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Acta Crystallogr Sect E Struct Rep Online. 2009 May 1; 65(Pt 5): m507.
Published online 2009 April 10. doi:  10.1107/S1600536809012975
PMCID: PMC2977568

Poly[μ2-chlorido-(μ2-3H +-1,3,4-thia­diazo­lium-2-thiol­ato-κ2 S:S)silver(I)]

Abstract

In the title compound, [AgCl(C2H2N2S2)]n, the AgI ion has a distorted tetra­hedral geometry, defined by two S atoms of two symmetry-related 1,3,4-thia­diazo­lium-2-thiol­ate ligands and two chloride ions. The AgI ions are bridged into a two-dimensional network parallel to the ab plane by chloride ions and thia­diazole ligands. In the network, the AgI ions are separated by 4.0316 (12) Å along the a axis and by 4.8822 (13) Å along the b axis. N—H(...)Cl hydrogen bonds are observed within the network.

Related literature

For bond-length data, see: Dinger et al. (1998 [triangle]); Wei et al. (2008 [triangle]).

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Object name is e-65-0m507-scheme1.jpg

Experimental

Crystal data

  • [AgCl(C2H2N2S2)]
  • M r = 261.50
  • Orthorhombic, An external file that holds a picture, illustration, etc.
Object name is e-65-0m507-efi3.jpg
  • a = 4.0316 (9) Å
  • b = 8.473 (2) Å
  • c = 18.368 (4) Å
  • V = 627.4 (2) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 4.19 mm−1
  • T = 294 K
  • 0.23 × 0.13 × 0.06 mm

Data collection

  • Bruker SMART CCD area-detector diffractometer
  • Absorption correction: multi-scan (SADABS; Bruker, 1997 [triangle]) T min = 0.446, T max = 0.786
  • 4169 measured reflections
  • 1161 independent reflections
  • 1085 reflections with I > 2σ(I)
  • R int = 0.035

Refinement

  • R[F 2 > 2σ(F 2)] = 0.031
  • wR(F 2) = 0.083
  • S = 1.09
  • 1161 reflections
  • 73 parameters
  • H-atom parameters constrained
  • Δρmax = 1.22 e Å−3
  • Δρmin = −0.65 e Å−3
  • Absolute structure: Flack (1983 [triangle]), 438 Friedel pairs
  • Flack parameter: 0.05 (6)

Data collection: SMART (Bruker, 1997 [triangle]); cell refinement: SAINT (Bruker, 1997 [triangle]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: SHELXTL (Sheldrick, 2008 [triangle]); software used to prepare material for publication: SHELXTL.

Table 1
Selected bond lengths (Å)
Table 2
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809012975/ci2771sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809012975/ci2771Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

The authors thank Luoyang Normal University for supporting this work.

supplementary crystallographic information

Comment

The asymmetric unit of the title compound consists of one AgI ion, one 1,3,4-thiadiazolium-2-thiolate ligand, and one Cl atom. As depicted in Fig. 1, the AgI ion is coordinated by two S atoms from two thiadiazole ligands and two Cl atoms in a distorted tetrahedral geometry. The Ag—S and Ag—Cl bond distances (Table 1) are within the range expected for such coordination bonds (Dinger et al., 1998; Wei et al., 2008). The thiadiazole ligand shows a monodentate bridging mode. The adjacent AgI atoms are bridged by Cl atoms to form chains, which are cross-linked by thiadiazole ligands to form a two-dimensional network parallel to the ab plane (Fig. 2). In the network, the Ag atoms are separated by 4.0316 (12) Å along the a axis and 4.8822 (13) Å along the b axis. Intramolecular N—H···Cl hydrogen bonds are observed in the network (Table 2).

Experimental

1,3,4-Thiadiazolium-2-thiolate (0.5 mmol) was added at room temperature to a ammonia solution (10 ml) of AgCl (0.5 mmol). After the addition, a colourless precipitate immediately formed and the suspension was stirred for 2 h. The precipitate was filtered off and washed with MeCN. Single crystals suitable for X-ray analysis were obtained by slow diffusion of Et2O into a water solution of the solid.

Refinement

H atoms were positioned geometrically and treated as riding, with N-H = 0.86 Å and Uiso(H) = 1.2Ueq(N), and C-H = 0.93 Å and Uiso(H) = 1.2Ueq(C).

Figures

Fig. 1.
A view of the local coordination of the AgI atom in the title compound. Displacement ellipsoids are drawn at the 30% probability level. Symmetry codes: (A) 2 -x, y - 1/2, 1/2 - z; (B) x - 1, y, z.
Fig. 2.
A view of the two-dimensional network parallel to the ab plane.

Crystal data

[AgCl(C2H2N2S2)]F(000) = 496
Mr = 261.50Dx = 2.768 Mg m3
Orthorhombic, P212121Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ac 2abCell parameters from 1870 reflections
a = 4.0316 (9) Åθ = 3.3–27.2°
b = 8.473 (2) ŵ = 4.19 mm1
c = 18.368 (4) ÅT = 294 K
V = 627.4 (2) Å3Block, colourless
Z = 40.23 × 0.13 × 0.06 mm

Data collection

Bruker SMART CCD area-detector diffractometer1161 independent reflections
Radiation source: fine-focus sealed tube1085 reflections with I > 2σ(I)
graphiteRint = 0.035
[var phi] and ω scansθmax = 25.5°, θmin = 2.7°
Absorption correction: multi-scan (SADABS; Bruker, 1997)h = −4→4
Tmin = 0.446, Tmax = 0.786k = −10→10
4169 measured reflectionsl = −22→22

Refinement

Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.031H-atom parameters constrained
wR(F2) = 0.083w = 1/[σ2(Fo2) + (0.0526P)2] where P = (Fo2 + 2Fc2)/3
S = 1.09(Δ/σ)max < 0.001
1161 reflectionsΔρmax = 1.22 e Å3
73 parametersΔρmin = −0.65 e Å3
0 restraintsAbsolute structure: Flack (1983), 438 Friedel pairs
Primary atom site location: structure-invariant direct methodsFlack parameter: 0.05 (6)

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

xyzUiso*/Ueq
Ag10.97702 (12)−0.03604 (5)0.18414 (2)0.04254 (19)
Cl11.4870 (4)−0.08711 (14)0.09609 (6)0.0323 (3)
S10.6628 (4)0.55205 (15)0.14333 (7)0.0346 (3)
S20.9323 (4)0.25800 (16)0.21696 (7)0.0356 (4)
N10.6067 (12)0.2855 (5)0.0889 (2)0.0350 (12)
H10.61880.18520.08230.042*
N20.4580 (15)0.3800 (5)0.0387 (2)0.0420 (13)
C10.7324 (12)0.3512 (6)0.1482 (2)0.0266 (11)
C20.4723 (15)0.5228 (6)0.0601 (3)0.0329 (12)
H20.38630.60560.03270.039*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Ag10.0574 (3)0.0311 (3)0.0391 (3)0.0042 (2)−0.0090 (2)0.00192 (16)
Cl10.0369 (7)0.0237 (6)0.0365 (6)−0.0013 (6)−0.0016 (6)−0.0009 (5)
S10.0485 (8)0.0187 (6)0.0364 (7)0.0010 (6)−0.0108 (6)−0.0037 (6)
S20.0546 (9)0.0215 (6)0.0307 (7)0.0065 (6)−0.0107 (6)−0.0034 (5)
N10.059 (3)0.019 (2)0.026 (2)0.003 (2)−0.007 (2)−0.0031 (18)
N20.065 (4)0.027 (3)0.034 (2)0.003 (3)−0.015 (3)0.0008 (19)
C10.032 (3)0.023 (3)0.025 (2)0.000 (2)0.004 (2)−0.001 (2)
C20.044 (3)0.026 (3)0.028 (2)0.002 (3)−0.008 (2)0.001 (2)

Geometric parameters (Å, °)

Ag1—S2i2.5454 (14)S2—C11.694 (5)
Ag1—S22.5695 (15)S2—Ag1iv2.5453 (14)
Ag1—Cl1ii2.5897 (15)N1—C11.323 (6)
Ag1—Cl12.6514 (15)N1—N21.361 (6)
Cl1—Ag1iii2.5897 (15)N1—H10.86
S1—C11.727 (5)N2—C21.273 (7)
S1—C21.729 (5)C2—H20.93
S2i—Ag1—S2120.49 (3)C1—N1—N2118.6 (4)
S2i—Ag1—Cl1ii116.15 (5)C1—N1—H1120.7
S2—Ag1—Cl1ii104.77 (4)N2—N1—H1120.7
S2i—Ag1—Cl1102.24 (5)C2—N2—N1109.3 (4)
S2—Ag1—Cl1110.84 (5)N1—C1—S2126.8 (4)
Cl1ii—Ag1—Cl1100.56 (5)N1—C1—S1108.1 (4)
Ag1iii—Cl1—Ag1100.56 (5)S2—C1—S1125.1 (3)
C1—S1—C288.6 (2)N2—C2—S1115.4 (4)
C1—S2—Ag1iv106.32 (18)N2—C2—H2122.3
C1—S2—Ag1108.09 (18)S1—C2—H2122.3
Ag1iv—S2—Ag1145.29 (5)
S2i—Ag1—Cl1—Ag1iii−60.05 (5)N2—N1—C1—S2−179.1 (4)
S2—Ag1—Cl1—Ag1iii69.61 (5)N2—N1—C1—S10.2 (6)
Cl1ii—Ag1—Cl1—Ag1iii180.0Ag1iv—S2—C1—N1−172.7 (5)
S2i—Ag1—S2—C1−158.63 (19)Ag1—S2—C1—N12.7 (5)
Cl1ii—Ag1—S2—C1−25.46 (19)Ag1iv—S2—C1—S18.2 (4)
Cl1—Ag1—S2—C182.19 (19)Ag1—S2—C1—S1−176.5 (3)
S2i—Ag1—S2—Ag1iv13.55 (10)C2—S1—C1—N1−0.5 (4)
Cl1ii—Ag1—S2—Ag1iv146.72 (12)C2—S1—C1—S2178.8 (4)
Cl1—Ag1—S2—Ag1iv−105.63 (12)N1—N2—C2—S1−0.9 (7)
C1—N1—N2—C20.4 (8)C1—S1—C2—N20.8 (5)

Symmetry codes: (i) −x+2, y−1/2, −z+1/2; (ii) x−1, y, z; (iii) x+1, y, z; (iv) −x+2, y+1/2, −z+1/2.

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
N1—H1···Cl1ii0.862.383.197 (4)158

Symmetry codes: (ii) x−1, y, z.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: CI2771).

References

  • Bruker (1997). SMART, SAINT and SADABS Bruker AXS Inc., Madison, Wisconsin, USA.
  • Dinger, M. B., Henderson, W., Nicholson, B. K. & Robinson, W. T. (1998). J. Organomet. Chem.560, 169–181.
  • Flack, H. D. (1983). Acta Cryst. A39, 876–881.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]
  • Wei, X. Y., Di, D., Chu, W., Zhu, Q. L. & Huang, R. D. (2008). Inorg. Chim. Acta, 361, 1819–1826.

Articles from Acta Crystallographica Section E: Structure Reports Online are provided here courtesy of International Union of Crystallography