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Volume 68 
Part 11 
Pages m1325-m1326  
November 2012  

Received 14 September 2012
Accepted 28 September 2012
Online 6 October 2012

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Key indicators
Single-crystal X-ray study
T = 100 K
Mean [sigma](C-C) = 0.005 Å
Disorder in solvent or counterion
R = 0.039
wR = 0.088
Data-to-parameter ratio = 15.4
Details
Open access

2-Aminopyridinium trans-diaquabis(oxalato-[kappa]2O,O)chromate(III)

Justin Nenwa,a* Gouet Bebga,b Signé Martin,a Michel M. Bélombé,a Mohammed Mbarkic and Boniface P. T. Fokwac

aDepartment of Inorganic Chemistry, University of Yaounde I, POB 812 Yaounde, Cameroon,bHigher Teacher Training College, POB 47, University of Yaounde 1, Cameroon, and cInstitut für Anorganische Chemie, RWTH Aachen, D-52056 Aachen, Germany
Correspondence e-mail: jnenwa@yahoo.fr

In the title hybrid salt, (C5H7N2)[Cr(H2O)2(C2O4)2], the CrIII ion is coordinated in a slightly distorted octahedral environment by four O atoms from two oxalate ligands in the equatorial plane and by two water O atoms in the axial sites. The 2-aminopyridinium cation is disordered over two sets of sites in a 0.800 (7):0.200 (7) ratio. In the crystal, N-H...O and O-H...O hydrogen bonds connect the components into a three-dimensional network. The crystal studied was an inversion twin with components in a ratio 0.75 (2):0.25 (2).

Related literature

For general background to the coordination chemistry of oxalates, see: Martin et al. (2007[Martin, L., Day, P., Clegg, W., Harrington, R. W., Horton, P. N., Bingham, A., Hursthouse, M. B., McMillan, P. & Firth, S. (2007). J. Mater. Chem. 17, 3324-3329.]). For the structural characterization of organic-inorganic salts containing the [Cr(H2O)2(C2O4)2]- anion, see: Bélombé et al. (2009[Bélombé, M. M., Nenwa, J. & Emmerling, F. (2009). Z. Kristallogr. New Cryst. Struct. 224, 239-240.]); Nenwa et al. (2010[Nenwa, J., Belombe, M. M., Ngoune, J. & Fokwa, B. P. T. (2010). Acta Cryst. E66, m1410.]); Chérif et al. (2011[Chérif, I., Abdelhak, J., Zid, M. F. & Driss, A. (2011). Acta Cryst. E67, m1648-m1649.]); Chérif, Abdelhak et al. (2012[Chérif, I., Abdelhak, J., Zid, M. F. & Driss, A. (2012). Acta Cryst. E68, m824-m825.]); Chérif, Zid et al. (2012[Chérif, I., Zid, M. F., El-Ghozzi, M. & Avignant, D. (2012). Acta Cryst. E68, m900-m901.]).

[Scheme 1]

Experimental

Crystal data

  • (C5H7N2)[Cr(H2O)2(C2O4)2]

  • Mr = 359.20

  • Monoclinic, I a

  • a = 6.8627 (14) Å

  • b = 19.434 (4) Å

  • c = 9.854 (2) Å

  • [beta] = 99.90 (3)°

  • V = 1294.7 (5) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 0.94 mm-1

  • T = 100 K

  • 0.23 × 0.15 × 0.10 mm
Data collection

  • Bruker SMART APEX CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2004[Bruker (2004). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.811, Tmax = 0.912

  • 9645 measured reflections

  • 3716 independent reflections

  • 3391 reflections with I > 2[sigma](I)

  • Rint = 0.035
Refinement

  • R[F2 > 2[sigma](F2)] = 0.039

  • wR(F2) = 0.088

  • S = 1.04

  • 3716 reflections

  • 241 parameters

  • 21 restraints

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

  • [Delta][rho]max = 0.52 e Å-3

  • [Delta][rho]min = -0.30 e Å-3

  • Absolute structure: Flack (1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]), 1793 Friedel pairs

  • Flack parameter: 0.25 (2)

Table 1
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
OW1-HW1A...O23i 0.82 (2) 1.86 (2) 2.660 (4) 166 (3)
OW1-HW1B...O11ii 0.80 (2) 1.92 (2) 2.663 (3) 156 (4)
OW2-HW2A...O24iii 0.85 (2) 1.78 (2) 2.621 (4) 172 (4)
OW2-HW2B...O12iv 0.80 (2) 1.95 (2) 2.687 (3) 153 (4)
N1-H1A...O12v 0.88 2.33 3.183 (5) 164
N1-H1B...O23 0.88 2.38 3.251 (4) 171
N2-H2...O13v 0.88 2.02 2.865 (3) 159
Symmetry codes: (i) [x, -y+{\script{1\over 2}}, z+{\script{1\over 2}}]; (ii) [x-{\script{1\over 2}}, -y+1, z]; (iii) [x, -y+{\script{1\over 2}}, z-{\script{1\over 2}}]; (iv) [x+{\script{1\over 2}}, -y+1, z]; (v) [x+{\script{1\over 2}}, y-{\script{1\over 2}}, z+{\script{1\over 2}}].

Data collection: APEX2 (Bruker, 2004[Bruker (2004). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2004[Bruker (2004). 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: DIAMOND (Brandenburg, 2010[Brandenburg, K. (2010). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: WinGX Farrugia (1999[Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.]).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: LH5534 ).

Acknowledgements

The authors thank Professor Barthelemy Nyasse (Organic Chemistry Department, University of Yaounde I) for the donation of 2-aminopyridin and Tobias Storp (RWTH Aachen) for his technical support during the X-ray experiments.

References

Bélombé, M. M., Nenwa, J. & Emmerling, F. (2009). Z. Kristallogr. New Cryst. Struct. 224, 239-240.
Brandenburg, K. (2010). DIAMOND. Crystal Impact GbR, Bonn, Germany.
Bruker (2004). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Chérif, I., Abdelhak, J., Zid, M. F. & Driss, A. (2011). Acta Cryst. E67, m1648-m1649.  [CSD] [CrossRef] [details]
Chérif, I., Abdelhak, J., Zid, M. F. & Driss, A. (2012). Acta Cryst. E68, m824-m825.  [CrossRef] [details]
Chérif, I., Zid, M. F., El-Ghozzi, M. & Avignant, D. (2012). Acta Cryst. E68, m900-m901.  [CSD] [CrossRef] [details]
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.  [CrossRef] [ChemPort] [details]
Flack, H. D. (1983). Acta Cryst. A39, 876-881.  [CrossRef] [details]
Martin, L., Day, P., Clegg, W., Harrington, R. W., Horton, P. N., Bingham, A., Hursthouse, M. B., McMillan, P. & Firth, S. (2007). J. Mater. Chem. 17, 3324-3329.  [ISI] [CSD] [CrossRef] [ChemPort]
Nenwa, J., Belombe, M. M., Ngoune, J. & Fokwa, B. P. T. (2010). Acta Cryst. E66, m1410.  [CSD] [CrossRef] [details]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]

Acta Cryst (2012). E68, m1325-m1326   [ doi:10.1107/S1600536812040950 ]

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