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Volume 66 
Part 2 
Pages m196-m197  
February 2010  

Received 8 January 2010
Accepted 15 January 2010
Online 23 January 2010

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Key indicators
Single-crystal X-ray study
T = 291 K
Mean [sigma](C-C) = 0.002 Å
R = 0.020
wR = 0.055
Data-to-parameter ratio = 14.8
Details
Open access

Redetermination of aqua(dihydrogen ethylenediaminetetraacetato-[kappa]5O,O',N,N',O'')nickel(II)

Ivana Kocanová,a Juraj Kuchár,a* Vladimíra Dankovicováa and Juraj Cernáka

aDepartment of Inorganic Chemistry, Institute of Chemistry, P. J.Safárik University, Moyzesova 11, 041 54 Kosice, Slovakia
Correspondence e-mail: juraj.kuchar@upjs.sk

The crystal structure of the title compound, [Ni(C10H14N2O8)(H2O)] or [Ni(H2edta)(H2O)] (H4edta is ethylenediaminetetraacetic acid), originally determined by Smith & Hoard [J. Am. Chem. Soc. (1959), 81, 556-561] has been redetermined to a significantly higher precision. The NiII atom is coordinated in a distorted octahedral geometry by two N atoms and three O atoms from three carboxylate groups of the H2edta2- ligand and by an O atom of a water molecule. The complex molecules are linked by intermolecular O-H...O hydrogen bonds into layers perpendicular to [100].

Related literature

For the crystal structures of nickel(II) complexes with deprotonized derivates of H4edta, see: Agre, Trunov et al. (1980[Agre, V. M., Trunov, V. K. & Sysoeva, T. F. (1980). Dokl. Akad. Nauk SSSR, 250, 1123-1126.]); Agre, Sysoeva et al. (1980[Agre, V. M., Sysoeva, T. F., Trunov, V. K., Efremov, V. A., Fridman, A. Y. & Barkhanova, N. N. (1980). Zh. Strukt. Khim. 21, 110-117.]); Agre et al. (1981[Agre, V. M., Sysoeva, T. F., Trunov, V. K., Fridman, A. Y. & Barkhanova, N. N. (1981). Zh. Strukt. Khim. 22, 114-120.]); Coronado et al. (1986[Coronado, E., Drillon, M., Fuertes, A., Beltran, D., Mosset, A. & Galy, J. (1986). J. Am. Chem. Soc. 108, 900-905.]); Sysoeva et al. (1981[Sysoeva, T. F., Agre, V. M., Trunov, V. K., Dyatlova, N. M., Fridman, A. Ya. & Barkhanova, N. N. (1981). Zh. Strukt. Khim. 22, 99-105.]); Porai-Koshits et al. (1975[Porai-Koshits, M. A., Nesterova, Y. M., Polynova, T. N. & de Garcia Banus, D. T. (1975). Koord. Khim. 1, 682.]); Sysoeva et al. (1986[Sysoeva, T. F., Agre, V. M., Trunov, V. K., Dyatlova, N. M. & Fridman, A. Ya. (1986). Zh. Strukt. Khim. 27, 108-114.]); Zubkowski et al. (1995[Zubkowski, J. D., Perry, D. L., Valente, E. J. & Lott, S. (1995). Inorg. Chem. 34, 6409-6411.]); Stephens (1969[Stephens, F. S. (1969). J. Chem. Soc. A, pp. 1723-1734.]). For the earlier determination of the title compound, see: Smith & Hoard (1959[Smith, G. S. & Hoard, J. L. (1959). J. Am. Chem. Soc. 81, 556-561.]).

[Scheme 1]

Experimental

Crystal data

  • [Ni(C10H14N2O8)(H2O)]

  • Mr = 366.96

  • Monoclinic, P 21 /c

  • a = 11.6786 (2) Å

  • b = 6.9358 (1) Å

  • c = 16.6343 (2) Å

  • [beta] = 91.140 (1)°

  • V = 1347.12 (3) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 1.49 mm-1

  • T = 291 K

  • 0.35 × 0.31 × 0.15 mm
Data collection

  • Oxford Diffraction Xcalibur diffractometer with a Sapphire2 detector

  • Absorption correction: numerical [Clark & Reid (1995[Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897.]) in CrysAlis PRO (Oxford Diffraction, 2009[Oxford Diffraction (2009). CrysAlis PRO. Oxford Diffraction Ltd, Yarnton, England.])] Tmin = 0.690, Tmax = 0.830

  • 43864 measured reflections

  • 2935 independent reflections

  • 2534 reflections with I > 2[sigma](I)

  • Rint = 0.030
Refinement

  • R[F2 > 2[sigma](F2)] = 0.020

  • wR(F2) = 0.055

  • S = 1.06

  • 2935 reflections

  • 198 parameters

  • H-atom parameters constrained

  • [Delta][rho]max = 0.33 e Å-3

  • [Delta][rho]min = -0.18 e Å-3

Table 1
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
O1-H1...O7i 0.82 1.77 2.5557 (14) 159
O3-H3...O5ii 0.82 1.79 2.5864 (13) 164
O6-H6A...O9iii 0.88 2.15 2.9294 (12) 148
O6-H6B...O2iv 0.86 1.81 2.6394 (11) 162
Symmetry codes: (i) -x+1, -y+1, -z+1; (ii) [x, -y-{\script{1\over 2}}, z+{\script{1\over 2}}]; (iii) -x+1, -y, -z+1; (iv) [-x+1, y-{\script{1\over 2}}, -z+{\script{3\over 2}}].

Data collection: CrysAlis PRO (Oxford Diffraction, 2009[Oxford Diffraction (2009). CrysAlis PRO. Oxford Diffraction Ltd, Yarnton, England.]); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; 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 (Crystal Impact, 2007[Crystal Impact (2007). DIAMOND. Crystal Impact, Bonn, Germany.]); software used to prepare material for publication: SHELXL97.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: RZ2407 ).

Acknowledgements

This work was supported by the Slovak grant agency APVV (contract Nos. APVV-VVCE-0058-07 and APVV-0006-07) and the grant agency VEGA (grant No. 1/0089/09). Support from P. J. Safárik University (VVGS 37/09-10) is also gratefully acknowledged.

References

Agre, V. M., Sysoeva, T. F., Trunov, V. K., Efremov, V. A., Fridman, A. Y. & Barkhanova, N. N. (1980). Zh. Strukt. Khim. 21, 110-117.  [ChemPort]
Agre, V. M., Sysoeva, T. F., Trunov, V. K., Fridman, A. Y. & Barkhanova, N. N. (1981). Zh. Strukt. Khim. 22, 114-120.  [ChemPort]
Agre, V. M., Trunov, V. K. & Sysoeva, T. F. (1980). Dokl. Akad. Nauk SSSR, 250, 1123-1126.  [ChemPort]
Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897.  [CrossRef] [details]
Coronado, E., Drillon, M., Fuertes, A., Beltran, D., Mosset, A. & Galy, J. (1986). J. Am. Chem. Soc. 108, 900-905.  [CrossRef] [ChemPort] [ISI]
Crystal Impact (2007). DIAMOND. Crystal Impact, Bonn, Germany.
Oxford Diffraction (2009). CrysAlis PRO. Oxford Diffraction Ltd, Yarnton, England.
Porai-Koshits, M. A., Nesterova, Y. M., Polynova, T. N. & de Garcia Banus, D. T. (1975). Koord. Khim. 1, 682.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Smith, G. S. & Hoard, J. L. (1959). J. Am. Chem. Soc. 81, 556-561.  [CrossRef] [ChemPort] [ISI]
Stephens, F. S. (1969). J. Chem. Soc. A, pp. 1723-1734.
Sysoeva, T. F., Agre, V. M., Trunov, V. K., Dyatlova, N. M. & Fridman, A. Ya. (1986). Zh. Strukt. Khim. 27, 108-114.  [ChemPort]
Sysoeva, T. F., Agre, V. M., Trunov, V. K., Dyatlova, N. M., Fridman, A. Ya. & Barkhanova, N. N. (1981). Zh. Strukt. Khim. 22, 99-105.  [ChemPort]
Zubkowski, J. D., Perry, D. L., Valente, E. J. & Lott, S. (1995). Inorg. Chem. 34, 6409-6411.  [CrossRef] [ChemPort] [ISI]

Acta Cryst (2010). E66, m196-m197   [ doi:10.1107/S1600536810002011 ]

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