(IUCr) A tetranuclear chlorido-bridged manganese(II) cluster with imidazole ligands

Volume 64
Part 10
Pages m1276-m1277
October 2008

Received 8 September 2008
Accepted 11 September 2008
Online 20 September 2008

Key indicators
Single-crystal X-ray study
T = 173 K
Mean (C-C) = 0.009 Å
Disorder in main residue
R = 0.058
wR = 0.143
Data-to-parameter ratio = 18.6
Details

A tetranuclear chlorido-bridged manganese(II) cluster with imidazole ligands

Mukhtar A. Kurawa,^a Christopher J. Adams ^a ^* and A. Guy. Orpen ^a

^aSchool of Chemistry, University of Bristol, Bristol, BS8 1TS, UK
Correspondence e-mail: C.J.Adams@bris.ac.uk

The crystal structure of di- [mu] ₃-chlorido-tetra- [mu] ₂-chlorido-dichloridoocta(imidazole- [kappa] N)tetramanganese(II) ethanol 1.234 solvate, [Mn₄Cl₈(C₃H₄N₂)₈]·1.234C₂H₅O or [Mn₄Cl₈(Him)₈]·1.234EtOH, where Him is imidazole (C₃H₄N₂), is based upon two Mn₄Cl₄ cubes which share one face, and which each lack one manganese vertex, giving a Mn₄Cl₆ unit. This contains two different octahedral coordination environments for the Mn atoms. Mn1 is coordinated by four bridging chlorido ligands and two imidazole N atoms, whereas Mn2 is coordinated by three bridging and one terminal Cl and two imidazole N atoms. The remaining two Mn centres are generated by inversion symmetry. A partial occupancy solvent molecule (ethanol) is present. The crystal structure displays several N-HCl and N-HO hydrogen bonds.

Related literature

Lee et al. (2000) reported the structure and magnetic properties of a similar chlorido-bridged tetranuclear cluster of cadmium(II) with 2(2-pyridyl)-4,4',5,5'-tetramethyl-4,5-dihydro-1H-imidazol-1-oxy-3-N-oxide (NIToPY). For the structure of [{CdCl₂(Him)₂}_n], see: Flook et al. (1973).

Experimental

Crystal data

[Mn₄Cl₈(C₃H₄N₂)₈]·1.234C₂H₅O
M_r = 1103.45
Triclinic, $[P \overline 1]$
a = 8.4763 (16) Å
b = 10.696 (2) Å
c = 12.764 (2) Å
= 99.206 (3)°
= 105.706 (4)°
= 96.187 (3)°
V = 1085.7 (3) Å³
Z = 1
Mo K radiation
= 1.68 mm^-1
T = 173 (2) K
0.35 × 0.10 × 0.10 mm

Data collection

Bruker APEX CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 2008a) T_min = 0.815, T_max = 0.850
11294 measured reflections
4920 independent reflections
3315 reflections with I > 2(I)
R_int = 0.048

Refinement

R[F² > 2(F²)] = 0.058
wR(F²) = 0.142
S = 1.04
4920 reflections
265 parameters
H-atom parameters constrained
_max = 1.17 e Å^-3
_min = -0.77 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
N8-H8O1ⁱ	0.88	2.09	2.865 (15)	147
N4-H6ACl3ⁱⁱ	0.88	2.49	3.289 (4)	152
N6-H10ACl4ⁱⁱ	0.88	2.48	3.247 (4)	146
N2-H2ACl4ⁱⁱⁱ	0.88	2.55	3.292 (4)	143
Symmetry codes: (i) x, y-1, z; (ii) x+1, y, z; (iii) -x, -y+1, -z+1.

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008b); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008b); molecular graphics: SHELXTL (Sheldrick, 2008b); software used to prepare material for publication: SHELXTL.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: SG2263 ).

Acknowledgements

MAK thanks Bayero University, Kano, Nigeria for funding.

References

Bruker (2001). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.
Flook, R. J., Freeman, H. C., Huq, F. & Rosalky, J. M. (1973). Acta Cryst. B29, 903-906.
Lee, C.-J., Wei, H.-H., Lee, G.-H. & Wang, Y. (2000). Inorg. Chem. Commun. 3, 690-693.
Sheldrick, G. M. (2008a). SADABS. University of Göttingen, Germany.
Sheldrick, G. M. (2008b). Acta Cryst. A64, 112-122.

metal-organic compounds