(Acetonitrile){2-[bis­(pyridin-2-ylmethyl-κ2N)amino-κN]-N-(2,6-dimethyl­phen­yl)acetamide-κO}(perchlorato-κO)zinc (acetonitrile){2-[bis­(pyridin-2-ylmethyl-κ2N)amino-κN]-N-(2,6-dimethyl­phen­yl)acetamide-κO}zinc tris­(perchlorate)

Åstrand, O.A.H.; Görbitz, C.H.; Kristoffersen, K.A.; Rongved, P.

doi:10.1107/S1600536813001396

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 (C-C) = 0.005 Å
Disorder in solvent or counterion
R = 0.045
wR = 0.124
Data-to-parameter ratio = 14.0
Details

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

Ove Alexander Høgmoen Åstrand,^a Carl Henrik Görbitz,^b Kenneth Aase Kristoffersen ^b and Pål Rongved ^a ^*

^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-HO 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). Acta Cryst. D65, 148-155.].

Related literature

For related structures found in the Cambridge Structural Database (Version 5.33 of November 2011; Allen, 2002), see: Xu et al. (2010a,b); Patten et al. (2008); Marlin et al. (2006). For biochemical background, see: Makhov et al. (2008); Xu et al. (2010a).

Experimental

Crystal data

[Zn(C₂₂H₂₄N₄O)(C₂H₃N)][Zn(ClO₄)(C₂₂H₂₄N₄O)(C₂H₃N)](ClO₄)₃
M_r = 1331.59
Monoclinic, C 2/c
a = 41.253 (8) Å
b = 15.057 (3) Å
c = 20.809 (4) Å
= 106.106 (2)°
V = 12418 (4) Å³
Z = 8
Mo K radiation
= 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) T_min = 0.531, T_max = 0.798
43906 measured reflections
10987 independent reflections
8503 reflections with I > 2(I)
R_int = 0.051

Refinement

R[F² > 2(F²)] = 0.045
wR(F²) = 0.124
S = 1.07
10987 reflections
782 parameters
8 restraints
H-atom parameters constrained
_max = 0.89 e Å^-3
_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-HA	D-H	HA	DA	D-HA
N1A-H1AO3Dⁱ	0.88	2.00	2.868 (3)	171
N1B-H1BO4Eⁱⁱ	0.88	2.15	2.979 (3)	157
N1B-H1BO3Eⁱⁱ	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); cell refinement: SAINT-Plus (Bruker, 2007); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL and Mercury (Macrae et al., 2008); 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

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