catena-Poly[[[2-(pyridin-2-yldisulfan­yl)pyridine-κ2 N,S]copper(I)]-μ1,5-dicyanamido]

Shixi Wu; Wei Jiang; Fengsheng Li; Li Liu

doi:10.1107/S1600536811002728

. 2011 Jan 29;67(Pt 2):m285. doi: 10.1107/S1600536811002728

catena-Poly[[[2-(pyridin-2-yldisulfanyl)pyridine-κ² N,S]copper(I)]-μ_1,5-dicyanamido]

Shixi Wu ^a, Wei Jiang ^a, Fengsheng Li ^a,^*, Li Liu ^a

PMCID: PMC3051621 PMID: 21522929

Abstract

In the title compound, [Cu(C₂N₃)(C₁₀H₈N₂S₂)]_n, the Cu^I atoms are connected by bridging dicyanamide ligands, forming chains parallel to [100]. Each Cu^I atom displays a tetrahedral coordination environment, formed by one S atom and three N atoms from one 2-(pyridin-2-yldisulfanyl)pyridine and two dicyanamide ligands. The crystal structure is stabilized by C—H⋯N hydrogen bonds, forming a three-dimensional network.

Related literature

For potential applications of metal-organic frameworks, see: Eddaoudi et al. (2001 ▶). For metal-organic frameworks constructed from flexible ligands, see: Xu et al. (2009 ▶). For related structures, see: Mal et al. (2006 ▶); Schlueter et al. (2007 ▶); Sen et al. (2007 ▶).

Experimental

Crystal data

[Cu(C₂N₃)(C₁₀H₈N₂S₂)]
M _r = 349.92
Triclinic,
a = 7.6294 (15) Å
b = 9.5964 (19) Å
c = 10.202 (2) Å
α = 84.19 (3)°
β = 80.63 (3)°
γ = 70.93 (3)°
V = 695.6 (2) Å³
Z = 2
Mo Kα radiation
μ = 1.87 mm⁻¹
T = 293 K
0.20 × 0.16 × 0.12 mm

Data collection

Bruker APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.893, T _max = 1.000
6615 measured reflections
2669 independent reflections
2301 reflections with I > 2σ(I)
R _int = 0.018

Refinement

R[F ² > 2σ(F ²)] = 0.028
wR(F ²) = 0.081
S = 1.07
2669 reflections
181 parameters
H-atom parameters constrained
Δρ_max = 0.39 e Å⁻³
Δρ_min = −0.29 e Å⁻³

Data collection: APEX2 (Bruker, 2007 ▶); cell refinement: SAINT (Bruker, 2007 ▶); 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/S1600536811002728/zq2085sup1.cif

e-67-0m285-sup1.cif^{(15.9KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536811002728/zq2085Isup2.hkl

e-67-0m285-Isup2.hkl^{(131.1KB, 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
C9—H9⋯N3ⁱ	0.93	2.53	3.453 (3)	171

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Symmetry code: (i) Inline graphic .

Acknowledgments

The authors are grateful for the financial support of the National Natural Science Foundation of China (Nos. 50602024, 50972060) and NUST Research Funding (No. 2010ZDJH06).

supplementary crystallographic information

Comment

Metal-organic compounds have attracted much attention because of their diverse structures (Eddaoudi et al., 2001). Flexible ligands can play different roles in constructing metal-organic frameworks (Xu et al., 2009). The title compound, {C₁₂H₈CuN₅S₂}_n, is constructed by two kinds of flexible ligands: briding dicyanamide ligands and chelate 2-(pyridin-2-yldisulfanyl)pyridine ligands. In this paper, the crystal structure of the title compound is presented. As illustrated in Fig. 1, the Cu atoms are connected by briding dicyanamide ligands, forming a serrate chain. Each Cu atom displays a tetrahedral coordination environment, formed by one S atom and three N atoms from one 2-(pyridin-2-yldisulfanyl)pyridine and two dicyanamide ligands, where the Cu—S and average Cu—N bonds are 2.472 (1) and 1.969 Å, respectively. The crystal structure is stabilized by C—H···N hydrogen bonds [H9···N3ⁱⁱⁱ = 2.53 Å, C9···N3ⁱⁱⁱ = 3.453 (3) Å, and C9—H9···N3ⁱⁱⁱ = 171°] between the central N atom of the dicyanamide and one H atom of a pyridine ring, forming a three-dimensional network [symmetry code: (iii) x + 1, y - 1, z].

Experimental

CuN(CN)₂ (0.4 mmol) and NaN(CN)₂ (1.2 mmol) were added into 2 ml DMF with thorough stir for 6 minutes. After filtration, the colorless filtrate was carefully laid on the surface with the solution of bis(2-pyridyl)disulfide (0.5 mmol) in 5 ml i-PrOH. Colorless crystals were obtained after 3 weeks.