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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

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)

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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