Hexa­kis­(μ3-2-hy­droxy­naphthalene-1-carboxaldehyde thio­semicarbazonato-κ3N2:S:S)hexa­silver(I) N,N-dimethyl­formamide tetra­solvate

Sun, Q.; Chai, L.; Liu, H.; Wang, J.

doi:10.1107/S1600536812050155

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 (C-C) = 0.007 Å
Disorder in solvent or counterion
R = 0.046
wR = 0.145
Data-to-parameter ratio = 15.1
Details

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

Qiaozhen Sun,^a ^* Liyuan Chai,^b Hui Liu ^b and Junke Wang ^a

^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 AgAg 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 OH-N hydrogen bonds to the complex molecule. Intramolecular O-HN 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); Forward et al. (1995). For structures of related compexes with thiosemicarbazone Schiff base ligands, see: Ashfield et al. (2004); Castiñeiras & Pedrido (2009); Li et al. (2010); Onodera et al. (2007); Pedrido et al. (2009); Sun (2011); Sun et al. (2012); Sun & Chai (2012); Xu et al. (2011). For bond-length data, see: Han et al. (2004).

Experimental

Crystal data

[Ag₆(C₁₂H₁₀N₃OS)₆]·4C₃H₇NO
M_r = 2405.34
Monoclinic, C 2/c
a = 24.604 (3) Å
b = 18.877 (3) Å
c = 24.816 (3) Å
= 94.763 (3)°
V = 11486 (3) Å³
Z = 4
Mo K radiation
= 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) T_min = 0.238, T_max = 0.373
28454 measured reflections
10056 independent reflections
7829 reflections with I > 2s(I)
R_int = 0.042

Refinement

R[F² > 2(F²)] = 0.046
wR(F²) = 0.145
S = 1.08
10056 reflections
667 parameters
63 restraints
H-atom parameters constrained
_max = 0.92 e Å^-3
_min = -0.42 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
N3-H3BO4	0.86	1.98	2.835 (8)	175
N6-H6BO6ⁱ	0.86	2.00	2.845 (7)	166
N9-H9AO5ⁱⁱ	0.86	2.31	3.049 (8)	145
N9-H9BO7	0.86	2.02	2.870 (6)	172
O1-H1BN1	0.82	1.86	2.588 (5)	147
O2-H2BN4	0.82	1.85	2.583 (4)	148
O3-H3CN7	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); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008); 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.
Brito, I., Vallejos, J., Cárdenas, A., López-Rodríguez, M., Bolte, M. & Llanos, J. (2011). Inorg. Chem. Commun. 14, 897-901.
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Castiñeiras, A. & Pedrido, R. (2009). Inorg. Chem. 48, 4847-4855.
Forward, J. M., Bohmann, D., Fackler, J. P. & Staples, R. J. (1995). Inorg. Chem. 34, 6330-6336.
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.
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Xu, C. Y., Sun, Q. Z., Chen, P. & Chai, L. Y. (2011). Chin. J. Struct. Chem. 30, 951-956.

metal-organic compounds

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