Bis[bis­(3,5-diamino-1H-1,2,4-triazol-4-ium)copper(I)] tris­(hexa­fluoridosilicate)

Mys'kiv, M.; Goreshnik, E.

doi:10.1107/S160053681004225X

Volume 66
Part 11
Pages m1453-m1454
November 2010

Received 14 September 2010
Accepted 18 October 2010
Online 23 October 2010

Key indicators
Single-crystal X-ray study
T = 293 K
Mean (N-C) = 0.004 Å
R = 0.053
wR = 0.155
Data-to-parameter ratio = 16.8
Details

Bis[bis(3,5-diamino-1H-1,2,4-triazol-4-ium)copper(I)] tris(hexafluoridosilicate)

Marian Mys'kiv ^a ^* and Evgeny Goreshnik ^b

^aDepartment of Inorganic Chemistry, Ivan Franko National University, Cyryla & Mefodia, 6, L'viv, Ukraine, and ^bDepartment of Inorganic Chemistry and Technology, Jozef Stefan Institute, Jamova 39 1000 Ljubljana, Slovenia
Correspondence e-mail: myskiv@franko.lviv.ua

In the title compound, [Cu(C₂H₆N₅)₂]₂(SiF₆)₃, the asymmetric unit is composed of one [Cu(HL)₂]³⁺ cation (where L is 3,5-diamino-1,2,4-triazole) and one and a half SiF₆^2- anions. The rather large positively charged guanazole ligand moiety promotes the low metal coordination number of 2 for the Cu^I atom. The compound was obtained using the electrochemical alternating-current technique starting from an ethanol-methanol solution of CuSiF₆·4H₂O and guanazole. In the crystal, N-HF hydrogen bonds play an important role in the formation of a three-dimensional network. As a result of these hydrogen bonds, there are also [pi] - [pi] interactions [centroid-centroid distance = 3.3024 (14) Å] involving one of the triazole groups in molecules related by an inversion center, and short CuN interactions [2.909 (3) Å] involving an -NH₂ group, leading to the formation of a dimer-like arrangement.

Related literature

For 1,2,4-triazole and its functionalized derivatives, see: Potts (1984). For complexes of the same ligand and copper(I) complexes of similar voluminous ligands, see: Aznar et al. (2006); Fabretti (1992); Goreshnik et al. (2004).

Experimental

Crystal data

[Cu(C₂H₆N₅)₂]₂(SiF₆)₃
M_r = 953.84
Triclinic, $[P \overline 1]$
a = 7.482 (2) Å
b = 8.366 (1) Å
c = 12.131 (3) Å
= 87.98 (2)°
= 89.11 (2)°
= 67.89 (2)°
V = 703.1 (3) Å³
Z = 1
Mo K radiation
= 1.81 mm^-1
T = 293 K
0.24 × 0.20 × 0.04 mm

Data collection

Siemens AED2 diffractometer
Absorption correction: numerical (de Meulanaer & Tompa, 1965) T_min = 0.649, T_max = 0.935
4089 measured reflections
4089 independent reflections
3367 reflections with I > 2(I)
3 standard reflections every 60 min intensity decay: 2%

Refinement

R[F² > 2(F²)] = 0.053
wR(F²) = 0.155
S = 1.06
4089 reflections
244 parameters
4 restraints
H atoms treated by a mixture of independent and constrained refinement
_max = 1.23 e Å^-3
_min = -1.01 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
N2-H2F2ⁱ	0.86 (2)	1.86 (2)	2.694 (3)	166 (4)
N3-H3F8	0.88 (2)	2.02 (3)	2.798 (3)	146 (4)
N4-H4BF1ⁱⁱ	0.86	1.95	2.742 (4)	153
N4-H4AF9ⁱⁱ	0.86	1.95	2.801 (3)	171
N5-H5AF6ⁱⁱⁱ	0.86	1.95	2.803 (3)	174
N5-H5BF9^iv	0.86	2.07	2.898 (3)	162
N7-H7F4ⁱ	0.86 (2)	1.85 (2)	2.686 (3)	162 (4)
N8-H8F7^v	0.86 (2)	2.04 (3)	2.812 (3)	148 (4)
N8-H8F3^v	0.86 (2)	2.22 (3)	2.813 (3)	126 (3)
N9-H9BF8^vi	0.86	2.05	2.892 (3)	166
N9-H9AF5^vii	0.86	2.02	2.841 (4)	159
N10-H10BF5^v	0.86	2.22	2.909 (3)	137
N10-H10AF6ⁱⁱⁱ	0.86	2.02	2.845 (3)	160
Symmetry codes: (i) x-1, y, z; (ii) -x+1, -y+1, -z; (iii) x, y-1, z; (iv) -x+2, -y, -z; (v) -x+1, -y, -z+1; (vi) x-1, y, z+1; (vii) -x, -y+1, -z+1.

Data collection: STADI4 (Stoe & Cie, 1998); cell refinement: STADI4; data reduction: X-RED (Stoe & Cie, 1998); program(s) used to solve structure: SHELXS86 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Crystal Impact, 2010), ORTEPIII (Burnett & Johnson, 1996) and ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: enCIFer (Allen et al., 2004).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: SU2214 ).

Acknowledgements

The authors thank the Slovenian Research Agency (ARRS) and the Ukrainian Ministry for Science and Higher Education for financial support (bilateral project BI-UA/09-10-015, M/55-2009)

References

Allen, F. H., Johnson, O., Shields, G. P., Smith, B. R. & Towler, M. (2004). J. Appl. Cryst. 37, 335-338.
Aznar, E., Ferrer, S., Borrás, J., Lloret, F., Liu-González, M., Rodríguez-Prieto, M. & García-Granda, S. (2006). Eur. J. Inorg. Chem. pp. 5115-5125.
Burnett, M. N. & Johnson, C. K. (1996). ORTEPIII. Report ORNL-6895. Oak Ridge National Laboratory, Tennessee, USA.
Crystal Impact (2010). DIAMOND. Crystal Impact GbR, Bonn, Germany
Fabretti, A. C. (1992). J. Crystallogr. Spectrosc. Res. 22, 523-526.
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.
Goreshnik, E., Schollmeyer, D. & Mys'kiv, M. (2004). Acta Cryst. E60, m279-m281.
Meulenaer, J. de & Tompa, H. (1965). Acta Cryst. 19, 1014-1018.
Potts, K. T. (1984). Editor. Comprehensive Heterocycle Chemistry, Vol. 5. Oxford: Pergamon Press.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Stoe & Cie (1998). STADI4 and X-RED. Stoe &Cie GmbH, Darmstadt, Germany.

metal-organic compounds