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Volume 69 
Part 6 
Pages m314-m315  
June 2013  

Received 22 March 2013
Accepted 3 May 2013
Online 15 May 2013

Key indicators
Single-crystal X-ray study
T = 100 K
Mean [sigma](C-C) = 0.005 Å
Disorder in main residue
R = 0.041
wR = 0.113
Data-to-parameter ratio = 14.2
Details
Open access

[Diaquasesqui(nitrato-[kappa]O)hemi(perchlorato-[kappa]O)copper(II)]-[mu]-{bis[5-methyl-3-(pyridin-2-yl)-1H-pyrazol-4-yl] selenide}-[triaqua(perchlorato-[kappa]O)copper(II)] nitrate monohydrate

aNational Taras Shevchenko University, Department of Chemistry, Volodymyrska str. 64, 01601 Kyiv, Ukraine, and bFaculty of Chemistry, University of Wroclaw, 14, F. Joliot-Curie Str., 50383, Wroclaw, Poland
Correspondence e-mail: pavlenko_vadim@univ.kiev.ua

In the binuclear title complex, [Cu2(ClO4)1.5(NO3)1.5(C18H16N6Se)(H2O)5]NO3·H2O, both CuII ions are hexacoordinated by O and N atoms, thus forming axially elongated CuO4N2 octahedra. The equatorial plane of each octahedron is formed by one chelating pyrazole-pyridine fragment of the organic ligand and two water molecules. The axial positions in one octahedron are occupied by a water molecule and a monodentately coordinated perchlorate anion, while those in the other are occupied by a nitrate anion and a disordered perchlorate/nitrate anion with equal site occupancy. The pyrazole-pyridine units of the organic selenide are trans-oriented to each other with a C-Se-C angle of 96.01 (14)°. In the crystal, uncoordinated nitrate anions and the coordinating water molecules are involved in O-H...O and N-H...O hydrogen bonds, forming a bridge between the pyrazole group and the coordinating water molecules. Further O-H...O hydrogen bonds between the complex molecules and a [pi]-[pi] stacking interaction with a centroid-centroid distance of 3.834 (4) Å are also observed.

Related literature

For structural studies of related pyrazolylselenides, see: Seredyuk et al. (2010[Seredyuk, M., Fritsky, I. O., Krämer, R., Kozlowski, H., Haukka, M. & Gütlich, P. (2010). Tetrahedron, 66, 8772-8777.]) and for structural studies of d-metal complexes of bis(3,5-dimethyl-1H-pyrazol-4-yl)selenide, see: Seredyuk et al. (2007[Seredyuk, M., Haukka, M., Fritsky, I. O., Kozlowski, H., Krämer, R., Pavlenko, V. A. & Gütlich, P. (2007). Dalton Trans. pp. 3183-3194.]). For related structures, see: Fritsky et al. (2004[Fritsky, I. O., Swiatek-Kozlowska, J., Dobosz, A., Sliva, T. Y. & Dudarenko, N. M. (2004). Inorg. Chim. Acta, 357, 3746-3752.]); Kanderal et al. (2005[Kanderal, O. M., Kozlowski, H., Dobosz, A., Swiatek-Kozlowska, J., Meyer, F. & Fritsky, I. O. (2005). Dalton Trans. pp. 1428-1437.]); Moroz et al. (2010[Moroz, Y. S., Szyrweil, L., Demeshko, S., Kozlowski, H., Meyer, F. & Fritsky, I. O. (2010). Inorg. Chem. 49, 4750-4752.]).

[Scheme 1]

Experimental

Crystal data
  • [Cu2(ClO4)1.5(NO3)1.5(C18H16N6Se)(H2O)5]NO3·H2O

  • Mr = 934.72

  • Triclinic, [P \overline 1]

  • a = 9.7233 (6) Å

  • b = 13.1987 (7) Å

  • c = 13.3217 (8) Å

  • [alpha] = 93.510 (4)°

  • [beta] = 108.858 (5)°

  • [gamma] = 93.494 (4)°

  • V = 1608.93 (16) Å3

  • Z = 2

  • Mo K[alpha] radiation

  • [mu] = 2.67 mm-1

  • T = 100 K

  • 0.30 × 0.25 × 0.12 mm

Data collection
  • Bruker SMART APEXII CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2009[Bruker (2009). APEX2, SAINT and SADABS. Bruker-Nonius BV, Delft, The Netherlands.]) Tmin = 0.468, Tmax = 0.728

  • 11167 measured reflections

  • 7085 independent reflections

  • 5817 reflections with I > 2[sigma](I)

  • Rint = 0.073

Refinement
  • R[F2 > 2[sigma](F2)] = 0.041

  • wR(F2) = 0.113

  • S = 1.02

  • 7085 reflections

  • 498 parameters

  • 12 restraints

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

  • [Delta][rho]max = 1.00 e Å-3

  • [Delta][rho]min = -0.95 e Å-3

Table 1
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
O1-H2O1...O10 0.83 (2) 1.93 (2) 2.737 (3) 164 (4)
O1-H1O1...O18i 0.81 (2) 2.00 (2) 2.801 (6) 174 (5)
O1-H1O1...O20i 0.81 (2) 1.99 (3) 2.747 (6) 155 (4)
O2-H1O2...O13ii 0.83 (2) 1.85 (2) 2.660 (3) 163 (4)
O2-H2O2...O3iii 0.83 (2) 1.99 (2) 2.805 (4) 167 (4)
O3-H1O3...O11i 0.83 (2) 2.03 (2) 2.842 (4) 166 (4)
O3-H1O3...O12i 0.83 (2) 2.47 (3) 3.130 (4) 137 (4)
O4-H1O4...O10iv 0.83 (2) 1.94 (2) 2.762 (3) 174 (4)
O4-H2O4...O1Wv 0.84 (2) 1.88 (2) 2.717 (4) 174 (5)
O5-H1O5...O13 0.82 (2) 1.87 (3) 2.617 (4) 150 (4)
O5-H2O5...O16 0.84 (2) 1.97 (3) 2.719 (11) 148 (4)
O5-H2O5...O16 0.84 (2) 1.97 (3) 2.719 (11) 148 (4)
O5-H2O5...O22 0.84 (2) 2.07 (3) 2.784 (10) 142 (4)
O1W-H2W1...O6iv 0.83 (2) 2.10 (3) 2.800 (4) 142 (4)
O1W-H1W1...O16vi 0.84 (2) 2.12 (3) 2.833 (9) 144 (4)
O1W-H1W1...O22vi 0.84 (2) 2.23 (3) 2.977 (11) 149 (4)
N2-H1N2...O11 0.86 1.98 2.829 (4) 168
N5-H1N5...O1W 0.86 1.94 2.762 (4) 160
Symmetry codes: (i) -x+1, -y+1, -z+1; (ii) x-1, y+1, z; (iii) -x, -y+1, -z+1; (iv) x, y-1, z; (v) -x+1, -y, -z+1; (vi) x-1, y, z.

Data collection: APEX2 (Bruker, 2009[Bruker (2009). APEX2, SAINT and SADABS. Bruker-Nonius BV, Delft, The Netherlands.]); cell refinement: SAINT (Bruker, 2009[Bruker (2009). APEX2, SAINT and SADABS. Bruker-Nonius BV, Delft, The Netherlands.]); data reduction: SAINT; program(s) used to solve structure: SIR2004 (Burla et al., 2005[Burla, M. C., Caliandro, R., Camalli, M., Carrozzini, B., Cascarano, G. L., De Caro, L., Giacovazzo, C., Polidori, G. & Spagna, R. (2005). J. Appl. Cryst. 38, 381-388.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: DIAMOND (Brandenburg, 2009[Brandenburg, K. (2009). DIAMOND. Crystal Impact GbR, 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: IS5261 ).


Acknowledgements

The financial support from the State Fund for Fundamental Researches of Ukraine (grant No. F40.3/041) and the Swedish Institute (Visby Program) is gratefully acknowledged. MS thanks the EU for a Marie Curie fellowship (IIF-253254).

References

Brandenburg, K. (2009). DIAMOND. Crystal Impact GbR, Bonn, Germany.
Bruker (2009). APEX2, SAINT and SADABS. Bruker-Nonius BV, Delft, The Netherlands.
Burla, M. C., Caliandro, R., Camalli, M., Carrozzini, B., Cascarano, G. L., De Caro, L., Giacovazzo, C., Polidori, G. & Spagna, R. (2005). J. Appl. Cryst. 38, 381-388.  [ISI] [CrossRef] [ChemPort] [details]
Fritsky, I. O., Swiatek-Kozlowska, J., Dobosz, A., Sliva, T. Y. & Dudarenko, N. M. (2004). Inorg. Chim. Acta, 357, 3746-3752.  [ISI] [CSD] [CrossRef] [ChemPort]
Kanderal, O. M., Kozlowski, H., Dobosz, A., Swiatek-Kozlowska, J., Meyer, F. & Fritsky, I. O. (2005). Dalton Trans. pp. 1428-1437.  [CrossRef] [PubMed]
Moroz, Y. S., Szyrweil, L., Demeshko, S., Kozlowski, H., Meyer, F. & Fritsky, I. O. (2010). Inorg. Chem. 49, 4750-4752.  [ISI] [CSD] [CrossRef] [ChemPort] [PubMed]
Seredyuk, M., Fritsky, I. O., Krämer, R., Kozlowski, H., Haukka, M. & Gütlich, P. (2010). Tetrahedron, 66, 8772-8777.  [ISI] [CSD] [CrossRef] [ChemPort]
Seredyuk, M., Haukka, M., Fritsky, I. O., Kozlowski, H., Krämer, R., Pavlenko, V. A. & Gütlich, P. (2007). Dalton Trans. pp. 3183-3194.  [CSD] [CrossRef] [PubMed]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [ChemPort] [details]


Acta Cryst (2013). E69, m314-m315   [ doi:10.1107/S1600536813012178 ]

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