Received 19 March 2013
The title compound, [Mn6(C7H4NO3)5(CH3CO2)2(C4H6N2)4.62(C3H7NO)1.38]·(C2H5)2O·C3H7NO·CH3OH·0.49H2O or MnII(OAc)2[15-MCMn(III)N(shi)-5](Me-Im)4.62(DMF)1.38·diethyl ether·DMF·MeOH·0.49H2O (where MC is metallacrown, -OAc is acetate, shi3- is salicylhydroximate, Me-Im is 1-methylimidazole, DMF is N,N-dimethylformamide, and MeOH is methanol), is comprised of five MnIII ions in the metallacrown ring and an MnII ion which is encapsulated in the central cavity. Four of the ring MnIII ions are six-coordinate with distorted octahedral geometries. Two of these MnIII ions have a planar configuration, while the other two MnIII have absolute stereoconfiguration. The fifth MnIII is five-coordinated with distorted square-pyramidal geometry. Four of the ring MnIII ions each bind one 1-methylimidazole, while the final ring MnIII ion binds a DMF solvent molecule in an axial position and located in a trans position is either a Me-Im or a DMF molecule. The occupancy ratio of Me-Im to DMF is 0.62 (2) to 0.38 (2). The central MnII is seven-coordinate with a geometry best described as distorted face-capped trigonal-prismatic. DMF, diethyl ether, MeOH, and water molecules are located in the interstitial voids between the metallacrown molecules. The methanol molecule is positionally disordered [0.51 (1):0.49 (1)] and associated with a partially occupied water molecule [0.49 (1)]. This disorder is also associated with the positional disorder of the diethyl ether molecule [0.51 (1):0.49 (1)].
For a general review of metallacrowns, see: Mezei et al. (2007). For related manganese and vanadium metallacrown structures, see: Lah & Pecoraro (1989) and Pecoraro (1989), respectively. For related Mn(II)[15-MCMn(III)N(shi)-5)] structures and synthetic procedures, see: Kessissoglou et al. (1994), Dendrinou-Samara et al. (2001, 2002, 2005); Emerich et al. (2010); Tigyer et al. (2011, 2012). For an explanation on how to calculate the s/h ratio, see: Stiefel & Brown (1972). For an explanation on how to calculate bond-valence-sum values, see: Liu & Thorp (1993). For an explanation on how to calculate the asymmetry parameter, see: Addison et al. (1984). For CELL_NOW software, see: Sheldrick (2008b).
Data collection: APEX2 (Bruker, 2012); cell refinement: SAINT (Bruker, 2012); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008a); program(s) used to refine structure: SHELXL2012 (Sheldrick, 2008a) and SHELXLE Rev600 (Hübschle et al., 2011); molecular graphics: Mercury (Macrae et al., 2006); software used to prepare material for publication: publCIF (Westrip, 2010).
Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: JJ2164 ).
This work was funded by the Shippensburg University Foundation (grant No. UGR2012/13-08) to BRT and CMZ. The diffractometer was funded by NSF grant No. 0087210, by Ohio Board of Regents grant No. CAP-491, and by YSU. The authors would like to thank Professor George M. Sheldrick for providing access to the beta version of SHELXL2012 prior to its official release.
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