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Volume 69 
Part 1 
Pages m50-m51  
January 2013  

Received 9 November 2012
Accepted 8 December 2012
Online 15 December 2012

Key indicators
Single-crystal X-ray study
T = 293 K
Mean [sigma](C-C) = 0.007 Å
Disorder in solvent or counterion
R = 0.046
wR = 0.145
Data-to-parameter ratio = 15.1
Details
Open access

Hexakis([mu]3-2-hydroxynaphthalene-1-carboxaldehyde thiosemicarbazonato-[kappa]3N2:S:S)hexasilver(I) N,N-dimethylformamide tetrasolvate

aDepartment of Materials Chemistry, School of Materials Science and Engineering, Key Laboratory of Nonferrous Metal of the Ministry of Education, Central South University, Changsha 410083, People's Republic of China, and bChinese National Engineering Research Center for Control & Treatment of Heavy Metal Pollution (CNERC-CTHMP), Environmental Engineering Institute, School of Metallurgical Science and Engineering, Central South University, Changsha 410083, People's Republic of China
Correspondence e-mail: rosesunqz@yahoo.com.cn

In the title compound, [Ag6(C12H10N3OS)6]·4C3H7NO, the hexanuclear complex molecule lies about an inversion center. The six Ag atoms form a distorted octahedron, with Ag...Ag distances in the range 2.933 (1)-3.401 (1) Å. Each Ag atom is surrounded by one N atom and two thiolate S atoms from two deprotonated 2-hydroxy-1-naphthaldehyde thiosemicarbazone ligands. Each ligand coordinates three Ag atoms via a bridging thiolate S atom and a monodentate N atom, thus two Ag3S3 hexagonal rings are linked together. Two dimethylformamide solvent molecules are located in four sets of sites with half-occupancy and form O...H-N hydrogen bonds to the complex molecule. Intramolecular O-H...N hydrogen bonds are also present. The discrete hexanuclear clusters are further linked through [pi]-[pi] interactions into layers parallel to (001), the shortest distance between the centroids of aromatic rings being 3.698 (2) Å.

Related literature

For the structure and luminescent properties of d10 metal complexes, see: Brito et al. (2011[Brito, I., Vallejos, J., Cárdenas, A., López-Rodríguez, M., Bolte, M. & Llanos, J. (2011). Inorg. Chem. Commun. 14, 897-901.]); Forward et al. (1995[Forward, J. M., Bohmann, D., Fackler, J. P. & Staples, R. J. (1995). Inorg. Chem. 34, 6330-6336.]). For structures of related compexes with thiosemicarbazone Schiff base ligands, see: Ashfield et al. (2004[Ashfield, L. J., Cowley, A. R., Dilworth, J. R. & Donnelly, P. S. (2004). Inorg. Chem. 43, 4121-4123.]); Castiñeiras & Pedrido (2009[Castiñeiras, A. & Pedrido, R. (2009). Inorg. Chem. 48, 4847-4855.]); Li et al. (2010[Li, M. X., Zhang, D., Zhang, L. Z. & Niu, J. Y. (2010). Inorg. Chem. Commun. 13, 1268-1271.]); Onodera et al. (2007[Onodera, K., Kasuga, N. C., Takashima, T., Hara, A., Amano, A., Murakami, H. & Nomiya, K. (2007). Dalton Trans. pp. 3646-3652.]); Pedrido et al. (2009[Pedrido, R., Romero, M. J., Bermejo, M. R., Martínez-Calvo, M., González-Noya, A. M. & Zaragoza, G. (2009). Dalton Trans. pp. 8329-8340.]); Sun (2011[Sun, Q. Z. (2011). Chin. J. Struct. Chem. 30, 1355-1360.]); Sun et al. (2012[Sun, Q. Z., Liao, S. Y., Chai, L. Y., Xu, X. W., Yao, J. J. & Fang, Q. J. L. (2012). Chin. J. Struct. Chem. 31, 1229-1234.]); Sun & Chai (2012[Sun, Q. Z. & Chai, L. Y. (2012). Chin. J. Struct. Chem. 31, 408-414.]); Xu et al. (2011[Xu, C. Y., Sun, Q. Z., Chen, P. & Chai, L. Y. (2011). Chin. J. Struct. Chem. 30, 951-956.]). For bond-length data, see: Han et al. (2004[Han, W., Yi, L., Liu, Z. Q., Gu, W., Yan, S. P., Cheng, P., Liao, D. Z. & Jiang, Z. H. (2004). Eur. J. Inorg. Chem. pp. 2130-2136.]).

[Scheme 1]

Experimental

Crystal data
  • [Ag6(C12H10N3OS)6]·4C3H7NO

  • Mr = 2405.34

  • Monoclinic, C 2/c

  • a = 24.604 (3) Å

  • b = 18.877 (3) Å

  • c = 24.816 (3) Å

  • [beta] = 94.763 (3)°

  • V = 11486 (3) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 1.17 mm-1

  • T = 293 K

  • 0.22 × 0.20 × 0.18 mm

Data collection
  • Bruker SMART CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996[Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.]) Tmin = 0.238, Tmax = 0.373

  • 28454 measured reflections

  • 10056 independent reflections

  • 7829 reflections with I > 2s(I)

  • Rint = 0.042

Refinement
  • R[F2 > 2[sigma](F2)] = 0.046

  • wR(F2) = 0.145

  • S = 1.08

  • 10056 reflections

  • 667 parameters

  • 63 restraints

  • H-atom parameters constrained

  • [Delta][rho]max = 0.92 e Å-3

  • [Delta][rho]min = -0.42 e Å-3

Table 1
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
N3-H3B...O4 0.86 1.98 2.835 (8) 175
N6-H6B...O6i 0.86 2.00 2.845 (7) 166
N9-H9A...O5ii 0.86 2.31 3.049 (8) 145
N9-H9B...O7 0.86 2.02 2.870 (6) 172
O1-H1B...N1 0.82 1.86 2.588 (5) 147
O2-H2B...N4 0.82 1.85 2.583 (4) 148
O3-H3C...N7 0.82 1.86 2.587 (5) 147
Symmetry codes: (i) [-x+{\script{1\over 2}}, -y+{\script{3\over 2}}, -z+1]; (ii) [-x+{\script{1\over 2}}, y-{\script{1\over 2}}, -z+{\script{1\over 2}}].

Data collection: SMART (Bruker, 2000[Bruker (2000). SMART and SAINT . Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2000[Bruker (2000). SMART and SAINT . Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: YK2079 ).


Acknowledgements

The authors acknowledge financial support from the National Science and Technology Support Program (2012BAC12B03), the Postdoctoral Science Foundation of Central South University and the Fundamental Research Funds for the Central Universities (No. 2012QNZT001).

References

Ashfield, L. J., Cowley, A. R., Dilworth, J. R. & Donnelly, P. S. (2004). Inorg. Chem. 43, 4121-4123.  [ISI] [CrossRef] [PubMed] [ChemPort]
Brito, I., Vallejos, J., Cárdenas, A., López-Rodríguez, M., Bolte, M. & Llanos, J. (2011). Inorg. Chem. Commun. 14, 897-901.  [ISI] [CSD] [CrossRef] [ChemPort]
Bruker (2000). SMART and SAINT . Bruker AXS Inc., Madison, Wisconsin, USA.
Castiñeiras, A. & Pedrido, R. (2009). Inorg. Chem. 48, 4847-4855.  [ISI] [PubMed]
Forward, J. M., Bohmann, D., Fackler, J. P. & Staples, R. J. (1995). Inorg. Chem. 34, 6330-6336.  [CrossRef] [ChemPort] [ISI]
Han, W., Yi, L., Liu, Z. Q., Gu, W., Yan, S. P., Cheng, P., Liao, D. Z. & Jiang, Z. H. (2004). Eur. J. Inorg. Chem. pp. 2130-2136.  [ISI] [CSD] [CrossRef]
Li, M. X., Zhang, D., Zhang, L. Z. & Niu, J. Y. (2010). Inorg. Chem. Commun. 13, 1268-1271.  [ISI] [CSD] [CrossRef] [ChemPort]
Onodera, K., Kasuga, N. C., Takashima, T., Hara, A., Amano, A., Murakami, H. & Nomiya, K. (2007). Dalton Trans. pp. 3646-3652.  [CSD] [CrossRef]
Pedrido, R., Romero, M. J., Bermejo, M. R., Martínez-Calvo, M., González-Noya, A. M. & Zaragoza, G. (2009). Dalton Trans. pp. 8329-8340.  [CSD] [CrossRef]
Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Sun, Q. Z. (2011). Chin. J. Struct. Chem. 30, 1355-1360.  [ChemPort]
Sun, Q. Z. & Chai, L. Y. (2012). Chin. J. Struct. Chem. 31, 408-414.  [ChemPort]
Sun, Q. Z., Liao, S. Y., Chai, L. Y., Xu, X. W., Yao, J. J. & Fang, Q. J. L. (2012). Chin. J. Struct. Chem. 31, 1229-1234.  [ChemPort]
Xu, C. Y., Sun, Q. Z., Chen, P. & Chai, L. Y. (2011). Chin. J. Struct. Chem. 30, 951-956.  [ChemPort]


Acta Cryst (2013). E69, m50-m51   [ doi:10.1107/S1600536812050155 ]

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