catena-Poly[[[aqua­(pyrazino­[2,3-f][1,10]phenanthroline-κ2 N 8,N 9)zinc(II)]-μ-penta­nedioato] monohydrate]

Wei Fang

doi:10.1107/S1600536810042340

. 2010 Nov 6;66(Pt 12):m1522–m1523. doi: 10.1107/S1600536810042340

catena-Poly[[[aqua(pyrazino[2,3-f][1,10]phenanthroline-κ² N ⁸,N ⁹)zinc(II)]-μ-pentanedioato] monohydrate]

Wei Fang ^a,^*

PMCID: PMC3011601 PMID: 21589224

Abstract

In the title compound, {[Zn(C₅H₆O₄)(C₁₄H₈N₄)(H₂O)]·H₂O}_n, the Zn²⁺ ion is coordinated by an N,N′-bidentate pyrazino[2,3-f][1,10]phenanthroline (pyphen) ligand, a water molecule and a monodentate glutarate (glu) dianion. A symmetry-generated O:O′-bidentate glu dianion completes a distorted cis-ZnN₂O₄ octahedral coordination geometry for the metal ion. The bridging glu species generates [110] polymeric chains in the crystal. O—H⋯O hydrogen bonds involving both the coordinated and uncoordinated water molecules help to consolidate the structure and neighbouring pyphen units interact through numerous aromatic π–π interactions [minimum centroid–centroid separation = 3.654 (3) Å], resulting in a two-dimensional network.

Related literature

For the synthesis of the ligand, see: Dickeson & Summers (1970 ▶). For related structures, see: Fang-Wei & Mei (2007 ▶); Li et al. (2006 ▶).

Experimental

Crystal data

[Zn(C₅H₆O₄)(C₁₄H₈N₄)(H₂O)]·H₂O
M _r = 463.74
Triclinic,
a = 6.397 (3) Å
b = 9.384 (5) Å
c = 16.409 (8) Å
α = 98.067 (5)°
β = 100.859 (5)°
γ = 101.274 (5)°
V = 932.5 (8) Å³
Z = 2
Mo Kα radiation
μ = 1.37 mm⁻¹
T = 292 K
0.78 × 0.52 × 0.36 mm

Data collection

Bruker SMART CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2002 ▶) T _min = 0.432, T _max = 0.611
8019 measured reflections
3702 independent reflections
2929 reflections with I > 2σ(I)
R _int = 0.062

Refinement

R[F ² > 2σ(F ²)] = 0.040
wR(F ²) = 0.100
S = 0.98
3702 reflections
283 parameters
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.86 e Å⁻³
Δρ_min = −0.59 e Å⁻³

Data collection: SMART (Bruker, 2002 ▶); cell refinement: SAINT (Bruker, 2002 ▶); 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 Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810042340/hb5645sup1.cif

e-66-m1522-sup1.cif^{(23.3KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810042340/hb5645Isup2.hkl

e-66-m1522-Isup2.hkl^{(179.2KB, hkl)}

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

Table 1. Selected bond lengths (Å).

Zn1—O2	1.987 (2)
Zn1—N1	2.120 (3)
Zn1—O5	2.137 (2)
Zn1—O4ⁱ	2.154 (2)
Zn1—N2	2.188 (2)
Zn1—O3ⁱ	2.347 (2)

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Symmetry code: (i) Inline graphic .

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

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O5—H5A⋯OW1ⁱⁱ	0.82	1.89	2.702 (3)	173
O5—H5B⋯O4ⁱⁱⁱ	1.00 (4)	1.91 (4)	2.856 (3)	157 (3)
OW1—HWA1⋯O4^iv	0.85 (4)	2.03 (4)	2.840 (4)	161 (3)
OW1—HWBA⋯O2	0.79 (4)	1.95 (4)	2.733 (4)	170 (4)

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

Acknowledgments

The author thanks Baicheng Normal University for supporting this work.

supplementary crystallographic information

Comment

The 1,10-phenanthroline (phen) ligand and its derivatives are important ligands with numerous uses in the construction of metal-organic complexes.Supramolecular architectures baswd on the phen derivative pyrazino[2,3-f][1,10]phenanthroline(PyPhen) molecule have considerably less attention (Li et al.,2006) A s part of our ongoing studies in this area (Fang-Wei & Mei, 2007). We selected glutaric acid (C₅H₆O₄^2-) to act as a metal-metal linker in its deprotonated form and L as a secondary ligand, generating the title compound, [Zn(C₁₄H₈N₄)(C₅H₆O₄)(H₂O).H₂O], a new coordinationg polymer, which is reported here. In compound (I), the Zn^II atom of unit is surrounded by two N atoms derived from the bidentate PyPhen ligand, three O atoms from two glutaric acid dianions (one monodentate, one bidentate) and one water molecule (Figure 1, Table 1) a distorted octahedral cis-ZnN₂O₄arrangement is formed. Neighboring Zn^II atoms are bridged by the centrosymmetric glutaric acid ligands forming a one-dimensional chain structure (Fig.2). In the crystal structure, adjacent chains are connected through π-π interactions between PyPhen and PyPhen ligands with a minimum centroid -centroid stacking distance of 3.372 Å. O—H···O hydrogen bonds involving the water molecules and carboxylate O atom acceptors (Table 2) complete the structure.

Experimental

The pyphen ligand was synthesized according to the literature method of Dickeson & Summers (1970). A mixture of ZnCl₂ (0.3 mmol), pyphen (0.1 mmol) and glutaric acid (0.3 mmol) in distilled water (30 ml) was stirred thoroughly for 1 h at ambient temperature. The pH was adjusted to 7.5 with aqueous NaOH solution. The suspension was then sealed in a Teflon-lined stainless steel reaction vessel (40 ml). The reaction was performed under autogeneous pressure and static conditions in an oven at 443 K for 4.5 d. The vessel was then cooled slowly inside the oven to 298 K at a rate of 5 K h^-1 before opening: amaranth (red) blocks of (I) were collected.