{6,6′-Dimeth­oxy-2,2′-[(cyclo­hexane-1,2-di­yl)bis­(nitriliomethyl­idyne)]diphenolato}trinitratolanthanum(III) methanol monosolvate

Chen, P.; Bao, Y.; Yan, P.-F.; Li, G.-M.

doi:10.1107/S1600536810033453

Volume 66
Part 9
Page m1177
September 2010

Received 15 July 2010
Accepted 19 August 2010
Online 28 August 2010

Key indicators
Single-crystal X-ray study
T = 293 K
Mean (C-C) = 0.005 Å
R = 0.033
wR = 0.092
Data-to-parameter ratio = 18.4
Details

{6,6'-Dimethoxy-2,2'-[(cyclohexane-1,2-diyl)bis(nitriliomethylidyne)]diphenolato}trinitratolanthanum(III) methanol monosolvate

Peng Chen,^a Yan Bao,^a Peng-Fei Yan ^a and Guang-Ming Li ^a ^*

^aSchool of Chemistry and Materials Science, Heilongjiang University, Harbin 150080, People's Republic of China
Correspondence e-mail: gmli_2000@163.com

In the title mononuclear complex, [La(NO₃)₃(C₂₂H₂₆N₂O₄)]·CH₃OH, the La^III ion is coordinated by three bidentate nitrate counter-ions and one zwitterionic 6,6'-dimethoxy-2,2'-[(cyclohexane-1,2- diyl)bis(nitriliomethylidyne)]diphenolate ligand through two phenolate and two methoxy O atoms, while the protonated N atoms remain uncoordinated. H atoms located on the two N atoms are involved in intramolecular hydrogen bonds with the deprotonated phenol O atoms, indicating that proton migration occurs during the lanthanum complexation.

Related literature

For the preparation of the ligand, see: Koner et al. (2005). For a related structure, see: Yan et al. (2009).

Experimental

Crystal data

[La(NO₃)₃(C₂₂H₂₆N₂O₄)]·CH₄O
M_r = 739.43
Triclinic, $[P \overline 1]$
a = 9.7809 (4) Å
b = 12.8783 (5) Å
c = 13.0904 (5) Å
= 79.374 (1)°
= 68.743 (1)°
= 82.270 (1)°
V = 1506.22 (10) Å³
Z = 2
Mo K radiation
= 1.49 mm^-1
T = 293 K
0.23 × 0.20 × 0.16 mm

Data collection

Rigaku R-AXIS RAPID diffractometer
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) T_min = 0.725, T_max = 0.796
10874 measured reflections
7145 independent reflections
6526 reflections with I > 2(I)
R_int = 0.010

Refinement

R[F² > 2(F²)] = 0.033
wR(F²) = 0.092
S = 1.01
7145 reflections
389 parameters
38 restraints
H-atom parameters constrained
_max = 0.97 e Å^-3
_min = -0.77 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
N1-H1AO1	0.86	1.86	2.562 (3)	137
N2-H2AO3	0.86	1.89	2.592 (3)	138
O14-H14O5ⁱ	0.84	2.40	2.981 (7)	127
Symmetry code: (i) x, y, z-1.

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: SHELXL97.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: VM2037 ).

Acknowledgements

This work was supported financially by the National Natural Science Foundation of China (Nos. 20872030 and 20972043), Heilongjiang Province (Nos. 2009RFXXG201, GC09A402 and 2010 t d03) and Heilongjiang University.

References

Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan.
Koner, R., Lee, G. H., Wang, Y., Wei, H.-H. & Mohanta, S. (2005). Eur. J. Inorg. Chem. pp. 1500-1505.
Rigaku (1998). RAPID-AUTO. Rigaku Corporation, Tokyo, Japan.
Rigaku/MSC (2002). CrystalClear. Rigaku/MSC Inc., The Woodlands, Texas, USA.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Yan, P.-F., Bao, Y., Li, H.-F. & Li, G.-M. (2009). Acta Cryst. E65, m832.

metal-organic compounds