supplementary materials
Poly[![[mu]](/logos/entities/mu_rmgif.gif)
2-chlorido-(2-3H+-1,3,4-thiadiazolium-2-thiolato-![[kappa]](/logos/entities/kappa_rmgif.gif)
2S:S)silver(I)]
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.
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.
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).
Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT (Bruker, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).
Poly[µ
2-chlorido-(µ
2-3
H+-1,3,4-thiadiazolium-2-thiolato-
κ2S:
S)silver(I)]
top
Crystal data top
| [AgCl(C2H2N2S2)] | F(000) = 496 |
| Mr = 261.50 | Dx = 2.768 Mg m−3 |
| Orthorhombic, P212121 | Mo Kα radiation, λ = 0.71073 Å |
| Hall symbol: P 2ac 2ab | Cell parameters from 1870 reflections |
| a = 4.0316 (9) Å | θ = 3.3–27.2° |
| b = 8.473 (2) Å | µ = 4.19 mm−1 |
| c = 18.368 (4) Å | T = 294 K |
| V = 627.4 (2) Å3 | Block, colourless |
| Z = 4 | 0.23 × 0.13 × 0.06 mm |
Data collection top
Bruker SMART CCD area-detector
diffractometer | 1161 independent reflections |
| Radiation source: fine-focus sealed tube | 1085 reflections with I > 2σ(I) |
| graphite | Rint = 0.035 |
| φ and ω scans | θmax = 25.5°, θmin = 2.7° |
Absorption correction: multi-scan
(SADABS; Bruker, 1997) | h = −4→4 |
| Tmin = 0.446, Tmax = 0.786 | k = −10→10 |
| 4169 measured reflections | l = −22→22 |
Refinement top
| Refinement on F2 | Secondary atom site location: difference Fourier map |
| Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
| R[F2 > 2σ(F2)] = 0.031 | H-atom parameters constrained |
| wR(F2) = 0.083 | w = 1/[σ2(Fo2) + (0.0526P)2]
where P = (Fo2 + 2Fc2)/3 |
| S = 1.09 | (Δ/σ)max < 0.001 |
| 1161 reflections | Δρmax = 1.22 e Å−3 |
| 73 parameters | Δρmin = −0.65 e Å−3 |
| 0 restraints | Absolute structure: Flack (1983), 438 Friedel pairs |
| Primary atom site location: structure-invariant direct methods | Flack parameter: 0.05 (6) |
Crystal data top
| [AgCl(C2H2N2S2)] | V = 627.4 (2) Å3 |
| Mr = 261.50 | Z = 4 |
| Orthorhombic, P212121 | Mo Kα radiation |
| a = 4.0316 (9) Å | µ = 4.19 mm−1 |
| b = 8.473 (2) Å | T = 294 K |
| c = 18.368 (4) Å | 0.23 × 0.13 × 0.06 mm |
Data collection top
Bruker SMART CCD area-detector
diffractometer | 1161 independent reflections |
Absorption correction: multi-scan
(SADABS; Bruker, 1997) | 1085 reflections with I > 2σ(I) |
| Tmin = 0.446, Tmax = 0.786 | Rint = 0.035 |
| 4169 measured reflections | θmax = 25.5° |
Refinement top
| R[F2 > 2σ(F2)] = 0.031 | H-atom parameters constrained |
| wR(F2) = 0.083 | Δρmax = 1.22 e Å−3 |
| S = 1.09 | Δρmin = −0.65 e Å−3 |
| 1161 reflections | Absolute structure: Flack (1983), 438 Friedel pairs |
| 73 parameters | Flack parameter: 0.05 (6) |
| 0 restraints | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top| | x | y | z | Uiso*/Ueq | |
| Ag1 | 0.97702 (12) | −0.03604 (5) | 0.18414 (2) | 0.04254 (19) | |
| Cl1 | 1.4870 (4) | −0.08711 (14) | 0.09609 (6) | 0.0323 (3) | |
| S1 | 0.6628 (4) | 0.55205 (15) | 0.14333 (7) | 0.0346 (3) | |
| S2 | 0.9323 (4) | 0.25800 (16) | 0.21696 (7) | 0.0356 (4) | |
| N1 | 0.6067 (12) | 0.2855 (5) | 0.0889 (2) | 0.0350 (12) | |
| H1 | 0.6188 | 0.1852 | 0.0823 | 0.042* | |
| N2 | 0.4580 (15) | 0.3800 (5) | 0.0387 (2) | 0.0420 (13) | |
| C1 | 0.7324 (12) | 0.3512 (6) | 0.1482 (2) | 0.0266 (11) | |
| C2 | 0.4723 (15) | 0.5228 (6) | 0.0601 (3) | 0.0329 (12) | |
| H2 | 0.3863 | 0.6056 | 0.0327 | 0.039* | |
Atomic displacement parameters (Å2) top| | U11 | U22 | U33 | U12 | U13 | U23 |
| Ag1 | 0.0574 (3) | 0.0311 (3) | 0.0391 (3) | 0.0042 (2) | −0.0090 (2) | 0.00192 (16) |
| Cl1 | 0.0369 (7) | 0.0237 (6) | 0.0365 (6) | −0.0013 (6) | −0.0016 (6) | −0.0009 (5) |
| S1 | 0.0485 (8) | 0.0187 (6) | 0.0364 (7) | 0.0010 (6) | −0.0108 (6) | −0.0037 (6) |
| S2 | 0.0546 (9) | 0.0215 (6) | 0.0307 (7) | 0.0065 (6) | −0.0107 (6) | −0.0034 (5) |
| N1 | 0.059 (3) | 0.019 (2) | 0.026 (2) | 0.003 (2) | −0.007 (2) | −0.0031 (18) |
| N2 | 0.065 (4) | 0.027 (3) | 0.034 (2) | 0.003 (3) | −0.015 (3) | 0.0008 (19) |
| C1 | 0.032 (3) | 0.023 (3) | 0.025 (2) | 0.000 (2) | 0.004 (2) | −0.001 (2) |
| C2 | 0.044 (3) | 0.026 (3) | 0.028 (2) | 0.002 (3) | −0.008 (2) | 0.001 (2) |
Geometric parameters (Å, °) top
| Ag1—S2i | 2.5454 (14) | S2—C1 | 1.694 (5) |
| Ag1—S2 | 2.5695 (15) | S2—Ag1iv | 2.5453 (14) |
| Ag1—Cl1ii | 2.5897 (15) | N1—C1 | 1.323 (6) |
| Ag1—Cl1 | 2.6514 (15) | N1—N2 | 1.361 (6) |
| Cl1—Ag1iii | 2.5897 (15) | N1—H1 | 0.86 |
| S1—C1 | 1.727 (5) | N2—C2 | 1.273 (7) |
| S1—C2 | 1.729 (5) | C2—H2 | 0.93 |
| | | |
| S2i—Ag1—S2 | 120.49 (3) | C1—N1—N2 | 118.6 (4) |
| S2i—Ag1—Cl1ii | 116.15 (5) | C1—N1—H1 | 120.7 |
| S2—Ag1—Cl1ii | 104.77 (4) | N2—N1—H1 | 120.7 |
| S2i—Ag1—Cl1 | 102.24 (5) | C2—N2—N1 | 109.3 (4) |
| S2—Ag1—Cl1 | 110.84 (5) | N1—C1—S2 | 126.8 (4) |
| Cl1ii—Ag1—Cl1 | 100.56 (5) | N1—C1—S1 | 108.1 (4) |
| Ag1iii—Cl1—Ag1 | 100.56 (5) | S2—C1—S1 | 125.1 (3) |
| C1—S1—C2 | 88.6 (2) | N2—C2—S1 | 115.4 (4) |
| C1—S2—Ag1iv | 106.32 (18) | N2—C2—H2 | 122.3 |
| C1—S2—Ag1 | 108.09 (18) | S1—C2—H2 | 122.3 |
| Ag1iv—S2—Ag1 | 145.29 (5) | | |
| | | |
| S2i—Ag1—Cl1—Ag1iii | −60.05 (5) | N2—N1—C1—S2 | −179.1 (4) |
| S2—Ag1—Cl1—Ag1iii | 69.61 (5) | N2—N1—C1—S1 | 0.2 (6) |
| Cl1ii—Ag1—Cl1—Ag1iii | 180.0 | Ag1iv—S2—C1—N1 | −172.7 (5) |
| S2i—Ag1—S2—C1 | −158.63 (19) | Ag1—S2—C1—N1 | 2.7 (5) |
| Cl1ii—Ag1—S2—C1 | −25.46 (19) | Ag1iv—S2—C1—S1 | 8.2 (4) |
| Cl1—Ag1—S2—C1 | 82.19 (19) | Ag1—S2—C1—S1 | −176.5 (3) |
| S2i—Ag1—S2—Ag1iv | 13.55 (10) | C2—S1—C1—N1 | −0.5 (4) |
| Cl1ii—Ag1—S2—Ag1iv | 146.72 (12) | C2—S1—C1—S2 | 178.8 (4) |
| Cl1—Ag1—S2—Ag1iv | −105.63 (12) | N1—N2—C2—S1 | −0.9 (7) |
| C1—N1—N2—C2 | 0.4 (8) | C1—S1—C2—N2 | 0.8 (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, °) top
| D—H···A | D—H | H···A | D···A | D—H···A |
| N1—H1···Cl1ii | 0.86 | 2.38 | 3.197 (4) | 158 |
| Symmetry codes: (ii) x−1, y, z. |
Table 1
Selected geometric parameters (Å) top| Ag1—S2i | 2.5454 (14) | Ag1—Cl1ii | 2.5897 (15) |
| Ag1—S2 | 2.5695 (15) | Ag1—Cl1 | 2.6514 (15) |
| Symmetry codes: (i) −x+2, y−1/2, −z+1/2; (ii) x−1, y, z. |
Table 2
Hydrogen-bond geometry (Å, °) top
| D—H···A | D—H | H···A | D···A | D—H···A |
| N1—H1···Cl1ii | 0.86 | 2.38 | 3.197 (4) | 158 |
| Symmetry codes: (ii) x−1, y, z. |
The authors thank Luoyang Normal University for supporting this work.
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.
Wei, X. Y., Di, D., Chu, W., Zhu, Q. L. & Huang, R. D. (2008). Inorg. Chim. Acta, 361, 1819–1826.
![[Figure 1]](./ci2771fig1thm.gif)
![[Figure 2]](./ci2771fig2thm.gif)
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).