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Volume 69 
Part 2 
Pages m112-m113  
February 2013  

Received 9 October 2012
Accepted 14 January 2013
Online 19 January 2013

Key indicators
Single-crystal X-ray study
T = 105 K
Mean [sigma](C-C) = 0.005 Å
Disorder in solvent or counterion
R = 0.045
wR = 0.124
Data-to-parameter ratio = 14.0
Details
Open access

(Acetonitrile){2-[bis(pyridin-2-ylmethyl-[kappa]2N)amino-[kappa]N]-N-(2,6-dimethylphenyl)acetamide-[kappa]O}(perchlorato-[kappa]O)zinc (acetonitrile){2-[bis(pyridin-2-ylmethyl-[kappa]2N)amino-[kappa]N]-N-(2,6-dimethylphenyl)acetamide-[kappa]O}zinc tris(perchlorate)

aSchool of Pharmacy, University of Oslo, PO Box 1068 Blindern, N-0316 Oslo, Norway, and bDepartment of Chemistry, University of Oslo, PO Box 1033 Blindern, N-0315 Oslo, Norway
Correspondence e-mail: pal.rongved@farmasi.uio.no

In the title salt, [Zn(C22H24N4O)(CH3CN)][Zn(ClO4)(C22H24N4O)(CH3CN)](ClO4)3, two differently coordinated zinc cations occur. In the first complex, the metal ion is coordinated by the N,N',N'',O-tetradentate acetamide ligand and an acetonitrile N atom, generating an approximate trigonal-bipyramidal coordination geometry, with the O atom in an equatorial site and the acetonitrile N atom in an axial site. In the second complex ion, a perchlorate ion is also bonded to the zinc ion, generating a distorted trans-ZnO2N4 octahedron. Of the uncoordinating perchlorate ions, one lies on a crystallographic twofold axis and one lies close to a twofold axis and has a site occupancy of 0.5. N-H...O and N-H...(O,O) hydrogen bonds are observed in the crystal. Disordered solvent molecules occupy about 11% of the unit-cell volume; their contribution to the scattering was removed with the SQUEEZE routine of the PLATON program [Spek (2009[Spek, A. L. (2009). Acta Cryst. D65, 148-155.]). Acta Cryst. D65, 148-155.].

Related literature

For related structures found in the Cambridge Structural Database (Version 5.33 of November 2011; Allen, 2002[Allen, F. H. (2002). Acta Cryst. B58, 380-388.]), see: Xu et al. (2010a[Xu, Z., Baek, K.-H., Kim, H. N., Cui, J., Qian, X., Spring, D. R., Shin, I. & Yoon, J. (2010a). J. Am. Chem. Soc. 132, 601-610.],b[Xu, Z., Han, S. J., Lee, C., Yoon, J. & Spring, D. R. (2010b). Chem. Commun. 46, 1679-1682.]); Patten et al. (2008[Patten, T. E., Olmstead, M. M. & Troeltzsch, C. (2008). Inorg. Chim. Acta, 361, 365-372.]); Marlin et al. (2006[Marlin, D. S., Cabrera, D. G., Leigh, D. A. & Slawin, A. M. Z. (2006). Angew. Chem. Int. Ed. 45, 77-83.]). For biochemical background, see: Makhov et al. (2008[Makhov, P., Golovine, K., Uzzo, R. G., Rothman, J., Crispen, P. L., Shaw, T., Scoll, B. J. & Kolenko, V. M. (2008). Cell Death Differ. 15, 1745-1751.]); Xu et al. (2010a[Xu, Z., Baek, K.-H., Kim, H. N., Cui, J., Qian, X., Spring, D. R., Shin, I. & Yoon, J. (2010a). J. Am. Chem. Soc. 132, 601-610.]).

[Scheme 1]

Experimental

Crystal data
  • [Zn(C22H24N4O)(C2H3N)][Zn(ClO4)(C22H24N4O)(C2H3N)](ClO4)3

  • Mr = 1331.59

  • Monoclinic, C 2/c

  • a = 41.253 (8) Å

  • b = 15.057 (3) Å

  • c = 20.809 (4) Å

  • [beta] = 106.106 (2)°

  • V = 12418 (4) Å3

  • Z = 8

  • Mo K[alpha] radiation

  • [mu] = 1.03 mm-1

  • T = 105 K

  • 0.91 × 0.29 × 0.22 mm

Data collection
  • Bruker APEXII CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2007[Bruker (2007). APEX2, SAINT-Plus and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.531, Tmax = 0.798

  • 43906 measured reflections

  • 10987 independent reflections

  • 8503 reflections with I > 2[sigma](I)

  • Rint = 0.051

Refinement
  • R[F2 > 2[sigma](F2)] = 0.045

  • wR(F2) = 0.124

  • S = 1.07

  • 10987 reflections

  • 782 parameters

  • 8 restraints

  • H-atom parameters constrained

  • [Delta][rho]max = 0.89 e Å-3

  • [Delta][rho]min = -0.66 e Å-3

Table 1
Selected bond lengths (Å)

Zn1A-N4A 2.058 (3)
Zn1A-N3A 2.059 (3)
Zn1A-N5A 2.060 (3)
Zn1A-O1A 2.087 (2)
Zn1A-N2A 2.236 (2)
Zn1A-O1D 2.310 (2)
Zn1B-N3B 2.020 (3)
Zn1B-O1B 2.025 (2)
Zn1B-N4B 2.040 (3)
Zn1B-N5B 2.043 (3)
Zn1B-N2B 2.240 (2)

Table 2
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
N1A-H1A...O3Di 0.88 2.00 2.868 (3) 171
N1B-H1B...O4Eii 0.88 2.15 2.979 (3) 157
N1B-H1B...O3Eii 0.88 2.41 3.138 (4) 141
Symmetry codes: (i) [x, -y+1, z+{\script{1\over 2}}]; (ii) [x, -y, z+{\script{1\over 2}}].

Data collection: APEX2 (Bruker, 2007[Bruker (2007). APEX2, SAINT-Plus and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT-Plus (Bruker, 2007[Bruker (2007). APEX2, SAINT-Plus and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL and Mercury (Macrae et al., 2008[Macrae, C. F., Bruno, I. J., Chisholm, J. A., Edgington, P. R., McCabe, P., Pidcock, E., Rodriguez-Monge, L., Taylor, R., van de Streek, J. & Wood, P. A. (2008). J. Appl. Cryst. 41, 466-470.]); software used to prepare material for publication: SHELXTL.


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: HB6972 ).


Acknowledgements

The work has been partly supported by Statoil Norge AS.

References

Allen, F. H. (2002). Acta Cryst. B58, 380-388.  [ISI] [CrossRef] [details]
Bruker (2007). APEX2, SAINT-Plus and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Macrae, C. F., Bruno, I. J., Chisholm, J. A., Edgington, P. R., McCabe, P., Pidcock, E., Rodriguez-Monge, L., Taylor, R., van de Streek, J. & Wood, P. A. (2008). J. Appl. Cryst. 41, 466-470.  [ISI] [CrossRef] [ChemPort] [details]
Makhov, P., Golovine, K., Uzzo, R. G., Rothman, J., Crispen, P. L., Shaw, T., Scoll, B. J. & Kolenko, V. M. (2008). Cell Death Differ. 15, 1745-1751.  [ISI] [CrossRef] [PubMed] [ChemPort]
Marlin, D. S., Cabrera, D. G., Leigh, D. A. & Slawin, A. M. Z. (2006). Angew. Chem. Int. Ed. 45, 77-83.  [ISI] [CSD] [CrossRef] [ChemPort]
Patten, T. E., Olmstead, M. M. & Troeltzsch, C. (2008). Inorg. Chim. Acta, 361, 365-372.  [ISI] [CSD] [CrossRef] [ChemPort]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Spek, A. L. (2009). Acta Cryst. D65, 148-155.  [ISI] [CrossRef] [details]
Xu, Z., Baek, K.-H., Kim, H. N., Cui, J., Qian, X., Spring, D. R., Shin, I. & Yoon, J. (2010a). J. Am. Chem. Soc. 132, 601-610.  [ISI] [CSD] [CrossRef] [ChemPort] [PubMed]
Xu, Z., Han, S. J., Lee, C., Yoon, J. & Spring, D. R. (2010b). Chem. Commun. 46, 1679-1682.  [CSD] [CrossRef] [ChemPort]


Acta Cryst (2013). E69, m112-m113   [ doi:10.1107/S1600536813001396 ]

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