[Journal logo]

Volume 67 
Part 7 
Pages m945-m946  
July 2011  

Received 23 May 2011
Accepted 11 June 2011
Online 18 June 2011

[hb5891sup1]
[3d view]

[Cited in]
[Download citation]
Key indicators
Single-crystal X-ray study
T = 296 K
Mean [sigma](C-C) = 0.008 Å
R = 0.035
wR = 0.086
Data-to-parameter ratio = 12.4
Details
Open access

Pyridinium [2,6-bis(5-phenyl-1H-pyrazol-3-yl-[kappa]N2)pyridine-[kappa]N]tetranitrato-[kappa]6O,O';[kappa]O-samarium(III) pyridine monosolvate

Shui Hu,a Yongfeng Zhao,a Huai-Ming Hub* and Li Liua*

aKey Laboratory of Carbon Fiber and Functional Polymers, Ministry of Education, Beijing University of Chemical Technology, Beijing 100029, People's Republic of China, and bCollege of Chemistry and Materials Science, Northwest University, Xi'an 710069, People's Republic of China
Correspondence e-mail: LiuL2001cn@yahoo.com.cn, chemhu1@nwu.edu.cn

In the title compound, (C5H6N)[Sm(NO3)4(C23H17N5)]·C5H5N, the SmIII atom is ten-coordinated by the N,N',N''-tridentate bis(pyrazole) ligand and seven O atoms from four nitrate anions (three bidentate and one monodentate). The dihedral angles between the central pyridine ring and adjacent pyrazole rings in the ligand are 1.3 (2) and 3.2 (2)°; the dihedral angles between the pyrazole rings and their pendant phenyl rings are 42.0 (3) and 16.1 (2)°. The conformation of the anionic complex ion is supported by an intramolecular N-H...O hydrogen bond. In the crystal, inversion dimers linked by pairs of N-H...O hydrogen bonds occur. The pyridinium cation forms an N-H...N hydrogen bond.

Related literature

For the synthesis of the ligand, see: Zhao et al. (2009[Zhao, B., Shu, H. M., Hu, H. M., Qin, T. & Chen, X. L. (2009). J. Coord. Chem. 62, 1025-1034.]). For related transition metal and lanthanide complexes, see: Argent et al. (2005[Argent, S. P., Adams, H., Harding, L. P., Riis-Johannessen, T., Jeffery, J. C. & Ward, M. D. (2005). New J. Chem. 29, 904-911.]); Bardwell et al. (1997[Bardwell, D. A., Jeffery, J. C., Jones, P. L., McCleverty, J. A., Psillakis, E., Reeves, Z. & Ward, M. D. (1997). J. Chem. Soc. Dalton Trans. pp. 2079-2086.]); Barrios et al. (2008[Barrios, L. A., Aromi, G., Ribas, J., Uber, J. S., Roubeau, O., Sakai, K., Masaoka, S., Gamez, P. & Reedijk, J. (2008). Eur. J. Inorg. Chem. pp. 3871-3876.]); Coronado et al. (2003[Coronado, E., Gimenez-Lopez, M. C., Gimenez-Saiz, C., Martinez-Agudo, J. M. & Romero, F. M. (2003). Polyhedron, 22, 2375-2380.]); Dong et al. (1999[Dong, D., Matthews, J. P., Craig, D. C. & Baker, A. T. (1999). Inorg. Chim. Acta, 284, 266-272.]); Dutta et al. (1996[Dutta, S. K., Nanda, K. K., Flörke, U., Bhadbhade, M. & Nag, K. (1996). J. Chem. Soc. Dalton Trans. pp. 2371-2379.]); Gamez et al. (2002[Gamez, P., Steensma, R. H., Driessen, W. L. & Reedijk, J. (2002). Inorg. Chim. Acta, 333, 51-56.]); Gimenez-Lopez et al. (2005[Gimenez-Lopez, M. C., Clemente-Leon, M., Coronado, E., Romero, F. M., Shova, S. & Tuchagues, J. P. (2005). Eur. J. Inorg. Chem. pp. 2783-2787.]); Scudder et al. (2005[Scudder, M. L., Craig, D. C. & Goodwin, H. A. (2005). CrystEngComm, 7, 642-649.]); Wei et al. (2008[Wei, Q. H., Argent, S. P., Adams, H. & Ward, M. D. (2008). New J. Chem. 32, 73-82.]).

[Scheme 1]

Experimental

Crystal data

  • (C5H6N)[Sm(NO3)4(C23H17N5)]·C5H5N

  • Mr = 921.01

  • Triclinic, [P \overline 1]

  • a = 10.5234 (19) Å

  • b = 12.826 (2) Å

  • c = 14.190 (3) Å

  • [alpha] = 75.970 (2)°

  • [beta] = 86.453 (2)°

  • [gamma] = 84.108 (2)°

  • V = 1847.0 (6) Å3

  • Z = 2

  • Mo K[alpha] radiation

  • [mu] = 1.67 mm-1

  • T = 296 K

  • 0.18 × 0.12 × 0.10 mm
Data collection

  • Bruker APEXII CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2005[Bruker (2005). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.753, Tmax = 0.851

  • 9121 measured reflections

  • 6391 independent reflections

  • 5442 reflections with I > 2[sigma](I)

  • Rint = 0.020
Refinement

  • R[F2 > 2[sigma](F2)] = 0.035

  • wR(F2) = 0.086

  • S = 1.09

  • 6391 reflections

  • 517 parameters

  • 1 restraint

  • H atoms treated by a mixture of independent and constrained refinement

  • [Delta][rho]max = 0.95 e Å-3

  • [Delta][rho]min = -0.67 e Å-3

Table 1
Selected bond lengths (Å)

Sm1-O10 2.435 (3)
Sm1-O5 2.485 (3)
Sm1-O7 2.490 (3)
Sm1-O1 2.495 (3)
Sm1-N2 2.513 (3)
Sm1-O2 2.520 (3)
Sm1-O4 2.528 (3)
Sm1-N4 2.544 (3)
Sm1-O8 2.628 (3)
Sm1-N3 2.661 (3)

Table 2
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
N1-H1...O12 0.86 1.99 2.807 (5) 159
N5-H5...O9i 0.86 2.10 2.947 (4) 169
N10-H10A...N11ii 0.85 (2) 1.90 (3) 2.727 (6) 166 (6)
Symmetry codes: (i) -x+1, -y, -z+2; (ii) x, y, z+1.

Data collection: APEX2 (Bruker, 2005[Bruker (2005). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2005[Bruker (2005). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; 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: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXTL.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: HB5891 ).

References

Argent, S. P., Adams, H., Harding, L. P., Riis-Johannessen, T., Jeffery, J. C. & Ward, M. D. (2005). New J. Chem. 29, 904-911.  [ChemPort]
Bardwell, D. A., Jeffery, J. C., Jones, P. L., McCleverty, J. A., Psillakis, E., Reeves, Z. & Ward, M. D. (1997). J. Chem. Soc. Dalton Trans. pp. 2079-2086.
Barrios, L. A., Aromi, G., Ribas, J., Uber, J. S., Roubeau, O., Sakai, K., Masaoka, S., Gamez, P. & Reedijk, J. (2008). Eur. J. Inorg. Chem. pp. 3871-3876.
Bruker (2005). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Coronado, E., Gimenez-Lopez, M. C., Gimenez-Saiz, C., Martinez-Agudo, J. M. & Romero, F. M. (2003). Polyhedron, 22, 2375-2380.  [ChemPort]
Dong, D., Matthews, J. P., Craig, D. C. & Baker, A. T. (1999). Inorg. Chim. Acta, 284, 266-272.  [ChemPort]
Dutta, S. K., Nanda, K. K., Flörke, U., Bhadbhade, M. & Nag, K. (1996). J. Chem. Soc. Dalton Trans. pp. 2371-2379.
Gamez, P., Steensma, R. H., Driessen, W. L. & Reedijk, J. (2002). Inorg. Chim. Acta, 333, 51-56.  [ChemPort]
Gimenez-Lopez, M. C., Clemente-Leon, M., Coronado, E., Romero, F. M., Shova, S. & Tuchagues, J. P. (2005). Eur. J. Inorg. Chem. pp. 2783-2787.
Scudder, M. L., Craig, D. C. & Goodwin, H. A. (2005). CrystEngComm, 7, 642-649.  [ChemPort]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Wei, Q. H., Argent, S. P., Adams, H. & Ward, M. D. (2008). New J. Chem. 32, 73-82.  [ChemPort]
Zhao, B., Shu, H. M., Hu, H. M., Qin, T. & Chen, X. L. (2009). J. Coord. Chem. 62, 1025-1034.  [ChemPort]

Acta Cryst (2011). E67, m945-m946   [ doi:10.1107/S1600536811022653 ]

This is an open-access article distributed under the terms of the Creative Commons Attribution Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.