catena-Poly[[bis­(3-benzoyl­pyridine-κN)zinc(II)]-di-μ-dicyanamido-κ4 N 1:N 5]

Fei Yu; Zhong-Shu Li; Bai-Wang Sun

doi:10.1107/S1600536808019880

. 2008 Jul 5;64(Pt 8):m993. doi: 10.1107/S1600536808019880

catena-Poly[[bis(3-benzoylpyridine-κN)zinc(II)]-di-μ-dicyanamido-κ⁴ N ¹:N ⁵]

Fei Yu ^a, Zhong-Shu Li ^a, Bai-Wang Sun ^a,^*

PMCID: PMC2961919 PMID: 21203088

Abstract

The title compound, [Zn(C₂N₃)₂(C₁₂H₉NO)₂]_n, is a polymeric zinc(II) complex with the metal ion located on an inversion centre. The Zn^II ion is six-coordinated by two N atoms of two 3-benzoylpyridine ligands and four N atoms from four dicyanamide ligands, forming a slightly distorted octahedral configuration. In the crystal structure, neighboring Zn atoms are linked together by double dicyanamide bridges to form a polymeric zinc(II) complex.

Related literature

For related literature, see: Armentano et al. (2006 ▶); Claramunt et al. (2000 ▶); Manson et al. (1998 ▶); Miller (2006 ▶).

Experimental

Crystal data

[Zn(C₂N₃)₂(C₁₂H₉NO)₂]
M _r = 563.89
Monoclinic,
a = 6.463 (4) Å
b = 7.490 (4) Å
c = 26.300 (15) Å
β = 98.399 (16)°
V = 1259.5 (13) Å³
Z = 2
Mo Kα radiation
μ = 1.02 mm⁻¹
T = 293 (2) K
0.07 × 0.04 × 0.03 mm

Data collection

Rigaku Scxmini 1K CCD area-detector diffractometer
Absorption correction: multi-scan (CrystalClear; Rigaku, 2005 ▶) T _min = 0.867, T _max = 1.000 (expected range = 0.841–0.970)
12079 measured reflections
2880 independent reflections
2342 reflections with I > 2σ(I)
R _int = 0.045

Refinement

R[F ² > 2σ(F ²)] = 0.050
wR(F ²) = 0.129
S = 1.09
2880 reflections
178 parameters
H-atom parameters constrained
Δρ_max = 0.60 e Å⁻³
Δρ_min = −0.56 e Å⁻³

Data collection: CrystalClear (Rigaku, 2005 ▶); cell refinement: CrystalClear; data reduction: CrystalClear ; 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/S1600536808019880/bq2086sup1.cif

e-64-0m993-sup1.cif^{(17.9KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808019880/bq2086Isup2.hkl

e-64-0m993-Isup2.hkl^{(141.4KB, hkl)}

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

Table 1. Selected geometric parameters (Å, °).

Zn1—N2	2.162 (3)
Zn1—N3	2.169 (2)
Zn1—N4	2.172 (3)

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N2—Zn1—N3	92.27 (11)
N2—Zn1—N4	90.79 (9)
N3—Zn1—N4	89.87 (9)

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supplementary crystallographic information

Comment

The dicyanamide ligand has frequently been used to bridge polynuclear transition metal complexes in the study of multidimensional molecule-based magnetic materials and other areas. Many such compounds have been reported (Manson et al., 1998; Claramunt et al., 2000; Armentano et al., 2006; Miller, 2006;). Here, we report the structure of the title Zn^II compound, (I). The structure of (I) is illustrated in Fig. 1, and bond distances and angles are given in Table 1. The Zn^II ion, which lies on the inversion centre, is in an octahedral geometry and is six-coordinated by six N atoms, from four dicyanamide ligands and two 3-benzoylpyridine ligands in a trans arrangement. The resulting coordination geometry is very close to that expected for an ideal octahedral complex. In the crystal structure, the Zn^II ions are bridged to form a one-dimensional chain by dicyanamide ligands, through single end-to-end coordination, the dicyanamide ligand acts as a bidentate bridging ligand by coordinating to adjacent Zn^II centres through its two terminal nitrile N atoms. No significant contacts are observed between adjacent chains in the crystal structure.

Experimental

All chemicals used (reagent grade) were commercially available. 3-benzoylpyridine (18.3 mg, 0.1 mmol) was added slowly with stirring in aqueous solution (5 ml) of Zn(CH₃COO)₂.2H₂O (21.9 mg, 0.1 mmol) and then sodium dicyanamide (17.8 mg, 0.2 mmol) in aqueous solution (5 ml) was added slowly. The resulting colorless solution was continuously stirred for about 30 min at room temperature and then filtered. The filtrate was slowly evaporated at room temperature over several days, and colorless needles crystals suitable for X-ray analysis were obtained.