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Volume 69 
Part 10 
Pages m532-m533  
October 2013  

Received 26 August 2013
Accepted 29 August 2013
Online 4 September 2013

Key indicators
Single-crystal X-ray study
T = 90 K
Mean [sigma](C-C) = 0.002 Å
R = 0.029
wR = 0.072
Data-to-parameter ratio = 15.4
Details
Open access

Bis[1-methoxy-2,2,2-tris(pyrazol-1-yl-[kappa]N2)ethane]nickel(II) bis(trifluoromethanesulfonate) dihydrate

aDepartment of Biochemistry, Chemistry and Physics, Southern Arkansas University, Magnolia, AR 71753, USA, and bDepartment of Chemistry, University of Kentucky, Lexington, KY 40506, USA
Correspondence e-mail: GannaLyubartseva@saumag.edu

In the title salt, [Ni(C12H14N6O)2](CF3SO3)2·2H2O, the NiII cation is located on an inversion centre and is coordinated by six N atoms from two tridentate 1-methoxy-2,2,2-tris(pyrazol-1-yl)ethane ligands in a distorted octahedral geometry. The Ni-N distances range from 2.0594 (12) to 2.0664 (12) Å, intra-ligand N-Ni-N angles range from 84.59 (5) to 86.06 (5)°, and adjacent inter-ligand N-Ni-N angles range between 93.94 (5) and 95.41 (5)°. In the crystal, inversion-related pyrazole rings are [pi]-[pi] stacked, with an interplanar spacing of 3.4494 (18) Å, forming chains that propagate parallel to the a-axis direction. Intermolecular O-H...O hydrogen bonds are present between water molecules and trifluoromethanesulfonate anions.

Related literature

Pyrazole-based tridentate ligands are drawing more attention because of their topology and nature of donor atoms, see: Paulo et al. (2004[Paulo, A., Correia, J. D. G., Campello, M. P. C. & Santos, I. (2004). Polyhedron, 23, 331-360.]); Bigmore et al. (2005[Bigmore, H. R., Lawrence, S. C., Mountford, P. & Tredget, C. S. (2005). Dalton Trans. pp. 635-651.]). For the ligand synthesis, see: Maria et al. (2007[Maria, L., Cunha, S., Videira, M., Gano, L., Paulo, A., Santos, I. C. & Santos, I. (2007). Dalton Trans. pp. 3010-3019.]). The compound reported here was prepared as part of our ongoing research effort to study nitrogen-donor tridentate scorpionate ligands coordinated to nickel, see: Lyubartseva et al. (2011[Lyubartseva, G., Parkin, S. & Mallik, U. P. (2011). Acta Cryst. E67, m1656-m1657.], 2012[Lyubartseva, G., Parkin, S., Mallik, U. P. & Jeon, H. K. (2012). Acta Cryst. E68, m888.]); Lyubartseva & Parkin (2009[Lyubartseva, G. & Parkin, S. (2009). Acta Cryst. E65, m1530.]).

[Scheme 1]

Experimental

Crystal data
  • [Ni(C12H14N6O)2](CF3O3S)2·2H2O

  • Mr = 909.46

  • Triclinic, [P \overline 1]

  • a = 8.5582 (2) Å

  • b = 9.6515 (2) Å

  • c = 12.2347 (2) Å

  • [alpha] = 110.399 (1)°

  • [beta] = 103.665 (1)°

  • [gamma] = 97.317 (1)°

  • V = 895.66 (3) Å3

  • Z = 1

  • Mo K[alpha] radiation

  • [mu] = 0.76 mm-1

  • T = 90 K

  • 0.26 × 0.22 × 0.15 mm

Data collection
  • Nonius KappaCCD diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 2008a[Sheldrick, G. M. (2008a). SADABS University of Göttingen, Germany.]) Tmin = 0.760, Tmax = 0.862

  • 25573 measured reflections

  • 4095 independent reflections

  • 3708 reflections with I > 2[sigma](I)

  • Rint = 0.023

Refinement
  • R[F2 > 2[sigma](F2)] = 0.029

  • wR(F2) = 0.072

  • S = 1.07

  • 4095 reflections

  • 266 parameters

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

  • [Delta][rho]max = 0.47 e Å-3

  • [Delta][rho]min = -0.49 e Å-3

Table 1
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
O1W-H2W...O3A 0.94 (3) 2.06 (3) 2.994 (2) 174 (2)
O1W-H1W...O3Ai 0.97 (3) 2.12 (3) 3.0613 (19) 163 (2)
Symmetry code: (i) -x+2, -y+2, -z+1.

Data collection: COLLECT (Nonius, 1998[Nonius (1998). COLLECT. Nonius BV, Delft, The Netherlands.]); cell refinement: SCALEPACK (Otwinowski & Minor, 1997[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.]); data reduction: DENZO-SMN (Otwinowski & Minor, 1997[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.]); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008b[Sheldrick, G. M. (2008b). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL2013 (Sheldrick, 2008b[Sheldrick, G. M. (2008b). Acta Cryst. A64, 112-122.]); molecular graphics: XP in SHELXTL (Sheldrick, 2008b[Sheldrick, G. M. (2008b). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXL2013.


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: TK5252 ).


Acknowledgements

GL gratefully acknowledges the Southern Arkansas University Faculty Research Grant for financial support.

References

Bigmore, H. R., Lawrence, S. C., Mountford, P. & Tredget, C. S. (2005). Dalton Trans. pp. 635-651.  [CrossRef] [PubMed]
Lyubartseva, G. & Parkin, S. (2009). Acta Cryst. E65, m1530.  [CSD] [CrossRef] [IUCr Journals]
Lyubartseva, G., Parkin, S. & Mallik, U. P. (2011). Acta Cryst. E67, m1656-m1657.  [CSD] [CrossRef] [ChemPort] [IUCr Journals]
Lyubartseva, G., Parkin, S., Mallik, U. P. & Jeon, H. K. (2012). Acta Cryst. E68, m888.  [CSD] [CrossRef] [IUCr Journals]
Maria, L., Cunha, S., Videira, M., Gano, L., Paulo, A., Santos, I. C. & Santos, I. (2007). Dalton Trans. pp. 3010-3019.  [CSD] [CrossRef]
Nonius (1998). 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.
Paulo, A., Correia, J. D. G., Campello, M. P. C. & Santos, I. (2004). Polyhedron, 23, 331-360.  [Web of Science] [CrossRef] [ChemPort]
Sheldrick, G. M. (2008a). SADABS University of Göttingen, Germany.
Sheldrick, G. M. (2008b). Acta Cryst. A64, 112-122.  [CrossRef] [ChemPort] [IUCr Journals]


Acta Cryst (2013). E69, m532-m533   [ doi:10.1107/S1600536813024252 ]

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