Bis[μ-N-(3-meth­oxy-2-oxidobenzyl­idene-1:2κ2O2:O2)-l-isoleucinato-2κ2N,O]bis­(1,10-phenanthroline-1κ2N,N′)dinickel(II) methanol tetra­solvate trihydrate

Li, Y.; Guo, Z.; Dong, J.; Li, L.

doi:10.1107/S1600536812008987

Volume 68
Part 4
Pages m371-m372
April 2012

Received 18 February 2012
Accepted 29 February 2012
Online 3 March 2012

Key indicators
Single-crystal X-ray study
T = 298 K
Mean (C-C) = 0.009 Å
Disorder in main residue
R = 0.054
wR = 0.157
Data-to-parameter ratio = 13.9
Details

Bis[-N-(3-methoxy-2-oxidobenzylidene-1:2²O²:O²)-L-isoleucinato-2²N,O]bis(1,10-phenanthroline-1²N,N')dinickel(II) methanol tetrasolvate trihydrate

Yan Li,^a ^* Zhenghua Guo,^a Jianfang Dong ^a and Lianzhi Li ^a

^aSchool of Chemistry and Chemical Engineering, Liaocheng University, Shandong 252059, People's Republic of China
Correspondence e-mail: lilianzhi1963@yahoo.com.cn

In the title complex, [Ni₂(C₁₄H₁₇NO₄)₂(C₁₂H₈N₂)₂]·4CH₃OH·3H₂O, the two Ni^II ions are bridged by two Schiff base anions, leading to a dinuclear complex. One Ni^II ion is six-coordinated by four O atoms and two N atoms of two tridentate Schiff base ligands derived from the condensation of L-isoleucine and o-vanillin. The other Ni^II ion is six-coordinated by four N atoms of two 1,10-phenanthroline ligands and two O atoms of the Schiff base ligands. In the crystal, intermolecular O-HO and C-HO hydrogen bonds lead to a three-dimensional structure. Intramolecular C-HO hydrogen bonds are also present. One of the methyl groups of the L-isoleucinate moieties is disordered over two sets of sites with an occupancy ratio of 0.687 (19):0.313 (19) and two methanol molecules are half-occupied.

Related literature

For transition metal compounds containing Schiff base ligands, see: Bernal et al. (1999); Chattopadhyay et al. (2009); Chohan et al. (1998).

Experimental

Crystal data

[Ni₂(C₁₄H₁₇NO₄)₂(C₁₂H₈N₂)₂]·4CH₄O·3H₂O
M_r = 1186.62
Orthorhombic, P 2₁ 2₁ 2₁
a = 14.1827 (15) Å
b = 14.3876 (16) Å
c = 28.787 (2) Å
V = 5874.1 (10) Å³
Z = 4
Mo K radiation
= 0.71 mm^-1
T = 298 K
0.50 × 0.36 × 0.35 mm

Data collection

Bruker SMART 1000 CCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) T_min = 0.718, T_max = 0.789
24389 measured reflections
10254 independent reflections
7528 reflections with I > 2(I)
R_int = 0.058

Refinement

R[F² > 2(F²)] = 0.054
wR(F²) = 0.157
S = 1.04
10254 reflections
740 parameters
H-atom parameters constrained
_max = 0.48 e Å^-3
_min = -0.38 e Å^-3
Absolute structure: Flack (1983), 4525 Friedel pairs
Flack parameter: 0.015 (16)

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
O9-H9O1	0.82	1.88	2.693 (7)	169
O10-H10O5	0.82	1.93	2.659 (7)	147
O11-H11O10ⁱ	0.82	1.81	2.632 (10)	178
O12-H12O15ⁱⁱ	0.82	1.97	2.75 (2)	158
O13-H13O15	0.82	2.12	2.94 (3)	179
O14-H14FO6	0.85	1.91	2.760 (8)	180
O14-H14GO2ⁱ	0.85	2.05	2.901 (8)	180
O15-H15CO9	0.85	1.85	2.690 (10)	169
O15-H15DO16	0.85	2.06	2.901 (14)	171
O16-H16CO11	0.85	1.97	2.817 (13)	178
O16-H16DO14	0.85	1.95	2.798 (11)	178
C18-H18BO6	0.97	2.52	3.192 (10)	126
C29-H29O4	0.93	2.60	3.348 (8)	138
C30-H30O12ⁱⁱⁱ	0.93	2.57	3.405 (15)	149
C53-H53CO6	0.96	2.53	3.460 (12)	164
Symmetry codes: (i) $[-x+1, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (ii) x, y, z+1; (iii) $[x-{\script{1\over 2}}, -y+{\script{3\over 2}}, -z+1]$ .

Data collection: SMART (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); 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: HY2519 ).

Acknowledgements

The authors thank the Natural Science Foundation of Shandong Province (No. Y2004B02) for a research grant.

References

Bernal, M., García-Vázquez, J. A., Romero, J., Gómez, C., Durán, M. L., Sousa, A., Sousa-Pedrares, A., Rose, D. J., Maresca, K. P. & Zubieta, J. (1999). Inorg. Chim. Acta, 295, 39-47.
Bruker (2007). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.
Chattopadhyay, S., Chakraborty, P., Drew, M. G. B. & Ghosh, A. (2009). Inorg. Chim. Acta, 362, 502-508.
Chohan, Z. H., Praveen, M. & Ghaffer, A. (1998). Synth. React. Inorg. Met. Org. Chem. 28, 1673-1687.
Flack, H. D. (1983). Acta Cryst. A39, 876-881.
Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.

metal-organic compounds

Bis[-N-(3-methoxy-2-oxidobenzylidene-1:22O2:O2)-L-isoleucinato-22N,O]bis(1,10-phenanthroline-12N,N')dinickel(II) methanol tetrasolvate trihydrate