Bis[μ-N-(2-oxidobenzyl­idene)pyridine-2-carbohydrazidato]bis­[chlorido(methanol-κO)erbium(III)]

Yang, H.

doi:10.1107/S1600536812013979

Volume 68
Part 5
Pages m580-m581
May 2012

Received 16 March 2012
Accepted 31 March 2012
Online 13 April 2012

Key indicators
Single-crystal X-ray study
T = 128 K
Mean (C-C) = 0.006 Å
R = 0.027
wR = 0.059
Data-to-parameter ratio = 18.7
Details

Bis[-N-(2-oxidobenzylidene)pyridine-2-carbohydrazidato]bis[chlorido(methanol-O)erbium(III)]

Hua Yang ^a ^*

^aCollege of Chemistry and Chemical Engineering, Yan'an University, Yan'an, Shaanxi 716000, People's Republic of China
Correspondence e-mail: yanghua7687@163.com

In the binuclear title complex, [Er₂(C₁₃H₉N₃O₂)₂Cl₂(CH₃OH)₂], the entire molecule is generated by the application of inversion symmetry. Each Er^III ion is seven-coordinated by two O atoms and one N atom from one N-(2-oxidobenzylidene)pyridine-2-carbohydrazidate (L^2-) ligand, one O atom and one N atom from the symmetry-related L^2- ligand, one O atom of a methanol molecule and one chloride anion. The coordination geometry is based on a pseudo-pentagonal bipyramid. Linear supramolecular chains along [010] are formed in the crystal packing through O-HCl hydrogen bonds.

Related literature

For complexes containing salicylaldehyde-2-pyridinecarboxyl-hydrazone and related ligands, see: Guo et al. (2011a,b); Bai et al. (2005, 2006); Wu et al. (2004); Milway et al. (2003). For the mechanism of the hydrolysis of salicylaldehyde thiosemicarbazone, see: Narang & Aggarwal (1974).

Experimental

Crystal data

[Er₂(C₁₃H₉N₃O₂)₂Cl₂(CH₄O)₂]
M_r = 947.97
Monoclinic, P 2₁ /c
a = 9.5810 (4) Å
b = 7.0906 (3) Å
c = 22.3504 (8) Å
= 96.920 (3)°
V = 1507.31 (10) Å³
Z = 2
Mo K radiation
= 5.76 mm^-1
T = 128 K
0.15 × 0.13 × 0.12 mm

Data collection

Bruker SMART CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker 2000) T_min = 0.479, T_max = 0.545
14182 measured reflections
3732 independent reflections
2931 reflections with I > 2(I)
R_int = 0.040

Refinement

R[F² > 2(F²)] = 0.027
wR(F²) = 0.059
S = 0.99
3732 reflections
200 parameters
H-atom parameters constrained
_max = 1.25 e Å^-3
_min = -0.71 e Å^-3

Table 1
Selected bond lengths (Å)

Er1-O1	2.157 (3)
Er1-O2ⁱ	2.284 (3)
Er1-O2	2.316 (3)
Er1-O3	2.327 (3)
Er1-N3	2.433 (3)
Er1-N1	2.488 (3)
Er1-Cl1	2.5901 (12)
Symmetry code: (i) -x+1, -y+2, -z+1.

Table 2
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
O3-H7Cl1ⁱⁱ	0.95	2.42	3.128 (4)	131
Symmetry code: (ii) x, y+1, z.

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: TK5069 ).

Acknowledgements

The author appreciates financial support from Yanan University (grant No. YD2011-20) and the Science and Technology Bureau of Yanan City (grant No. kn2009-16).

References

Bai, Y., Dang, D. B., Cao, X., Duan, C. Y. & Meng, Q. J. (2006). Inorg. Chem. Commun. 9, 86-89.
Bai, Y., Dang, D. B., Duan, C. Y., Song, Y. & Meng, Q. J. (2005). Inorg. Chem. 44, 5972-5974.
Bruker (2000). SADABS, SAINT and SMART. Bruker AXS Inc., Madison, Wisconsin, USA.
Guo, Y. N., Chen, X. H., Xue, S. F. & Tang, J. K. (2011a). Inorg. Chem. 50, 9705-9713.
Guo, Y. N., Xu, G. F., Wernsdorfer, W., Ungur, L., Guo, Y., Tang, J. K., Zhang, H. J., Chibotaru, L. F. & Powell, A. K. (2011b). J. Am. Chem. Soc. 133, 11948-11951.
Milway, V. A., Zhao, L., Abedin, T. S. M., Thompson, L. K. & Xu, Z. Q. (2003). Polyhedron, 22, 1271-1279.
Narang, K. K. & Aggarwal, A. (1974). Inorg. Chim. Acta, 9, 137-142.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Wu, W. S., Feng, Y. L., Lan, X. R. & Huang, T. T. (2004). Chin. J. Appl. Chem. 21, 135-139.

metal-organic compounds