[μ-N,N,N′,N′-Tetra­kis(2-pyridylmeth­yl)­hexane-1,6-diamine]bis­[dichlorido­manganese(II)]

In-Chul Hwang; Nam-Ho Kim; Kwang Ha

doi:10.1107/S1600536809003663

. 2009 Feb 4;65(Pt 3):m249. doi: 10.1107/S1600536809003663

[μ-N,N,N′,N′-Tetrakis(2-pyridylmethyl)hexane-1,6-diamine]bis[dichloridomanganese(II)]

In-Chul Hwang ^a, Nam-Ho Kim ^b, Kwang Ha ^b,^*

PMCID: PMC2968529 PMID: 21582043

Abstract

The asymmetric unit of the title compound, [Mn₂Cl₄(C₃₀H₃₆N₆)], contains one-half of the formula unit; a centre of inversion is located at the mid-point of the molecule. The two Mn²⁺ ions are bridged by the dual tridentate N,N,N′,N′-tetrakis(2-pyridylmethyl)hexane-1,6-diamine ligand to form a dinuclear complex. Each Mn atom is five-coordinated in an approximately square-pyramidal geometry by three N atoms from the ligand and two Cl atoms. Intermolecular π–π interactions between adjacent pyridine rings with a centroid–centroid distance of 3.576 (2) Å are reported.

Related literature

For structural details of some related complexes, see: Hwang & Ha (2007 ▶); Song et al. (2008 ▶).

Experimental

Crystal data

[Mn₂Cl₄(C₃₀H₃₆N₆)]
M _r = 732.33
Triclinic,
a = 7.7149 (13) Å
b = 8.4660 (14) Å
c = 14.263 (2) Å
α = 83.309 (3)°
β = 88.329 (3)°
γ = 66.666 (3)°
V = 849.4 (2) Å³
Z = 1
Mo Kα radiation
μ = 1.09 mm⁻¹
T = 293 (2) K
0.35 × 0.18 × 0.06 mm

Data collection

Bruker SMART 1000 CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2000 ▶) T _min = 0.707, T _max = 0.937
4845 measured reflections
3368 independent reflections
2705 reflections with I > 2σ(I)
R _int = 0.013

Refinement

R[F ² > 2σ(F ²)] = 0.043
wR(F ²) = 0.118
S = 1.07
3368 reflections
190 parameters
H-atom parameters constrained
Δρ_max = 0.42 e Å⁻³
Δρ_min = −0.29 e Å⁻³

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: PLATON (Spek, 2003 ▶); software used to prepare material for publication: SHELXL97.

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809003663/cs2107sup1.cif

e-65-0m249-sup1.cif^{(18.9KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809003663/cs2107Isup2.hkl

e-65-0m249-Isup2.hkl^{(165.2KB, hkl)}

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

This work was supported by the Korea Research Foundation (grant No. 2006-353-C00028).

supplementary crystallographic information

Comment

The asymmetric unit of the title compound, [Mn₂Cl₄(C₃₀H₃₆N₆)], contains one half of the formula unit; a centre of inversion is located in the midpoint of the compound (Figs. 1 and 2). In the complex, the two Mn²⁺ ions are bridged by the hexadentate ligand N,N,N',N'-tetrakis(2-pyridylmethyl)hexane-1,6-diamine (tphn) to form a centrosymmetric dinuclear complex. Mn atoms are five-coordinated in an approximately square pyramidal geometry by three N atoms from the tphn ligand and two Cl atoms. The Mn—N(amine) bond length (2.339 (2) Å) is slightly longer than the Mn—N(pyridyl) bond lengths (2.246 (3) and 2.232 (2) Å). The complex displays intermolecular π-π interactions between adjacent pyridine rings. The shortest distance between Cg1 (the centroid of six-membered ring N1—C5) and Cg1ⁱ (symmetry code i: 2 - x, 1 - y, 1 - z) is 3.576 (2) Å.

Experimental

To a solution of N,N,N',N'-tetrakis(2-pyridylmethyl)hexane-1,6-diamine (0.50 g, 1.04 mmol) in EtOH (15 ml) was added MnCl₂.4H₂O (0.21 g, 1.06 mmol) and stirred for 1 h at room temparature. The volume of the solvent was reduced to 3 ml and ether (20 ml) was added. The so formed precipitate was separated by filtration and washed with EtOH/ether and dried under vacuum, to give a pale yellow powder (0.36 g). Crystals suitable for X-ray analysis were obtained from the slow evaporation of a MeOH solution. MS (FAB): m/z 570, 572 (Mn(tphn)Cl⁺).