Hexaaqua­magnesium(II) bis­[4-(3-pyrid­yl)pyrimidine-2-sulfonate] tetra­hydrate

Yan-Ping Wang; Jian Li; Hua-Ze Dong

doi:10.1107/S160053680904344X

. 2009 Oct 28;65(Pt 11):m1436. doi: 10.1107/S160053680904344X

Hexaaquamagnesium(II) bis[4-(3-pyridyl)pyrimidine-2-sulfonate] tetrahydrate

Yan-Ping Wang ^a, Jian Li ^a, Hua-Ze Dong ^a,^*

PMCID: PMC2970970 PMID: 21578168

Abstract

The asymmetric unit of the title compound, [Mg(H₂O)₆](C₉H₆N₃O₃S)₂·4H₂O, contains half of a centrosymmetric cation, one 4-(3-pyridyl)pyrimidin-2-sulfonate anion and two solvent water molecules. Intermolecular O—H⋯O and O—H⋯N hydrogen bonds link the cations, anions and water molecules into a three-dimensional supramolecular structure. The crystal packing also exhibits intermolecular π–π interactions between the aromatic rings of the anions with a centroid–centroid distance of 3.604 (2) Å.

Related literature

For coordination complexes with pyridin-2-sulfonate ligands, see: Kimura et al. (1999 ▶); Lobana et al. (2004 ▶). For coordination complexes with 4-(pyridin-yl)pyrimidin-2-sulfonate, see: Zhu et al. (2007 ▶); Fang et al. (2009 ▶).

Experimental

Crystal data

[Mg(H₂O)₆](C₉H₆N₃O₃S)₂·4H₂O
M _r = 676.95
Monoclinic,
a = 6.9835 (2) Å
b = 13.3600 (3) Å
c = 16.2565 (4) Å
β = 98.7240 (10)°
V = 1499.18 (7) Å³
Z = 2
Mo Kα radiation
μ = 0.28 mm⁻¹
T = 291 K
0.30 × 0.15 × 0.12 mm

Data collection

Bruker SMART CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2000 ▶) T _min = 0.917, T _max = 0.966
14712 measured reflections
3438 independent reflections
2848 reflections with I > 2σ(I)
R _int = 0.025

Refinement

R[F ² > 2σ(F ²)] = 0.038
wR(F ²) = 0.102
S = 1.04
3438 reflections
236 parameters
7 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.23 e Å⁻³
Δρ_min = −0.40 e Å⁻³

Data collection: SMART (Bruker, 2000 ▶); cell refinement: SAINT (Bruker, 2000 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S160053680904344X/cv2632sup1.cif

e-65-m1436-sup1.cif^{(17.7KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S160053680904344X/cv2632Isup2.hkl

e-65-m1436-Isup2.hkl^{(168.6KB, hkl)}

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

Table 1. Hydrogen-bond geometry (Å, °).

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O4—H4A⋯O1ⁱ	0.83 (2)	1.94 (2)	2.7650 (19)	180 (3)
O4—H4B⋯O2	0.86 (2)	1.89 (2)	2.7475 (19)	176 (2)
O5—H5B⋯O3ⁱ	0.83 (2)	2.04 (2)	2.8705 (19)	177.0 (18)
O5—H5A⋯O8ⁱⁱ	0.86 (2)	1.91 (2)	2.755 (3)	167 (3)
O6—H6B⋯O3ⁱⁱⁱ	0.83 (2)	2.03 (3)	2.8601 (19)	178 (2)
O6—H6A⋯N3^iv	0.85 (3)	1.92 (3)	2.763 (2)	173 (2)
O7—H7B⋯O3^v	0.84 (3)	2.51 (3)	3.110 (2)	130 (3)
O7—H7B⋯N2^v	0.84 (3)	2.21 (3)	2.984 (2)	154 (3)
O7—H7A⋯O2	0.84 (3)	2.12 (3)	2.923 (2)	161 (3)
O8—H8B⋯O1^vi	0.85 (4)	2.43 (4)	3.064 (2)	132 (4)
O8—H8A⋯O7ⁱⁱⁱ	0.85 (3)	1.93 (3)	2.769 (3)	170 (3)

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

Acknowledgments

The authors are indebted to the Anhui Provincial Natural Science Research Project (KJ2009B240Z) and the National Natural Science Foundation of China (grant No. 20871039) for financial support.

supplementary crystallographic information

Comment

The rational design and synthesis of coordination complexes derived from heterocyclic sulfonate ligands have been of increasing interest recently in chemical research (Kimura et al., 1999; Lobana et al., 2004). In our previous work (Zhu et al., 2007; Fang et al., 2009), we have also studied transition metal coordination complexes with the heterocyclic sulfonate ligands, namely 4-(pyridin-2-yl)pyrimidin-2-sulfonate and 4-(pyridin-4-yl)pyrimidin-2-sulfonate. Herein, we report the magnesium(II) coordination complex with its analog, viz. 4-(pyridin-3-yl)pyrimidin-2-sulfonate.

The asymmetric unit of the title compound (Fig. 1) consists of a 4-(3-pyridyl)pyrimidin-2-sulfonate anion, one half of an [Mg(H₂O)₆]²⁺ cation and two free water molecules. The averaged Mg—O coordinating bond length is 2.0664 (13) Å. In the crystal structure, intermolecular O—H···O and O—H···N hydrogen bonds (Table 1) link cations, anions and crystalline water molecules into three-dimensinal network. The crystal packing exhibits also intermolecular π—π interactions between the aromatic rings of the anions with the centroid-centroid distance of 3.604 (2) Å.

Experimental

All solvents and chemicals were of analytical grade and were used without further purification. 4-(3-Pyridyl)pyrimidin-2-sulfonate (L) was prepared by similar procedure reported in the literature (Zhu et al., 2007; Fang et al., 2009). For the synthesis of title compoud, a solution of L (0.1 mmol), MgSO₄(0.1 mmol) in 30 ml methanol was stirred for 1 h at room temperature. After filtration, the mother liguid was stood for one week to give the colourless crystals suitable for X-ray diffraction annalysis.