Home Physical Sciences Crystal structure of poly[(μ3-2-(pyrazin-2-ylthio)acetato-κ3N:O:S)silver(I)], C6H5AgN2O2S
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Crystal structure of poly[(μ3-2-(pyrazin-2-ylthio)acetato-κ3N:O:S)silver(I)], C6H5AgN2O2S

  • Hui-Tao Fan EMAIL logo , Shu-Guang Qi , Shan-Shan Liu and Ling Zhao
Published/Copyright: May 26, 2017

Abstract

C6H5AgN2O2S, monoclinic, P21/c (no. 14), a = 10.0546(4) Å, b = 10.7329(5) Å, c = 6.9044(7) Å, β = 99.255(6)°, V = 735.39(9) Å3, Z = 4, Rgt(F) = 0.0422, wRref(F2) = 0.0967, T = 293(2) K.

CCDC no.:: 1524996

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 block
Size:0.20 × 0.18 × 0.16 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:29.7 cm−1
Diffractometer, scan mode:Xcalibur Eos, ω scans
2θmax, completeness:50°, >99%
N(hkl)measured, N(hkl)unique, Rint:2661, 1290, 0.036
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 1067
N(param)refined:109
Programs:SHELX [1], CrysAlisPRO [2]
Table 2

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

AtomxyzUiso*/Ueq
Ag11.07998(5)0.02959(4)0.82878(9)0.0419(2)
S10.84968(14)−0.00186(14)0.6007(2)0.0260(4)
O10.8937(3)−0.2611(4)0.6126(6)0.0326(11)
O20.6941(4)−0.3273(4)0.6726(7)0.0377(11)
N10.7864(4)0.3621(4)0.6046(7)0.0236(11)
N20.6381(4)0.1448(4)0.6435(7)0.0260(12)
C30.8381(5)0.2502(5)0.5909(8)0.0244(14)
H30.92590.24360.56530.029*
C20.6566(5)0.3665(6)0.6347(9)0.0309(15)
H20.61500.44330.64310.037*
C50.7238(5)−0.1110(5)0.6557(9)0.0251(14)
H5A0.7039−0.09470.78620.030*
H5B0.6414−0.09990.56290.030*
C40.7665(5)0.1414(5)0.6134(9)0.0240(13)
C60.7733(5)−0.2448(5)0.6447(9)0.0268(14)
C10.5854(5)0.2583(5)0.6531(9)0.0273(14)
H10.49630.26480.67310.033*

Source of materials

An excess of an aqueous NH3 solution was added dropwise to a suspension of Ag2O (0.023 g, 0.1 mmol) in MeOH/H2O (8 mL, 1:1 v/v), and the mixture was stirred for 15 min. 2-(Pyrazin-2-ylthio)acetic acid (0.018 g, 0.1 mmol) was then slowly added, and stirring was continued for another 30 min. The resultant colorless solution was allowed to stand in the dark at room temperature for a week. Colorless prism crystals of the title complex were obtained.

Experimental details

Absorption corrections were applied by using the multi-scan method [2]. Hydrogen atoms were located in difference electron density maps, and treated as riding atoms. The Uiso values of the hydrogen atoms were set to 1.2Ueq(C).

Comment

In the past few decades, the syntheses of silver(I) complexes attracted great interest because silver(I) principally is known for short Ag⋯Ag contacts. Furthermore Ag(I) has a high affinity for hard donor atoms such as nitrogen, oxygen or sulfur atoms, being a favorable and fashionable building block for MOFs [3], [4], [5], [6], [7]. With the aim of constructing unusual coordination architectures, we have engaged in the synthesis of coordination polymer based on 2-(pyrazin-2-ylthio)acetic acid (HL) with silver HL which comprise a pyrazinyl moiety and a carboxylic groups, may show a rich variety of coordination modes with nitrogen, oxygen and sulfur atoms and help to construct novel coordination polymers. On the other hand, it is a flexible ligand because the carboxylic groups can rotate aroud the C—S single bond.

Single crystal structure analysis reveals that the title structure consists of one crystallographically unique Ag(I) atom, and one L ligand. All geomtric parameters within the L ligand are in the expected ranges. The central Ag1 cation adopts Y-shaped coordination with one nitrogen atom [Ag1—N1 = 2.247(4) Å], one oxygen atom [Ag1—O1 = 2.291(4) Å] and one sulfur atom [Ag1—S1 = 2.604(1) Å] (cf. the figure). Both Ag—O and Ag—N bonds are within normal ranges [8]. Each L ligand links adjacent Ag(I) centers to form infinite double chains along the b axis. Such chains are further interconnected through the weak Ag⋯Ag contact (Ag1⋯Ag1 = 3.131(9) Å) to give rise to a sheet structure.

Acknowledgement

We gratefully acknowledge the financial support by Collaborative Innovation Center of Water Security for Water Source Region of Mid-line of South-to-North Diversion Project, Henan Province, and Key Laboratory of Ecological Security for Water Source Region of Mid-line of South-to-North Diversion Project of Henan Province, the National Natural Science Foundation of China (No. 21401112), the Science and Technology Research Key Project Department of Education in Henan Province (14A150026) and Nanyang Normal University Scientific Research Foundation Project (QN2016015).

References

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Received: 2016-12-30
Accepted: 2017-5-13
Published Online: 2017-5-26
Published in Print: 2017-7-26

©2017 Hui-Tao Fan 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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