Tetra­aqua­bis{2-[4-(3-pyrid­yl)pyrimidin-2-ylsulfan­yl]acetato}manganese(II) dihydrate

Hai-Bin Zhu; Gang Xu; Yan-Yan Sun

doi:10.1107/S1600536809033078

. 2009 Aug 22;65(Pt 9):m1126. doi: 10.1107/S1600536809033078

Tetraaquabis{2-[4-(3-pyridyl)pyrimidin-2-ylsulfanyl]acetato}manganese(II) dihydrate

Hai-Bin Zhu ^a,^*, Gang Xu ^a, Yan-Yan Sun ^a

PMCID: PMC2970048 PMID: 21577466

Abstract

In the title compound, [Mn(C₁₁H₈N₃O₂S)₂(H₂O)₄]·2H₂O, the Mn^II ion lies on an inversion centre and is coordinated by four water molecules in equatorial positions and two N atoms from two 2-[4-(3-pyridyl)pyrimidin-2-ylsulfanyl]acetate ligands in the axial positions. The water molecules, including the uncoordinated water molecules, and the acetate O atoms are involved in O—H⋯O and O—H⋯N hydrogen-bonding interactions, which link the components into layers parallel to the a (b + c) plane.

Related literature

For hydro(solvo)thermal reactions between (heterocyclicthio)acetic acid and metal ions, see: Zhu et al. (2009 ▶); Hao et al. (2008 ▶); He et al. (2007 ▶). For a Cu(II) coordination compound with 4-(pyridin-4-yl)pyrimidine-2-sulfonate, see Li et al. (2009 ▶).

Experimental

Crystal data

[Mn(C₁₁H₈N₃O₂S)₂(H₂O)₄]·2H₂O
M _r = 655.58
Triclinic,
a = 8.459 (3) Å
b = 9.240 (3) Å
c = 9.360 (4) Å
α = 87.396 (6)°
β = 75.862 (5)°
γ = 79.872 (5)°
V = 698.4 (4) Å³
Z = 1
Mo Kα radiation
μ = 0.69 mm⁻¹
T = 298 K
0.14 × 0.12 × 0.10 mm

Data collection

Bruker APEXII CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2001 ▶) T _min = 0.884, T _max = 0.920
4518 measured reflections
3181 independent reflections
2443 reflections with I > 2σ(I)
R _int = 0.031

Refinement

R[F ² > 2σ(F ²)] = 0.037
wR(F ²) = 0.094
S = 0.98
3181 reflections
187 parameters
H-atom parameters constrained
Δρ_max = 0.49 e Å⁻³
Δρ_min = −0.55 e Å⁻³

Data collection: APEX2 (Bruker, 2007 ▶); cell refinement: SAINT-Plus (Bruker, 2007 ▶); data reduction: SAINT-Plus; 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 Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809033078/cv2600sup1.cif

e-65-m1126-sup1.cif^{(18.6KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809033078/cv2600Isup2.hkl

e-65-m1126-Isup2.hkl^{(156.1KB, 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
O2—H1⋯O3ⁱ	0.85	1.82	2.655 (2)	168
O1—H2⋯O4	0.85	1.88	2.709 (2)	165
O2—H3⋯O4	0.85	1.97	2.743 (2)	150
O1—H4⋯O5ⁱⁱ	0.85	1.81	2.642 (3)	167
O5—H5⋯N1ⁱⁱⁱ	0.85	2.09	2.888 (3)	155
O5—H6⋯O3	0.85	2.01	2.775 (3)	149

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

Acknowledgments

The authors acknowledge financial support from the China Postdoctoral Research Fund (grant No. 20070411010) and the Young Teachers’ Starting Fund of Southeast University.

supplementary crystallographic information

Comment

Hydro(solvo)thermal reactions of (heterocyclicthio)acetic acid with both transition metal ions and lanthanide ions have been investigated in several reports (Zhu et al., 2009; Hao et al., 2008; He et al., 2007), wherein in situ C—S cleavage has taken place under these situations. Herein, we report a manganese (II) coordination complex with a newly synthesized (heterocyclicthio)acetic acid, namely 2-(4-(pyridine-3-yl)pyrimidin-2-ylthio)acetic acid.

As shown in Fig. 1, the coordination arrangement around Mn(II) center is similar to our previously reported Cu(II) compound with the ligand of 4-(pyridin-4-yl)pyrimidine-2-sulfonate (Li et al., 2009). The Mn(II) center also adopts an octahedral coordination geometry completed by four water O atoms in equatorial positions and two N atoms in apical positions. In the title complex, the Mn^II atom sits on an inversion centre with the asymmetric unit containing half of the complex and one free water molecule. The Mn—O bond lengths vary from 2.189 (2) to 2.192 (2) Å and the Mn—N bond distance is 2.276 (2) Å. Intra- and intermolecular hydrogen bonding interactions, such as O—H···O and O—H···N are observed in the crystal structure (Table 1).

Experimental

The mixture of Mn(OAc)₂ (0.1 mmol), 2-(4-(pyridine-3-yl)pyrimidin-2-ylthio)acetic acid (0.2 mmol) and NaOH (0.2 mmol) in 6 ml of H₂O was stirred for 20 min at room temperature. After filtration, the mother liquid was stood for one week to give the colorless crystals suitable for X-raydiffraction analysis.