Startseite The crystal structure of (4-(1H-1,2,4-triazol-1-yl)benzoato-κN)-[4-(1H-1,2,4-triazol-1-yl)benzoic acid-κN]silver(I), C18H13AgN6O4
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The crystal structure of (4-(1H-1,2,4-triazol-1-yl)benzoato-κN)-[4-(1H-1,2,4-triazol-1-yl)benzoic acid-κN]silver(I), C18H13AgN6O4

  • Chuan-Bo Sun , Ai-Yun Fu EMAIL logo , Jun-Cheng Jin und Yue-Hua Zhang
Veröffentlicht/Copyright: 10. Mai 2017

Abstract

C18H13AgN6O4, monoclinic, C2/c (no. 15), a = 12.9022(12) Å, b = 8.9088(8) Å, c = 15.3383(14) Å, β = 106.810(3)°, V = 1687.7(3) Å3, Z = 4, Rgt(F) = 0.0247, wRref(F2) = 0.0600, T = 296(2) K.

CCDC no.:: 1545093

The asymmetric unit of the title 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 needle
Size:0.40 × 0.38 × 0.37 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:12.4 cm−1
Diffractometer, scan mode:Bruker SMART, φ and ω
2θmax, completeness:50°, >99%
N(hkl)measured, N(hkl)unique, Rint:4780, 1502, 0.019
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 1411
N(param)refined:132
Programs:Bruker [1], SHELX [2, 3]
Table 2

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

AtomxyzUiso*/Ueq
Ag10.00000.38370(4)1.25000.04350(13)
N10.08909(15)0.3523(2)1.00326(13)0.0247(4)
N20.00200(17)0.2569(3)0.98336(14)0.0362(5)
N30.02957(16)0.3574(2)1.12215(13)0.0294(5)
O10.43393(13)0.4916(2)0.79315(11)0.0347(4)
H1a0.46910.49470.75640.052*
O20.31279(15)0.3765(2)0.67872(12)0.0405(5)
C10.34256(18)0.4275(3)0.75632(15)0.0258(5)
C20.27129(18)0.4156(3)0.81891(15)0.0241(5)
C30.18038(19)0.3241(3)0.79601(15)0.0281(5)
H30.15990.27680.73960.034*
C40.11938(18)0.3023(3)0.85660(15)0.0279(5)
H40.05890.24010.84130.033*
C50.15039(17)0.3749(2)0.93982(15)0.0233(5)
C60.2392(2)0.4691(3)0.96308(16)0.0327(6)
H60.25820.51931.01860.039*
C70.2997(2)0.4877(3)0.90217(16)0.0321(6)
H70.36030.54960.91770.039*
C8−0.0297(2)0.2643(3)1.05683(17)0.0353(6)
H8−0.08840.20991.06370.042*
C90.10400(18)0.4105(3)1.08599(15)0.0256(5)
H90.15830.47811.11410.031*
  1. aOccupancy: 0.50.

Source of material

AgNO3 (8.5 mg, 0.05 mmol), 4-(1H-1,2,4-triazol-1-yl)benzoic acid (18.9 mg, 0.1 mmol), NaOH (4.0 mg, 0.1 mmol) and water (20 mL) were placed in a Teflon-lined stainless steel autoclave (20 mL). The autoclave was heated at 383 K for 2 days. After cooling to room temperature, large colorless rod-shaped crystals of the title complex were obtained.

Experimental details

The carbon-bound hydrogen atoms were placed in calculated positions (C—Hphenyl = 0.93 Å), and were included with Uiso(H) = 1.2Ueq(C). The water H-atoms were placed in calculated positions (O—H = 0.85 Å), and were included with Uiso(H) = 1.2Ueq(O).

Discussion

In recent years, considerable attention has been devoted to the design of new bioactive complexes [4], [5], [6] due to a worldwide movement toward the development of new efficient antimicrobial, disinfecting, and sanitizing agents. In particular, different silver(I) compounds constitute a family of potent antimicrobial ion-releasing materials [7], [8], [9].

The crystal structure analysis reveals that the asymmetric unit consists of one half of a Ag(I) and one 4-(1H-1,2,4-triazol-1-yl)benzoate, which appeared to be protonated at the carboxylate group for every second (crystallographically related) ligand (cf. the figure). The Ag(I) metal has a linear coordination geometry, being coordinated by the molecular and anionic ligands. The H(1) localize at special positions with site occupancy of 0.5, indicating 4-(H-1,2,4-triazol-1-yl)benzoate and 4-(1H-1,2,4-triazol-1-yl)benzoic acid molecule become interchangeable from each other. The angle sandwiched of 77.68° is measured between the ligands’ planes. The Ag-N distance is 2.1164(19) Å and the N—Ag—N angle is 167.27(11)°. In addition, the hydrogen bonds of O—H⋯O [O(1)⋯O(1A), 2.442 Å] extend the complexes into one-dimensional supramolecular array.

Acknowledgement

We are grateful for financial support from the NSF of China (21401143, 21671031); Anhui Province Training Programs of Innovation and Entrepreneurship for Undergraduates (AH201510376003).

References

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Received: 2017-1-14
Accepted: 2017-4-21
Published Online: 2017-5-10
Published in Print: 2017-7-26

©2017 Chuan-Bo Sun et al., published by De Gruyter.

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

Artikel in diesem Heft

  1. Cover and Frontmatter
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  26. Crystal structure of 3-(4-methoxyphenyl)-1-(4-methylphenyl)prop-2-en-1-one, C17H16O2
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  61. Corrigendum
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