A salen-type trinuclear Zn2Gd complex

Tian, Y.-M.; Li, H.-F.; Han, B.-L.; Zhang, Q.; Sun, W.-B.

doi:10.1107/S160053681204634X

Volume 68
Part 12
Pages m1500-m1501
December 2012

Received 24 October 2012
Accepted 9 November 2012
Online 17 November 2012

Key indicators
Single-crystal X-ray study
T = 296 K
Mean (C-C) = 0.012 Å
R = 0.053
wR = 0.157
Data-to-parameter ratio = 19.7
Details

A salen-type trinuclear Zn₂Gd complex

Yong-Mei Tian,^a Hong-Feng Li,^a Bing-Lu Han,^a Qian Zhang ^a and Wen-Bin Sun ^a ^*

^aKey Laboratory of Functional Inorganic Material Chemistry (HLJU), Ministry of Education, School of Chemistry and Materials Science, Heilongjiang University, Harbin 150080, People's Republic of China
Correspondence e-mail: sunwbchem@gmail.com

In the trinuclear title complex, di- [mu] -acetato-1:2 [kappa] ²O:O';2:3 [kappa] ²O:O'-bis{ [mu] -6,6'-dimethoxy-2,2'-[cyclohexane-1,2-diylbis(methanylylidene)]diphenolato}-1:2 [kappa] ⁶O¹,N,N',O^1':O⁶,O^6';2:3 [kappa] ⁶O⁶,O^6':O¹,N,N',O^1'-2-gadolinium(III)-1,3-dizinc hexafluoridophosphate methanol monosolvate monohydrate, [GdZn₂(C₂₂H₂₄N₂O₄)₂(CH₃COO)₂]PF₆·CH₃OH·H₂O, the two Zn^II ions are located in the inner N₂O₂ cavities of two 6,6'-dimethoxy-2,2'-[cyclohexane-1,2-diylbis(methanylylidene)]diphenolate (L) ligands. Both Zn^II ions are five-coordinated by two O atoms and two N atoms from the L ligand and one O atom of an acetic acid molecule, giving rise to a square-pyramidal geometry around the Zn^II ions. The Gd^III ion is nine-coordinated by four O atoms from the outer O₂O₂ sites of one ligand, and three O atoms from another ligand, in which there is one non-coordinating methoxy O atom. Two further O atom from different acetate ligands complete the nine-coordinate environment.

Related literature

For crystal structures of similar trinuclear complexes of salen-type Schiff base ligands, see: Wong et al. (2006); Wang et al. (2009).

Experimental

Crystal data

[GdZn₂(C₂₂H₂₄N₂O₄)₂(C₂H₃O₂)₂]PF₆·CH₄O·H₂O
M_r = 1361.97
Monoclinic, P 2₁ /n
a = 15.8127 (12) Å
b = 20.6405 (16) Å
c = 18.5036 (14) Å
= 114.369 (1)°
V = 5501.2 (7) Å³
Z = 4
Mo K radiation
= 2.17 mm^-1
T = 296 K
0.20 × 0.18 × 0.16 mm

Data collection

Rigaku R-AXIS RAPID diffractometer
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) T_min = 0.671, T_max = 0.723
39974 measured reflections
13701 independent reflections
6858 reflections with I > 2(I)
R_int = 0.066

Refinement

R[F² > 2(F²)] = 0.053
wR(F²) = 0.157
S = 0.98
13701 reflections
695 parameters
19 restraints
H-atom parameters constrained
_max = 1.02 e Å^-3
_min = -0.71 e Å^-3

Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); 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: PV2601 ).

Acknowledgements

The authors gratefully acknowledge financial support from the NSFC of China (No. 21102039), Heilongjiang Province (Nos. 11551336 and 11521205), the Undergraduate Open Experiment Programme of Heilongjiang University and the Undergraduate Science and Technique Innovation Programme of Students and Heilongjiang University (No. QL201021).

References

Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan.
Rigaku (1998). RAPID-AUTO. Rigaku Corporation, Tokyo, Japan.
Rigaku/MSC (2002). CrystalStructure. Rigaku/MSC Inc., The Woodlands, Texas, USA.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Wang, H. L., Zhang, D. P., Ni, Z. H., Li, X. Y., Tian, L. J. & Jiang, J. Z. (2009). Inorg. Chem. 48, 5946-5956.
Wong, W. K., Yang, X. P., Jones, R. A., Rivers, J. H., Lynch, V., Lo, W. K., Xiao, D., Oye, M. M. & Holmes, A. (2006). Inorg. Chem. 45, 4340-4345.

metal-organic compounds