cis-Bis(1,10-phenanthroline-κ2N,N′)bis­(pyridin-4-amine-κN1)ruthenium(II) bis­(hexa­fluoridophosphate)Part I. Ruthenium(II) coordination complexes with 4-amino­pyridine and α-diimine ligands.

Camilo, M.R.; Martins, F.T.; Malta, V.R.S.; Ellena, J.; Carlos, R.M.

doi:10.1107/S1600536812051999

Volume 69
Part 2
Pages m75-m76
February 2013

Received 7 December 2012
Accepted 28 December 2012
Online 9 January 2013

Key indicators
Single-crystal X-ray study
T = 298 K
Mean (C-C) = 0.011 Å
R = 0.053
wR = 0.151
Data-to-parameter ratio = 13.5
Details

cis-Bis(1,10-phenanthroline-²N,N')bis(pyridin-4-amine-N¹)ruthenium(II) bis(hexafluoridophosphate)¹

Mariana R. Camilo,^a Felipe T. Martins,^b Valéria R. S. Malta,^c Javier Ellena ^d and Rose M. Carlos ^a ^*

^aUniversidade Federal de São Carlos, Departamento de Química, CP 676, CEP 13565-905, São Carlos/SP, Brazil,^bUniversidade Federal de Goias, Instituto de Química, Campus Samambaia, CP 131, CEP 74001-970, Goiania/GO, Brazil,^cUniversidade Federal de Alagoas, Centro de Ciências Exatas e Naturais, Departamento de Química, CEP 57072-970, Maceió/AL, Brazil, and ^dUniversidade de São Paulo, Instituto de Física de Sao Carlos, CP 369, CEP 13560-970, São Carlos/SP, Brazil
Correspondence e-mail: rosem@ufscar.br

In the title complex, [Ru(C₁₂H₈N₂)₂(C₅H₆N₂)₂](PF₆)₂, the Ru^II atom is bonded to two [alpha] -diimine ligands, viz. 1,10-phenanthroline (phen), in a cis configuration, in addition with with two 4-aminopyridine (4Apy) ligands, resulting in a distorted octahedral coordination geometry. N-HF hydrogen-bonding interactions play an important role in the crystal assembly: 2₁-screw-axis-related complex molecules and PF₆^- counter-ions alternate in helical chains formed along the a axis by means of these contacts. N-H [pi] contacts (Hcentroid = 3.45 Å) are responsible for cross-linking between the helical chains along [001].

Related literature

For compounds with similar properties, see Bonneson et al. (1983); Salassa et al. (2009). For the use of 4Apy, see Sinha & Shrivastava (2012). For similar structures, see: Stoyanov et al. (2002).

Experimental

Crystal data

[Ru(C₁₂H₈N₂)₂(C₅H₆N₂)₂](PF₆)₂
M_r = 939.65
Orthorhombic, P 2₁ c n
a = 13.0943 (3) Å
b = 14.5730 (3) Å
c = 19.9366 (5) Å
V = 3804.37 (15) Å³
Z = 4
Mo K radiation
= 0.59 mm^-1
T = 298 K
0.40 × 0.20 × 0.10 mm

Data collection

Nonius KappaCCD diffractometer
Absorption correction: Gaussian (Coppens et al., 1965) T_min = 0.699, T_max = 0.938
29253 measured reflections
6964 independent reflections
5348 reflections with I > 2(I)
R_int = 0.066

Refinement

R[F² > 2(F²)] = 0.053
wR(F²) = 0.151
S = 1.04
6964 reflections
514 parameters
1 restraint
H-atom parameters constrained
_max = 0.39 e Å^-3
_min = -0.48 e Å^-3
Absolute structure: Flack (1983), 3264 Friedel pairs
Flack parameter: 0.25 (6)

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
N4-H4AF5	0.86	2.45	3.231 (12)	151
N4A-H4A1F1Aⁱ	0.86	2.23	3.063 (12)	163
N4A-H4A2F3Aⁱⁱ	0.86	2.34	3.18 (2)	165
Symmetry codes: (i) $[x, -y+{\script{3\over 2}}, z-{\script{1\over 2}}]$ ; (ii) $[x+{\script{1\over 2}}, y+{\script{1\over 2}}, -z+{\script{3\over 2}}]$ .

Data collection: COLLECT (Nonius, 2000); cell refinement: SCALEPACK (Otwinowski & Minor, 1997); data reduction: DENZO (Otwinowski & Minor, 1997) and SCALEPACK; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012) and Mercury (Macrae et al., 2006); software used to prepare material for publication: WinGX (Farrugia, 2012).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: BG2495 ).

Acknowledgements

The authors wish to thank FAPESP (Proc. 2009/08218-0; 2008/52859-7), CNPq (Universal 470890/2010-0) and CAPES for the grants and fellowships given to this research.

References

Bonneson, P. J., Walsh, L., Pennington, W. T., Cordes, A. W. & Durham, B. (1983). Inorg. Chem. 22, 1761-1765.
Coppens, P., Leiserowitz, L. & Rabinovich, D. (1965). Acta Cryst. 18, 1035-1038.
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.
Flack, H. D. (1983). Acta Cryst. A39, 876-881.
Macrae, C. F., Edgington, P. R., McCabe, P., Pidcock, E., Shields, G. P., Taylor, R., Towler, M. & van de Streek, J. (2006). J. Appl. Cryst. 39, 453-457.
Nonius (2000). COLLECT. Nonius BV, Delft, The Netherlands.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307-326. New York: Academic Press.
Salassa, L., Garino, C., Salassa, G., Nervi, C., Gobetto, R., Lamberti, C., Gianolio, D., Bizzarri, R. & Sadler, P. J. (2009). Inorg. Chem. 48, 1469-1481.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Sinha, S. K. & Shrivastava, S. K. (2012). Med. Chem. Res. 21, 4395-4402.
Stoyanov, S. R., Villegas, J. M. & Rillema, D. P. (2002). Inorg. Chem. 41, 2941-2945.

metal-organic compounds

cis-Bis(1,10-phenanthroline-2N,N')bis(pyridin-4-amine-N1)ruthenium(II) bis(hexafluoridophosphate)1