Di-μ-thio­semicarbazide-κ4S:S-bis­[chlori­dobis(triphenyl­phosphane-κP)silver(I)]

Wattanakanjana, Y.; Pakawatchai, C.; Nimthong, R.

doi:10.1107/S1600536812051562

Volume 69
Part 2
Pages m83-m84
February 2013

Received 17 December 2012
Accepted 21 December 2012
Online 9 January 2013

Key indicators
Single-crystal X-ray study
T = 293 K
Mean (C-C) = 0.004 Å
R = 0.026
wR = 0.069
Data-to-parameter ratio = 20.0
Details

Di--thiosemicarbazide-⁴S:S-bis[chloridobis(triphenylphosphane-P)silver(I)]

Yupa Wattanakanjana,^a ^* Chaveng Pakawatchai ^b and Ruthairat Nimthong ^b

^aDepartment of Chemistry, Faculty of Science, Prince of Songkla University, Hat Yai, Songkhla 90112, Thailand, and ^bDepartment of Chemistry and Center of Excellence for Innovation in Chemistry, Faculty of Science, Prince of Songkla University, Hat Yai, Songkhla 90112, Thailand
Correspondence e-mail: yupa.t@psu.ac.th

The dinuclear title complex, [Ag₂Cl₂(CH₅N₃S)₂(C₁₈H₁₅P)₂], lies across an inversion center. The Ag^I ion exhibits a slightly distorted tetrahedral coordination geometry formed by a P atom from a triphenylphosphane ligand, two metal-bridging S atoms from thiosemicabazide ligands and one chloride ion. The S atoms bridge two symmetry-related Ag^I ions, forming a strictly planar Ag₂S₂ core with an AgAg separation of 2.7802 (7) Å. There is an intramolecular N-HCl hydrogen bond. In the crystal, N-HCl and N-HS hydrogen bonds link complex molecules, forming layers parallel to (001). These layers are connected through [pi] - [pi] stacking interactions [centroid-centroid distance = 3.665 (2) Å], leading to the formation of a three-dimensional network.

Related literature

For metal(I) complexes of phosphine ligands as precursors for the preparation of mixed-ligand complexes, see: Ferrari et al. (2007); Pakawatchai et al. (2012). For potential applications of thiosemicarbazide derivatives and their metal complexes, see: Pandeya et al. (1999); Wujec et al. (2009); Mohareb & Mohamed (2012); He et al. (2012). For examples of related discrete complexes, see: Wattanakanjana et al. (2012); Lobana et al. (2008).

Experimental

Crystal data

[Ag₂Cl₂(CH₅N₃S)₂(C₁₈H₁₅P)₂]
M_r = 993.46
Triclinic, $[P \overline 1]$
a = 8.7845 (4) Å
b = 9.4656 (4) Å
c = 13.7529 (6) Å
= 109.276 (1)°
= 98.306 (1)°
= 99.739 (1)°
V = 1038.94 (8) Å³
Z = 1
Mo K radiation
= 1.28 mm^-1
T = 293 K
0.38 × 0.30 × 0.10 mm

Data collection

Bruker SMART CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2003) T_min = 0.638, T_max = 0.880
14302 measured reflections
5026 independent reflections
4627 reflections with I > 2(I)
R_int = 0.036

Refinement

R[F² > 2(F²)] = 0.026
wR(F²) = 0.069
S = 1.06
5026 reflections
251 parameters
5 restraints
H atoms treated by a mixture of independent and constrained refinement
_max = 0.38 e Å^-3
_min = -0.55 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
N3-H3BCl1ⁱ	0.87 (2)	2.67 (2)	3.535 (2)	171 (2)
N2-H2S1ⁱⁱ	0.83 (2)	2.66 (2)	3.4320 (15)	155 (2)
N1-H1BCl1ⁱⁱⁱ	0.85 (2)	2.63 (2)	3.4088 (16)	154 (2)
N1-H1ACl1	0.89 (2)	2.45 (2)	3.3239 (16)	170 (2)
Symmetry codes: (i) x-1, y, z; (ii) -x+1, -y+2, -z+1; (iii) -x+2, -y+3, -z+1.

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: Mercury (Macrae et al., 2008); software used to prepare material for publication: SHELXL97 and publCIF (Westrip, 2010).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: LH5573 ).

Acknowledgements

We gratefully acknowledge financial support from the Center for Innovation in Chemistry (PERCH-CIC), the Commission on Higher Education, Ministry of Education, the Department of Chemistry and the Graduate School, Prince of Songkla University.

References

Bruker (1998). SMART. Bruker AXS Inc., Madison, Wisconsin, USA.
Bruker (2003). SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Ferrari, M. B., Bisceglie, F., Cavalli, E., Pelosi, G., Tarasconi, P. & Verdolino, V. (2007). Inorg. Chim. Acta, 360, 3233-3240.
He, J., Wang, X., Zhao, X., Liang, Y., He, H. & Fu, L. (2012). Eur. J. Med. Chem. 54, 925-930.
Lobana, T. S., Sharma, R. S. & Butcher, R. J. (2008). Polyhedron, 27, 1375-1380.
Macrae, C. F., Bruno, I. J., Chisholm, J. A., Edgington, P. R., McCabe, P., Pidcock, E., Rodriguez-Monge, L., Taylor, R., van de Streek, J. & Wood, P. A. (2008). J. Appl. Cryst. 41, 466-470.
Mohareb, R. M. & Mohamed, A. A. (2012). Int. J. Pure. Appl. Chem. 2, 144-155.
Pakawatchai, C., Jantaramas, P., Mokhagul, J. & Nimthong, R. (2012). Acta Cryst. E68, m1506-m1507.
Pandeya, S. N., Sriram, D., Nath, G. & DeClercq, E. (1999). Eur. J. Pharm. Sci. 9, 25-31.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Wattanakanjana, Y., Pakawatchai, C., Kowittheeraphong, S. & Nimthong, R. (2012). Acta Cryst. E68, m1572-m1573.
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.
Wujec, M., Stefanska, J., Siwek, A. & Tatarczak, M. (2009). Acta Polon. Pharm. Drug Res. 66, 73-82.