Poly[octa-μ-aqua-tetra­aqua­bis(μ4-5-sulfonatobenzene-1,3-dicarboxyl­ato)nickel(II)tetra­sodium]

Bing-Yu Zhang; Jing-Jing Nie; Duan-Jun Xu

doi:10.1107/S1600536809009489

. 2009 Mar 25;65(Pt 4):m429–m430. doi: 10.1107/S1600536809009489

Poly[octa-μ-aqua-tetraaquabis(μ₄-5-sulfonatobenzene-1,3-dicarboxylato)nickel(II)tetrasodium]

Bing-Yu Zhang ^a, Jing-Jing Nie ^a, Duan-Jun Xu ^a,^*

PMCID: PMC2969070 PMID: 21582369

Abstract

In the crystal structure of the title compound, [Na₄Ni(C₈H₃O₇S)₂(H₂O)₁₂]_n, the Ni^II cation occupies an inversion centre and is coordinated by the carboxyl groups of the sulfoisophthalate trianions and water molecules in a distorted octahedral geometry. Two independent Na^I atoms are connected by the carboxyl and sulfonate groups of the sulfoisophthalate ligands anions and water molecules in a distorted octahedral geometry. The sulfoisophthalate ligands and coordinated water molecules bridge the Ni^II and Na^I cations, forming a three-dimensional polymeric structure. Weak π–π stacking is present between parallel benzene rings [centroid–centroid distance = 3.9349 (10) Å]. Extensive O—H⋯O and C—H⋯O hydrogen bonding helps to stabilize the crystal structure.

Related literature

For general background, see: Su & Xu (2004 ▶); Pan et al. (2006 ▶). For the isotypic structure of the Co analogue, see: Zhang et al. (2009 ▶).

Experimental

Crystal data

[Na₄Ni(C₈H₃O₇S)₂(H₂O)₁₂]
M _r = 853.19
Monoclinic,
a = 7.8770 (9) Å
b = 17.229 (2) Å
c = 11.7474 (13) Å
β = 93.292 (4)°
V = 1591.7 (3) Å³
Z = 2
Mo Kα radiation
μ = 0.90 mm⁻¹
T = 295 K
0.30 × 0.22 × 0.20 mm

Data collection

Rigaku R-AXIS RAPID IP diffractometer
Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T _min = 0.770, T _max = 0.835
17574 measured reflections
3107 independent reflections
2866 reflections with I > 2σ(I)
R _int = 0.023

Refinement

R[F ² > 2σ(F ²)] = 0.025
wR(F ²) = 0.071
S = 1.08
3107 reflections
223 parameters
H-atom parameters constrained
Δρ_max = 0.42 e Å⁻³
Δρ_min = −0.40 e Å⁻³

Data collection: PROCESS-AUTO (Rigaku, 1998 ▶); cell refinement: PROCESS-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: ORTEP-3 for Windows (Farrugia, 1997 ▶); software used to prepare material for publication: WinGX (Farrugia, 1999 ▶).

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809009489/ng2561sup1.cif

e-65-0m429-sup1.cif^{(20.1KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809009489/ng2561Isup2.hkl

e-65-0m429-Isup2.hkl^{(149.4KB, hkl)}

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Table 1. Selected bond lengths (Å).

Ni—O1	2.0252 (11)
Ni—O8	2.0731 (14)
Ni—O9	2.0727 (11)

Open in a new tab

Table 2. Hydrogen-bond geometry (Å, °).

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O8—H8A⋯O13ⁱ	0.84	2.03	2.861 (2)	173
O8—H8B⋯O4ⁱⁱ	0.85	1.99	2.8130 (19)	162
O9—H9A⋯O7ⁱⁱⁱ	0.85	2.16	2.9854 (17)	163
O9—H9B⋯O2	0.84	1.82	2.6168 (17)	159
O10—H10A⋯O7ⁱⁱ	0.83	2.04	2.8553 (19)	167
O10—H10B⋯O3^iv	0.85	1.83	2.6615 (19)	165
O11—H11A⋯O7ⁱⁱⁱ	0.89	1.90	2.7659 (18)	167
O11—H11B⋯O3^iv	0.87	1.92	2.783 (2)	175
O12—H12A⋯O1^v	0.84	2.11	2.9470 (18)	173
O12—H12B⋯O4^vi	0.89	2.04	2.8994 (19)	163
O13—H13A⋯O4ⁱⁱ	0.84	1.94	2.733 (2)	157
O13—H13B⋯O6^vii	0.88	2.21	2.9486 (19)	141
C7—H7⋯O11^viii	0.93	2.50	3.371 (2)	157

Open in a new tab

Symmetry codes: (i) Inline graphic ; (ii) ; (iii) ; (iv) ; (v) ; (vi) ; (vii) ; (viii) .

Acknowledgments

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

supplementary crystallographic information

Comment

As a part of investigation on π-π stacking between aromatic rings (Su & Xu, 2004; Pan et al., 2006), the title Ni^II compound has recently been prepared in our laboratory, and its crystal structure is reported here.

A part of the three dimensional polymeric structure of the title compound is shown in Fig. 1. The Ni^II compound is isomorphous with the Co^II compound (Zhang et al., 2009). The Ni atom occupies a special position in an inversion centre and assumes a distorted NiO₆ octahedral geometry, The Ni—O bond distances (Table 1) are about 0.03 Å shorter than corresponding Co—O bond distances found in the isomorphous Co^II compound. Both crystallograohically indenpendent Na^I atoms are in distorted octahedral coordination geometry. The sulfoisophthalate trianions and water molecules bridge the metal atoms to form the polymeric structure.

The extensive O—H···O hydrogen bonding network presents in the crystal structue (Table 2), weak C—H···O hydrogen bonding also helps to stabilize the crystal structure. The distance between parallel the C2-benzne plane and C2^v-benzene plane is 3.551 (9) Å [symmetry code: (v) 1 - x, 1 - y, -z], and the centroids distance between the benzene rings is 3.9349 (10) Å. These findings suggest a weak π-π stacking involving sulfoisophthlate ligand.

Experimental

A water-ethanol solution (25 ml, 3:2) containing monosodium 5-sulfoisophthalate (0.270 g, 1 mmol), Na₂CO₃ (0.212 g, 2 mmol) and NiCl₂.6H₂O (0.600 g, 2.5 mmol) was refluxed for 8 h and filtered after cooling to room temperature. The single crystals of the title compound were obtained from the filtrate after 3 weeks.