057
Data-to-parameter ratio = 12.0
Details

Bis(-2-{[2-(1,3-benzothiazol-2-yl)hydrazinylidene]methyl}-6-methoxyphenolato)bis[dinitratodysprosium(III)] methanol disolvate

Xuebin Xu,^a Shuai Ding,^a Si Shen,^b Jinkui Tang ^b and Zhiliang Liu ^a ^*

^aCollege of Chemistry and Chemical Engineering, Inner Mongolia University, Hohhot 010021, People's Republic of China, and ^bState Key Laboratory of Rare Earth Resource Utilization, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022, People's Republic of China.
Correspondence e-mail: cezlliu@imu.edu.cn

In the centrosymmetric dinuclear title compound, [Dy₂(C₁₅H₁₂N₃O₂S)₂(NO₃)₄]·2CH₃OH, the two Dy^III atoms are coordinated by two deprotonated 2-{[2-(1,3-benzothiazol-2-yl)hydrazinylidene]methyl}-6-methoxyphenol ligands and four nitrate ions, all of which are chelating. The crystal packing is stabilized by intermolecular N-HO hydrogen bonds and weak O-HO interactions, forming a two-dimensional network parallel to (010).

Related literature

For applications of dysprosium complexes in data storage and processing, see: Lin et al. (2010). For the preparation of the 2-{[2-(1,3-benzothiazol-2-yl)hydrazinylidene]methyl}-6-methoxyphenol ligand, see: Patil et al. (2009). For related structures, see: Lin & Hong (2009); Lin et al. (2008); Xu et al. (2010).

Experimental

Crystal data

[Dy₂(C₁₅H₁₂N₃O₂S)₂(NO₃)₄]·2CH₄O
M_r = 1233.82
Triclinic, $[P \overline 1]$
a = 9.6191 (6) Å
b = 10.1002 (7) Å
c = 11.6151 (8) Å
= 112.045 (1)°
= 105.065 (1)°
= 93.154 (1)°
V = 995.23 (12) Å³
Z = 1
Mo K radiation
= 3.92 mm^-1
T = 159 K
0.20 × 0.10 × 0.10 mm

Data collection

Rigaku Saturn CCD area-detector diffractometer
Absorption correction: multi-scan (CrystalClear; Rigaku, 2002) T_min = 0.631, T_max = 0.676
5083 measured reflections
3502 independent reflections
3162 reflections with I > 2(I)
R_int = 0.016

Refinement

R[F² > 2(F²)] = 0.025
wR(F²) = 0.057
S = 1.07
3502 reflections
292 parameters
H-atom parameters constrained
_max = 0.83 e Å^-3
_min = -0.51 e Å^-3

Table 1
Selected bond lengths (Å)

Dy1-O2	2.280 (3)
Dy1-O2ⁱ	2.374 (2)
Dy1-O1ⁱ	2.394 (3)
Dy1-O4	2.422 (3)
Dy1-O3	2.433 (3)
Dy1-N4	2.461 (3)
Dy1-O6	2.471 (3)
Dy1-N5	2.494 (3)
Dy1-O8	2.530 (3)
Symmetry code: (i) -x+1, -y, -z+2.

Table 2
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
O9-H9AO3ⁱⁱ	0.84	2.64	3.206 (4)	126
O9-H9AO8ⁱⁱⁱ	0.84	2.24	3.049 (4)	161
N9-H9O9^iv	0.88	1.91	2.751 (4)	160
Symmetry codes: (ii) x, y, z-1; (iii) -x+1, -y, -z+1; (iv) -x, -y, -z+1.

Data collection: CrystalClear (Rigaku, 2002); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg & Putz, 2006) and XP (Siemens, 1994); software used to prepare material for publication: publCIF (Westrip, 2010).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: JJ2083 ).

Acknowledgements

Financial support by the NSFC (20761004, 21061009) and the Inner Mongolia Autonomous Region Fund for Natural Science (2010MS0201) is gratefully acknowledged. This work was supported by the "211 project" of the postgraduate student programme of Inner Mongolia University.

References

Brandenburg, K. & Putz, H. (2006). DIAMOND. Crystal Impact GbR, Bonn, Germany.
Lin, P.-H., Burchell, T. J., Clérac, R. & Murugesu, M. (2008). Angew. Chem. Int. Ed. 47, 8848-8851.
Lin, S.-Y., Guo, Y.-N., Xu, G.-F. & Tang, J.-K. (2010). Chin. J. Appl. Chem. 27, 1365-1371.
Lin, Y.-C. & Hong, F.-E. (2009). Acta Cryst. E65, m1077.
Patil, S. A., Weng, C.-M., Huang, P.-C. & Hong, F.-E. (2009). Tetrahedron, 65, 2889-2897.
Rigaku (2002). CrystalClear. Rigaku Corporation, Tokyo, Japan.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Siemens (1994). XP. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA.
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.
Xu, G.-F., Wang, Q.-L., Gamez, P., Ma, Y., Clérac, R., Tang, J.-K., Yan, S.-P., Cheng, P. & Liao, D.-Z. (2010). Chem. Commun. 46, 1506-1508.

metal-organic compounds