catena-Poly[[bromidocopper(I)]-μ-η2,σ1-3-(2-allyl-2H-tetra­zol-5-yl)pyridine]

Wei Wang

doi:10.1107/S1600536808010313

. 2008 May 3;64(Pt 6):m759. doi: 10.1107/S1600536808010313

catena-Poly[[bromidocopper(I)]-μ-η²,σ¹-3-(2-allyl-2H-tetrazol-5-yl)pyridine]

Wei Wang ^a,^*

PMCID: PMC2961586 PMID: 21202452

Abstract

The title compound, [CuBr(C₉H₉N₅)]_n, has been prepared by the solvothermal treatment of CuBr with 3-(2-allyl-2H-tetrazol-5-yl)pyridine. It is a new homometallic Cu^I olefin coordination polymer in which the Cu^I atoms are linked by the 3-(2-allyl-2H-tetrazol-5-yl)pyridine ligands and bonded to one terminal Br atom each. The organic ligand acts as a bidentate ligand connecting two neighboring Cu centers through the N atom of the pyridine ring and the double bond of the allyl group. A three-dimensional structure is formed through weak Cu—Br [3.1579 (8) Å], C—H⋯Br and C—H⋯N interactions.

Related literature

For the solvothermal synthesis and related structures, see: Ye et al. (2005 ▶, 2007 ▶).

Experimental

Crystal data

[CuBr(C₉H₉N₅)]
M _r = 330.66
Triclinic,
a = 7.4464 (15) Å
b = 7.7982 (16) Å
c = 9.940 (2) Å
α = 80.15 (3)°
β = 76.02 (3)°
γ = 85.13 (3)°
V = 551.3 (2) Å³
Z = 2
Mo Kα radiation
μ = 5.58 mm⁻¹
T = 293 (2) K
0.2 × 0.15 × 0.1 mm

Data collection

Rigaku Mercury2 diffractometer
Absorption correction: multi-scan (CrystalClear; Rigaku, 2005 ▶) T _min = 0.720, T _max = 1 (expected range = 0.412–0.572)
5748 measured reflections
2522 independent reflections
2173 reflections with I > 2σ(I)
R _int = 0.032

Refinement

R[F ² > 2σ(F ²)] = 0.032
wR(F ²) = 0.072
S = 1.11
2522 reflections
145 parameters
H-atom parameters constrained
Δρ_max = 0.41 e Å⁻³
Δρ_min = −0.44 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: PLATON (Spek, 2003 ▶) and CAMERON (Pearce et al., 2000 ▶); software used to prepare material for publication: SHELXL97.

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808010313/dn2335sup1.cif

e-64-0m759-sup1.cif^{(15KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808010313/dn2335Isup2.hkl

e-64-0m759-Isup2.hkl^{(123.9KB, 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
C1—H1⋯Br1ⁱ	0.93	2.90	3.776 (3)	157
C2—H2⋯N5ⁱ	0.93	2.62	3.415 (4)	144
C9—H9A⋯N3ⁱⁱ	0.97	2.88	3.800 (4)	159

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

Acknowledgments

This work was supported by a Start-up Grant from SEU to Professor Ren-Gen Xiong.

supplementary crystallographic information

Comment

Under hydrothermal or solvothermal conditions, some interesting reactions can be carried out leading to new compounds, while It is worth noting that these products could not be synthesized using conventional solution techniques. In sealed tube, unstable copper (I) salt can exist under vacuums, and then interesting copper (I) coordination compound can be obtained (Ye et al., 2005, 2007). The title compound is obtained through solvothermal treatment of CuBr and 3-(2-allyl-2H-tetrazol -5-yl) pyridine in methanol solvent at 75°C, colorless block crystals suitable for X-ray diffractions have been isolated. have been isolated.

The copper(I) is coordinated to two olefinic ligands and one terminal Br atom in a trigonal environment (Fig 1). The olefin ligands link the neighbouring Cu centers to form an homometallic Cu^I coordination polymer developping along the c axis. The 3-(2-allyl-2H-tetrazol-5-yl) pyridine ligands coordinate to copper (I) centers through N atom of pyridine ring and double bond of allyl group. Unfortunately, the N atoms of tetrazole ring fail to coordinate to Cu(I).

Finally, weak Cu—Br, C-H···Br and C—H···N (Table 1) interactions result in the formation of a three-dimensionnal structure (Fig. 2)

Experimental

A mixture of 3-(2-allyl-2H-tetrazol-5-yl) pyridine(20 mg, 0.2 mmol), CuBr (17.9 mg,0.2 mmol), and methanol (2 mL) sealed in a glass tube were maintained at 75 °C. Crystals suitable for X-ray analysis were obtained after 5 days