Startseite Crystal structure of dibromido-bis[μ-1-[(2-methyl-1H-benzoimidazol-1-yl)methyl]-1H-benzotriazole-κN]mercury(II), C30H26Br2HgN10
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Crystal structure of dibromido-bis[μ-1-[(2-methyl-1H-benzoimidazol-1-yl)methyl]-1H-benzotriazole-κN]mercury(II), C30H26Br2HgN10

  • Xia Wang , Jing-Jing Shi , Shu-Ling Zhang und Han-Bing Li EMAIL logo
Veröffentlicht/Copyright: 27. September 2016

Abstract

C30H26Br2HgN10, monoclinic, C2/c (no. 15), a = 15.5262(6) Å, b = 13.2099(7) Å, c = 14.8370(5) Å, β = 95.688(3)°, V = 3028.1(2) Å3, Z = 4, Rgt(F) = 0.0329, wRref(F2) = 0.0561, T = 291(2) K.

CCDC no.:: 1502533

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

Table 1

Data collection and handling.

Crystal:Colourless prism Size 0.24 × 0.20 × 0.18 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:77.6 cm−1
Diffractometer, scan mode:Xcalibur, ω
2θmax, completeness:52.8°, >99%
N(hkl)measured, N(hkl)unique, Rint:6535, 3094, 0.030
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 2484
N(param)refined:196
Programs:SHELX [7], CrysAlisPRO [8]
Table 2

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

AtomxyzUiso*/Ueq
Hg10.50000.599472(19)0.25000.04310(9)
Br10.36446(3)0.70037(4)0.19862(3)0.05419(15)
N10.4768(2)0.4742(2)0.3552(2)0.0370(8)
N20.4136(2)0.3489(3)0.4222(2)0.0380(8)
N30.3603(2)0.1793(3)0.4198(2)0.0432(9)
N40.3569(3)0.1045(3)0.4837(2)0.0603(12)
N50.3669(3)0.0177(3)0.4452(3)0.0709(13)
C10.6278(3)0.4418(4)0.4304(3)0.0445(11)
H10.65480.49430.40250.053*
C20.6741(3)0.3781(4)0.4919(3)0.0510(13)
H20.73340.38760.50510.061*
C30.6330(3)0.3002(4)0.5342(3)0.0541(13)
H30.66580.25940.57570.065*
C40.5463(3)0.2812(4)0.5171(3)0.0469(12)
H40.51940.22890.54550.056*
C50.5004(3)0.3449(3)0.4545(2)0.0336(10)
C60.5397(3)0.4242(3)0.4121(2)0.0344(10)
C70.4032(3)0.4276(3)0.3626(3)0.0373(10)
C80.3178(3)0.4549(4)0.3160(3)0.0588(13)
H8A0.32090.52100.28960.088*
H8B0.27540.45500.35890.088*
H8C0.30170.40630.26920.088*
C90.3460(3)0.2817(3)0.4475(3)0.0461(11)
H9A0.34440.28380.51260.055*
H9B0.29050.30490.41940.055*
C100.3718(3)0.1377(4)0.3378(3)0.0426(11)
C110.3766(3)0.0344(4)0.3554(3)0.0514(12)
C120.3886(3)−0.0349(5)0.2871(4)0.0710(16)
H120.3915−0.10410.29850.085*
C130.3960(3)0.0027(6)0.2030(4)0.0768(18)
H130.4053−0.04150.15610.092*
C140.3898(3)0.1063(6)0.1855(3)0.0729(18)
H140.39400.12890.12670.088*
C150.3778(3)0.1770(4)0.2520(3)0.0560(14)
H150.37400.24600.24000.067*

Source of material

The ligand 1-[(2-methyl-1H-benzoimidazol-1-yl)methyl]-1H-benzotriazole (0.04 mmol, 0.0105 g) in methanol (6 mL) was added dropwise to a methanol solution (6 mL) of HgBr2 (0.04 mmol, 0.0144 g) in methanol. The resulting solution was allowed to stand at room temperature. After 2 weeks colourless crystals were obtained.

Experimental details

H atoms were generated geometrically and refined as riding atoms with C—H = 0.93 Å and Uiso(H) = 1.2 times Ueq(C) for aromatic H atoms, with C—H = 0.97 Å and Uiso(H) = 1.2 times, Ueq(C) for methylene H atoms, and with C—H = 0.96 Å and Uiso(H) = 1.5 times Ueq(C) for methyl H atoms.

Discussion

Imidazole and benzotriazole derivatives have been widely used in the syntheses of complexes since they can act as polydentate ligands and function as bridging ligands [1, 2]. Many symmetric imidazole and benzotriazole ligands have been applied [3, 4]. However, studies involving asymmetric imidazole and benzotriazole ligands are rather rare [5, 6]. We are engaged in the synthesis of unsymmetrical N-heterocyclic ligands and synthesized compound 1-[(2-methyl-1H-benzoimidazol-1-yl)methyl]-1H-benzotriazole. As part of this study, we selected this compound as ligand and generate a new complex [Hg(C15H13N5)2Br2], which is reported here.

The title compound is a mononuclear complex, located on a two-fold axis in the space group C2/c. As is shown in the figure, the Hg(II) atom is four-coordinated by two N atoms from two 1-[(2-methyl-1H-benzoimidazol-1-yl)methyl]-1H-benzotriazole ligands and two Br atoms in a distorted tetrahedral coordination environment (with Hg—N bond length of 2.327(3) Å, with Hg—Br bond length of 2.5433(5) Å). The bond angles around Hg(II) ion range from 89.35 to 116.79°. In addition, the benzoimidazol rings in adjacent molecules are almost parallel. The average interplanar distance is 3.54 Å, which suggests π–π interactions.

Acknowledgements:

This work was financially supported by the Science and Technology Department of Henan Province (No. 142102210458) and Foundation for University Key Teacher by the Henan Province (2013GGJS-090), and the Program for Innovative Research Team (in Science and Technology) in Henan College of Chinese Medicine (STITHCCM-2013XCXRC02). The authors thank the Professor Hong-Wei Hou and Yu Zhu of Zhengzhou University for their help.

References

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Received: 2016-5-18
Accepted: 2016-9-5
Published Online: 2016-9-27
Published in Print: 2017-1-1

©2016 Xia Wang et al., published by De Gruyter.

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

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  2. Editorial
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