Home Crystal structure of bis(μ2-azido-κ2N:N)-dichlorido-bis(μ2-2-(pyridin-2-yl)ethan-1-ol-κ2O,N)dicopper(II), C14H18Cl2Cu2N8O2
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Crystal structure of bis(μ2-azido-κ2N:N)-dichlorido-bis(μ2-2-(pyridin-2-yl)ethan-1-ol-κ2O,N)dicopper(II), C14H18Cl2Cu2N8O2

  • Wang Xin , Lv Huichao , Yang Liguo EMAIL logo and Dai Yuqiang
Published/Copyright: March 28, 2017

Abstract

C14H18Cl2Cu2N8O2, monoclinic, P21/n (no. 14), a = 6.0166(6) Å, b = 15.2792(14) Å, c = 11.5833(12) Å, β = 100.295(1)°, V = 1047.70(18) Å3, Z = 2, Rgt(F) = 0.0412, wRref(F2) = 0.0884, T = 298 K.

CCDC no.:: 1535400

The crystal structure is shown in the figure. Tables 1 and 2 contain details on crystal structure and measurement conditions and a list of the atoms including atomic coordinates and displacement parameters.

Table 1

Data collection and handling.

Crystal:Black block
Size:0.41 × 0.18 × 0.15 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:23.1 cm−1
Diffractometer, scan mode:Bruker SMART, φ and ω
2θmax, completeness:50°, >99%
N(hkl)measured, N(hkl)unique, Rint:5221, 1842, 0.048
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 1331
N(param)refined:127
Programs:SHELX [7]
Table 2

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2).

AtomxyzUiso*/Ueq
Cu10.16199(8)0.57579(3)0.55314(4)0.03893(19)
Cl10.39785(18)0.65706(8)0.46611(9)0.0557(3)
N10.3382(5)0.5948(2)0.7136(3)0.0383(8)
N20.0393(6)0.4569(2)0.5965(3)0.0475(9)
N30.0188(6)0.4345(2)0.6939(3)0.0420(8)
N40.0068(7)0.4122(3)0.7863(3)0.0672(12)
O1−0.1133(5)0.6531(2)0.6040(3)0.0709(10)
H1−0.25670.64690.55890.085*
C1−0.0892(8)0.7109(3)0.6993(4)0.0590(13)
H1A−0.13600.68270.76600.071*
H1B−0.18280.76220.67880.071*
C20.1546(7)0.7369(3)0.7294(4)0.0520(12)
H2A0.16770.78510.78450.062*
H2B0.20200.75810.65870.062*
C30.3144(7)0.6658(3)0.7813(3)0.0410(10)
C40.4407(8)0.6732(3)0.8924(4)0.0583(13)
H40.42420.72230.93760.070*
C50.5904(9)0.6089(4)0.9369(4)0.0685(15)
H50.67430.61391.01220.082*
C60.6156(8)0.5372(3)0.8694(4)0.0598(13)
H60.71730.49300.89720.072*
C70.4857(7)0.5328(3)0.7592(4)0.0483(11)
H70.50110.48380.71360.058*

Source of material

All reagents and solvents were of high purity grade and were purchased from commercial sources and received unless noted otherwise. To a methanolic solution (30 mL) of 2-(pyridin-2-yl)ethan-1-ol (224 mg, 2.04 mmol) and copper(II) acetate monohydrate (75 mg, 1.02 mmol), a methanol solution (10 mL) of NaN3 (99.12 mg, 1.02 mmol) was added. The reaction mixture was allowed to stand at room temperature for several days. Dark green crystals formed, and were filtered off and dried in vacuo. Yield 80%, Combustion Anal. Calc. for Cu2C14H18Cl2N8O2: C, 31.83; H, 3.43; N, 21.21. Found: C, 31.78; H, 3.40; N, 21.19.

Experimental details

Hydrogen atoms were placed in calculated positions and were included in the refinement in the riding model approximation, with Uiso(H) set to 1.2Ueq(C).

Discussion

A large number of dinuclear copper complexes have been reported recently as model compounds for the active sites of biological metalloenzymes. The best-investigated binuclear proteins are hemocyanin, and tyrosinase or catechol oxidase.

As shown in figure, the Cu atom exhibits a tetrahedral coordination geometry with basal positions occupied by one nitrogen atom of azido group, one oxygen atom and one nitrogen atom of the organic ligand, and one chlorine atom. The three nitrogen atoms of the azido group are as expected nearly collinear (177.6°). The azido group makes an average angle Cu—N—N of 126.49°. The bond lengths between the Cu atom and the nitrogen atoms of the two coordinating azido groups are 1.993(3) and 2.056(3) Å, respectively. The bonding distance between the Cu atom and the nitrogen atom of the pyridinyl nitrogen atom is 1.990(3) Å. The Cu—O bond length is 2.199(3) Å. The Cu—Cl bond length is 2.4545(11) Å.

Each hydroxy group of the neutral organic ligand forms a OH ⋯Cl hydrogen bond to an adjacent complex, creating a chain structure along the [100] direction.

Acknowledgement

This work was supported by the Key Scientific Research Projects of Colleges and Universities, Henan Province (Nos. 16A150001, 16A430012).

References

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Received: 2016-10-27
Accepted: 2017-3-1
Published Online: 2017-3-28
Published in Print: 2017-5-24

©2017 Wang Xin et al., published by De Gruyter, Berlin/Boston

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.

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