Perchlorato[N,N,N′,N′-tetra­kis(2-pyridyl­meth­yl)cyclo­hexane-1,2-diamine]manganese(II) perchlorate

Hwang, I.-C.; Ha, K.

doi:10.1107/S1600536808025804

Volume 64
Part 9
Page m1178
September 2008

Received 5 August 2008
Accepted 11 August 2008
Online 16 August 2008

Key indicators
Single-crystal X-ray study
T = 293 K
Mean (C-C) = 0.005 Å
Disorder in main residue
R = 0.039
wR = 0.093
Data-to-parameter ratio = 12.0
Details

Perchlorato[N,N,N',N'-tetrakis(2-pyridylmethyl)cyclohexane-1,2-diamine]manganese(II) perchlorate

In-Chul Hwang ^a and Kwang Ha ^b ^*

^aDepartment of Chemistry, Pohang University of Science and Technology, Pohang 790-784, Republic of Korea, and ^bSchool of Applied Chemical Engineering, Research Institute of Catalysis, Chonnam National University, Gwangju 500-757, Republic of Korea
Correspondence e-mail: hakwang@chonnam.ac.kr

The asymmetric unit of the title compound, [Mn(ClO₄)(C₃₀H₃₄N₆)]ClO₄, consists of a cationic [Mn(ClO₄)(C₃₀H₃₄N₆)]⁺ complex and a perchlorate anion. In the complex, the Mn²⁺ ion is seven-coordinated in an approximately pentagonal-bipyramidal environment by six N atoms from the hexadentate N,N,N',N'-tetrakis(2-pyridylmethyl)cyclohexane-1,2-diamine (tpdach) ligand and one O atom from a perchlorate anion. The complex displays intermolecular [pi] - [pi] interactions between adjacent pyridine rings (centroid-to-centroid distance 4.133 Å). Moreover, there are weak intra- and intermolecular C-HO hydrogen bonds. The Cl atom and two O atoms of the perchlorate are disordered, with a site-occupancy factor of 0.59 (2) for the major component.

Related literature

For details of some other tpdach complexes, see: Hwang & Ha (2006); McCusker et al. (1993). For the synthesis of the ligand, see: Toftlund & Yde-Anderson (1981).

Experimental

Crystal data

[Mn(ClO₄)(C₃₀H₃₄N₆)]ClO₄
M_r = 732.47
Monoclinic, C c
a = 14.223 (5) Å
b = 14.121 (5) Å
c = 16.504 (6) Å
= 105.987 (6)°
V = 3186.6 (19) Å³
Z = 4
Mo K radiation
= 0.64 mm^-1
T = 293 (2) K
0.25 × 0.25 × 0.20 mm

Data collection

Bruker SMART 1000 CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2000) T_min = 0.690, T_max = 0.879
9661 measured reflections
5412 independent reflections
4446 reflections with I > 2(I)
R_int = 0.020

Refinement

R[F² > 2(F²)] = 0.039
wR(F²) = 0.093
S = 0.96
5412 reflections
452 parameters
2 restraints
H-atom parameters constrained
_max = 0.39 e Å^-3
_min = -0.29 e Å^-3
Absolute structure: Flack (1983), with 1804 Friedel pairs
Flack parameter: 0.007 (16)

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
C7-H7O1	0.93	2.41	3.006 (5)	122
C17-H17AO2ⁱ	0.97	2.48	3.413 (5)	161
C18-H18O8ⁱⁱ	0.98	2.47	3.436 (6)	170
C20-H20O6	0.93	2.46	3.347 (6)	159
C25-H25O1	0.93	2.46	3.038 (5)	121
C25-H25O2	0.93	2.51	3.199 (5)	131
C28-H28O8ⁱⁱⁱ	0.93	2.48	3.243 (6)	139
C30-H30AO3Aⁱ	0.97	2.55	3.434 (11)	152
Symmetry codes: (i) $[x, -y+1, z+{\script{1\over 2}}]$ ; (ii) $[x, -y, z+{\script{1\over 2}}]$ ; (iii) $[x-{\script{1\over 2}}, -y+{\script{1\over 2}}, z+{\script{1\over 2}}]$ .

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 (Farrugia, 1997) and PLATON (Spek, 2003); software used to prepare material for publication: SHELXL97.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: ZL2134 ).

Acknowledgements

This work was supported by a Korea Research Foundation Grant funded by the Korean Government (MOEHRD) (KRF-2007-412-J02001).

References

Bruker (2000). SADABS, SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.
Flack, H. D. (1983). Acta Cryst. A39, 876-881.
Hwang, I.-C. & Ha, K. (2006). Z. Kristallogr. New Cryst. Struct. 221, 468-470.
McCusker, J. K., Toftlund, H., Rheingold, A. L. & Hendrickson, D. N. (1993). J. Am. Chem. Soc. 115, 1797-1804.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13.
Toftlund, H. & Yde-Anderson, S. (1981). Acta Chem. Scand. A, 35, 575-585.

metal-organic compounds