Bis(μ-2,4-dihy­droxy­benzoato-κ2O:O′)bis­[aqua­(2,4-dihy­droxy­benzoato-κO)(1,10-phenanthroline-κ2N,N′)cadmium(II)]

Nie, J.-J.; Pan, T.-T.; Su, J.-R.; Xu, D.-J.

doi:10.1107/S1600536810021252

Volume 66
Part 7
Pages m760-m761
July 2010

Received 16 May 2010
Accepted 3 June 2010
Online 9 June 2010

Key indicators
Single-crystal X-ray study
T = 296 K
Mean (C-C) = 0.004 Å
Disorder in main residue
R = 0.028
wR = 0.067
Data-to-parameter ratio = 13.0
Details

Bis(-2,4-dihydroxybenzoato-²O:O')bis[aqua(2,4-dihydroxybenzoato-O)(1,10-phenanthroline-²N,N')cadmium(II)]

Jing-Jing Nie,^a Tian-Tian Pan,^a Jian-Rong Su ^a and Duan-Jun Xu ^a ^*

^aDepartment of Chemistry, Zhejiang University, People's Republic of China
Correspondence e-mail: xudj@mail.hz.zj.cn

In the title centrosymmetric dimeric Cd^II complex, [Cd₂(C₇H₅O₄)₄(C₁₂H₈N₂)₂(H₂O)₂], the Cd^II cation is coordinated by a bidentate phenanthroline (phen) ligand, three dihydroxybenzoate (dhba) anions and one water molecule in a distorted CdN₂O₄ octahedral geometry. Among the dhba anions, two anions bridge two Cd^II cations to form the dimeric complex with significant different Cd-O bond distances of 2.2215 (19) and 2.406 (2) Å. The centroid-centroid distance of 3.4615 (19) Å between two nearly parallel benzene rings of the dhba and phen ligands coordinating to the same Cd^II cation indicates the existence of intramolecular [pi] - [pi] stacking in the complex. Extensive O-HO hydrogen bonding and intermolecular weak C-HO hydrogen bonding help to stabilize the crystal structure. One hydroxy group of the monodentate dhba ligand is disordered over two sites with a site-occupancy ratio of 0.9:0.1.

Related literature

For the correlation between [pi] - [pi] stacking and electron-transfer processes in some biological systems, see: Deisenhofer & Michel (1989). For general background to [pi] - [pi] stacking, see: Li et al. (2005). For [pi] - [pi] stacking involving a dihydroxybenzoate ligand in an Ni complex, see: Yang et al. (2006). Intramolecular [pi] - [pi] stacking was previously observed in a Sr complex with a hydroxybenzoate ligand, see: Su et al. (2005).

Experimental

Crystal data

[Cd₂(C₇H₅O₄)₄(C₁₂H₈N₂)₂(H₂O)₂]
M_r = 1233.68
Monoclinic, P 2₁ /n
a = 14.899 (4) Å
b = 6.874 (2) Å
c = 23.400 (6) Å
= 103.378 (2)°
V = 2331.4 (11) Å³
Z = 2
Mo K radiation
= 1.00 mm^-1
T = 296 K
0.26 × 0.17 × 0.11 mm

Data collection

Rigaku R-AXIS RAPID diffractometer
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) T_min = 0.758, T_max = 0.890
19273 measured reflections
4654 independent reflections
4015 reflections with I > 2(I)
R_int = 0.031

Refinement

R[F² > 2(F²)] = 0.028
wR(F²) = 0.067
S = 1.11
4654 reflections
358 parameters
3 restraints
H atoms treated by a mixture of independent and constrained refinement
_max = 0.66 e Å^-3
_min = -0.38 e Å^-3

Table 1
Selected bond lengths (Å)

Cd-N1	2.326 (2)
Cd-N2	2.324 (2)
Cd-O1	2.215 (2)
Cd-O5	2.406 (2)
Cd-O6ⁱ	2.2215 (19)
Cd-O9	2.361 (2)
Symmetry code: (i) -x+1, -y+1, -z+1.

Table 2
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
O3-H3AO2	0.82	1.81	2.540 (3)	148
O3'-H3BO1	0.82	1.56	2.332 (19)	156
O4-H4AO7ⁱⁱ	0.82	1.91	2.719 (3)	172
O7-H7AO6	0.82	1.80	2.523 (3)	147
O8-H8AO3ⁱⁱⁱ	0.82	1.94	2.752 (3)	169
O9-H9AO2	0.86 (1)	1.97 (2)	2.738 (3)	148 (3)
O9-H9BO5^iv	0.86 (1)	2.03 (2)	2.842 (3)	158 (3)
C24-H24O5ⁱ	0.93	2.58	3.433 (4)	152
Symmetry codes: (i) -x+1, -y+1, -z+1; (ii) x-1, y, z; (iii) $[-x+{\script{1\over 2}}, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (iv) x, y+1, z.

Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: NG2775 ).

Acknowledgements

The project was supported by the ZIJIN project of Zhjiang University, China.

References

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Li, H., Yin, K.-L. & Xu, D.-J. (2005). Acta Cryst. C61, m19-m21.
Rigaku (1998). PROCESS-AUTO. Rigaku Corporation, Tokyo, Japan.
Rigaku/MSC (2002). CrystalStructure. Rigaku/MSC, The Woodlands, Texas, USA.
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