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Volume 66 
Part 10 
Pages m1185-m1186  
October 2010  

Received 9 July 2010
Accepted 25 August 2010
Online 4 September 2010

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Key indicators
Single-crystal X-ray study
T = 93 K
Mean [sigma](C-C) = 0.007 Å
R = 0.039
wR = 0.089
Data-to-parameter ratio = 20.5
Details
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A tetrasilver(I)ditungsten(VI) cluster with sulfide and bis(diphenylphosphino)methane ligands

Rong Wang,a Li-Li Song,a Ke-Yi Hu,a* Qiong-Hua Jina and Cun-Lin Zhangb

aDepartment of Chemistry, Capital Normal University, Beijing 100048, People's Republic of China, and bBeijing Key Laboratory for Terahertz Spectroscopy and Imaging, Key Laboratory of Terahertz Optoelectronics, Ministry of Education, Capital Normal University, Beijing 100048, People's Republic of China
Correspondence e-mail: jinqh204@163.com

The asymmetric unit of the title complex, [Ag4W2S8(C25H22P2)3]·2C3H7NO, tris[[mu]2-bis(diphenylphosphino)methane]-3:6[kappa]2P:P';4:5[kappa]2P:P';5:6[kappa]2P:P'-[mu]5-sulfido-2:3:4:5:6[kappa]5S-[mu]3-sulfido-1:3:4[kappa]3S-tetra-[mu]2-sulfido-1:3[kappa]2S;1:4[kappa]2S;2:5[kappa]2S;2:6[kappa]2S-disulfido-1[kappa]S,2[kappa]S-tetrasilver(I)ditungsten(VI) N,N-dimethylformamide disolvate, contains two [WS4]2- anions, four silver cations, three bidentate-bridging bis(diphenylphosphino)methane (dppm) ligands and two N,N-dimethylformamide (DMF) solvent molecules. The coordination geometry of each Ag atom is distorted tetrahedral. Two Ag ions are coordinated by [mu]2-S and [mu]5-S atoms, and by two P atoms from two dppm ligands, while the other two Ag atoms are coordinated by [mu]2-S, [mu]3-S and [mu]5-S atoms, and by one P atom from a dppm ligand.

Related literature

For related structures, see: Yu et al. (2001[Yu, H., Xu, Q. F., Sun, Z. R., Ji, S. Z., Chen, J. X., Liu, Q., Lang, J. P. & Tatsumi, K. (2001). Chem. Commun. pp. 2614-2615.]). For general background to Mo(W)-Cu(Ag)-S clusters derived from tetrathiotungstate and tetrathiomolybdate [MS4]2-(M = Mo, W) synthons, see: George et al.(2000[George, G. N., Pickering, I. J., Yu, E. Y., Prince, R. C., Bursakov, S. A., Bursakov, O. Y. & Moura, I. J. (2000). J. Am. Chem. Soc. 122, 8321-8322.], 2003[George, G. N., Pickering, I. J., Yu, E. Y., Harris, H. H., Gailer, J., Klein, D., Lichtmannegger, J. & Summer, K. H. (2003). J. Am. Chem. Soc. 125, 1704-1705.]); Hong et al. (1997[Hong, M., Wu, D., Cao, R., Lei, X., Liu, H. & Lu, J. (1997). Inorg. Chim. Acta, 258, 25-32.]); Lang et al. (2006[Lang, J. P., Xu, Q. F., Zhang, W. H., Li, H. X., Ren, Z. G., Chen, J. X. & Zhang, Y. (2006). Inorg. Chem. 45, 10487-10496.]); Niu et al. (2005[Niu, Y. Y., Song, Y. L., Hou, H. W. & Zhu, Y. (2005). Inorg. Chem. 44, 2553-2559.]); Ren et al. (2006[Ren, Z. G., Li, H. X., Liu, G. F., Zhang, W. H., Lang, J. P., Zhang, Y. & Song, Y. L. (2006). Organometallics, 25, 4351-4357.]); Shi et al. (1995[Shi, S., Chen, Z. R., Hou, H. W., Xin, X. Q. & Yu, K. B. (1995). Chem. Mater. 7, 1519-1524.]); Yu et al. (2001[Yu, H., Xu, Q. F., Sun, Z. R., Ji, S. Z., Chen, J. X., Liu, Q., Lang, J. P. & Tatsumi, K. (2001). Chem. Commun. pp. 2614-2615.]); Zhang et al. (2000[Zhang, Q. F., Xiong, Y. N., Lai, T. S., Ji, W. & Xin, X. Q. (2000). J. Phys. Chem. B, 204, 3446-3449.], 2004[Zhang, W. J., Behrens, A., Galtjens, J., Ebel, M., Wu, X. T. & Rehder, D. (2004). Inorg. Chem. 43, 3020-3023.]).

[Scheme 1]

Experimental

Crystal data

  • [Ag4W2S8(C25H22P2)3]·2C3H7NO

  • Mr = 2354.95

  • Monoclinic, P 21 /c

  • a = 22.931 (2) Å

  • b = 14.0395 (12) Å

  • c = 27.855 (3) Å

  • [beta] = 107.224 (1)°

  • V = 8565.6 (14) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 3.93 mm-1

  • T = 93 K

  • 0.47 × 0.43 × 0.43 mm
Data collection

  • Rigaku R-AXIS RAPID diffractometer

  • Absorption correction: multi-scan (ABSCOR; Higashi, 1995[Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan.]) Tmin = 0.262, Tmax = 0.281

  • 69256 measured reflections

  • 19520 independent reflections

  • 18777 reflections with I > 2[sigma](I)

  • Rint = 0.045
Refinement

  • R[F2 > 2[sigma](F2)] = 0.039

  • wR(F2) = 0.089

  • S = 1.14

  • 19520 reflections

  • 950 parameters

  • H-atom parameters constrained

  • [Delta][rho]max = 1.20 e Å-3

  • [Delta][rho]min = -1.36 e Å-3

Data collection: RAPID-AUTO (Rigaku, 2004[Rigaku (2004). RAPID-AUTO. Rigaku Corporation, Tokyo, Japan.]); cell refinement: RAPID-AUTO; data reduction: RAPID-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: ORTEPIII (Burnett & Johnson, 1996[Burnett, M. N. & Johnson, C. K. (1996). ORTEPIII. Report ORNL-6895. Oak Ridge National Laboratory, Tennessee, USA.]) and ORTEP-3 for Windows (Farrugia, 1997[Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.]); software used to prepare material for publication: SHELXL97.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: DN2590 ).

Acknowledgements

This work was supported by the National Keystone Basic Research Program (973 Program) under grant No. 2007CB310408, No. 2006CB302901 and the Funding Project for Academic Human Resources Development in Institutions of Higher Learning Under the Jurisdiction of Beijing Municipality. It was also supported by the State Key Laboratory of Functional Materials for Informatics, Shanghai Institute of Microsystem and Information Technology, Chinese Academy of Sciences.

References

Burnett, M. N. & Johnson, C. K. (1996). ORTEPIII. Report ORNL-6895. Oak Ridge National Laboratory, Tennessee, USA.
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.  [CrossRef] [details]
George, G. N., Pickering, I. J., Yu, E. Y., Harris, H. H., Gailer, J., Klein, D., Lichtmannegger, J. & Summer, K. H. (2003). J. Am. Chem. Soc. 125, 1704-1705.  [ISI] [CrossRef] [PubMed] [ChemPort]
George, G. N., Pickering, I. J., Yu, E. Y., Prince, R. C., Bursakov, S. A., Bursakov, O. Y. & Moura, I. J. (2000). J. Am. Chem. Soc. 122, 8321-8322.  [ISI] [CrossRef] [ChemPort]
Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan.
Hong, M., Wu, D., Cao, R., Lei, X., Liu, H. & Lu, J. (1997). Inorg. Chim. Acta, 258, 25-32.  [ChemPort]
Lang, J. P., Xu, Q. F., Zhang, W. H., Li, H. X., Ren, Z. G., Chen, J. X. & Zhang, Y. (2006). Inorg. Chem. 45, 10487-10496.  [ISI] [CSD] [CrossRef] [PubMed] [ChemPort]
Niu, Y. Y., Song, Y. L., Hou, H. W. & Zhu, Y. (2005). Inorg. Chem. 44, 2553-2559.  [ISI] [CrossRef] [PubMed] [ChemPort]
Ren, Z. G., Li, H. X., Liu, G. F., Zhang, W. H., Lang, J. P., Zhang, Y. & Song, Y. L. (2006). Organometallics, 25, 4351-4357.  [CSD] [CrossRef] [ChemPort]
Rigaku (2004). RAPID-AUTO. Rigaku Corporation, Tokyo, Japan.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Shi, S., Chen, Z. R., Hou, H. W., Xin, X. Q. & Yu, K. B. (1995). Chem. Mater. 7, 1519-1524.  [CrossRef] [ChemPort] [ISI]
Yu, H., Xu, Q. F., Sun, Z. R., Ji, S. Z., Chen, J. X., Liu, Q., Lang, J. P. & Tatsumi, K. (2001). Chem. Commun. pp. 2614-2615.  [CSD] [CrossRef]
Zhang, W. J., Behrens, A., Galtjens, J., Ebel, M., Wu, X. T. & Rehder, D. (2004). Inorg. Chem. 43, 3020-3023.  [ISI] [CSD] [CrossRef] [PubMed] [ChemPort]
Zhang, Q. F., Xiong, Y. N., Lai, T. S., Ji, W. & Xin, X. Q. (2000). J. Phys. Chem. B, 204, 3446-3449.  [CrossRef]

Acta Cryst (2010). E66, m1185-m1186   [ doi:10.1107/S1600536810034197 ]

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